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WO2025040240A1 - Perfume oil capsules for solid formulations with fragrance boost - Google Patents

Perfume oil capsules for solid formulations with fragrance boost Download PDF

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Publication number
WO2025040240A1
WO2025040240A1 PCT/EP2023/072855 EP2023072855W WO2025040240A1 WO 2025040240 A1 WO2025040240 A1 WO 2025040240A1 EP 2023072855 W EP2023072855 W EP 2023072855W WO 2025040240 A1 WO2025040240 A1 WO 2025040240A1
Authority
WO
WIPO (PCT)
Prior art keywords
fragrance
pastille
weight
polymer
microcapsule
Prior art date
Application number
PCT/EP2023/072855
Other languages
French (fr)
Inventor
Julian Alexander GEORGI
Thorsten BÖDDEKER
Nelli LESCHENKO
Jonas MEISEL
Bennet GRIMM
Edison Diaz
Original Assignee
Symrise Ag
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Symrise Ag filed Critical Symrise Ag
Priority to PCT/EP2023/072855 priority Critical patent/WO2025040240A1/en
Publication of WO2025040240A1 publication Critical patent/WO2025040240A1/en

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Classifications

    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q13/00Formulations or additives for perfume preparations
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/02Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/11Encapsulated compositions
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/50Perfumes
    • C11D3/502Protected perfumes
    • C11D3/505Protected perfumes encapsulated or adsorbed on a carrier, e.g. zeolite or clay
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/005Compositions containing perfumes; Compositions containing deodorants
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/41Particular ingredients further characterized by their size
    • A61K2800/412Microsized, i.e. having sizes between 0.1 and 100 microns
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/56Compounds, absorbed onto or entrapped into a solid carrier, e.g. encapsulated perfumes, inclusion compounds, sustained release forms
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/80Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof

Definitions

  • the present invention relates to the field of perfumed particles in particular for solid consumer product formulations such as textile care products or the like. More specifically, the present invention relates to a composition comprising or consisting of at least one pastille, wherein said pastille comprises or consists of at least one microcapsule as well as a polymer matrix embedding said at least one microcapsule, wherein the composition further comprises free fragrance as well as to a composition additionally comprising or consisting of at least one adhesion agent in said matrix. Moreover, the present invention relates to a process for the preparation of a corresponding composition and their use for the preparation of consumer products as well as consumer products as such comprising or consisting of the compositions according to the invention.
  • the fragrant substances or cosmetic ingredients of such products interact with other components of the product formulation, or the more volatile components of the perfume formulation tend to evaporate prematurely. Consequently, this leads to an undesired change and/or decrease of the fragrance impression or premature “use” of the cosmetic ingredient over time or might even cause disadvantageous reactions with the other ingredients of the product formulation resulting in a reduced product quality and/or stability.
  • the fragrances or other active ingredients can be added to the formulation in encapsulated form.
  • a broad variety of consumer products comprise encapsulated active ingredients such as fragrances in their formulations.
  • textile care formulations such as liquid detergents or fabric softener comprise a plurality of such perfumed microcapsules.
  • said formulations require the incorporation of preservatives in order to increase their stability and durability such as methylisothiazolinone (MIT) which can cause allergic reactions or skin irritations, while powdered detergents usually do not require the addition of preservatives and cause a reduced environmental pollution.
  • MIT methylisothiazolinone
  • microcapsules are incorporated into powdered formulations such as powdered detergent.
  • powdered formulations such as powdered detergent
  • the incorporation of microcapsules into powdered formulations is considerably aggravated as a mixing of the microcapsule component and the other detergent components leads to breakage of the fragile microcapsules resulting in a loss of for example olfactory performance.
  • microcapsules that have both good stability and good release properties.
  • the ability of the capsules to retain the active ingredient and thus to prevent the loss of volatile components depends in particular on the stability of the capsules in the product base.
  • very stable microcapsules e.g. capsules having a comparably thick capsule wall
  • very stable microcapsules usually tend to exhibit a low performance as the break of the microcapsules and thus the release of the active ingredient(s) is hindered.
  • they are too unstable, they are already destroyed during storage or result in a leakage of the active ingredient and do not perform either.
  • an increase of the capsule wall i.e. a multi-layered microcapsule shell or a thicker shell, respectively, likewise result in a decreased performance as the targeted release of the active ingredient is aggravated and said microcapsules usually require a complex multi-step preparation process.
  • compositions for solid consumer product formulations should be obtained more easily and the resulting compositions should show improved properties, e.g. in terms of their olfactory qualities.
  • the present invention was made in view of the disadvantages described above. To solve the above-mentioned drawbacks, the present invention provides a composition and a method for the preparation thereof, allowing for the efficient incorporation of active ingredients with improved olfactory performances and stabilities into solid consumer product formulations and/or for the preparation of consumer products as such.
  • the present invention provides a process allowing for the facilitated processing of corresponding compositions, simultaneously showing improved olfactory properties.
  • the present invention relates to a composition
  • a composition comprising or consisting of at least one pastille, wherein said pastille (based on the total weight of the pastille) comprises or consists of:
  • adhesion agent is preferably selected from the group consisting of fatty acids, fatty alcohols, fatty acid esters or mixtures thereof, such as waxes;
  • the polymer is preferably polyethylene glycol
  • the adhesion agent is preferably selected from the group consisting of animal and/or vegetable waxes, and is preferably beeswax.
  • the present invention relates to a process for the preparation of a composition comprising or consisting of a plurality of pastilles, comprising the following steps of:
  • step (v) forming pastilles by dripping the mixture of step (iv);
  • the present invention relates to a composition comprising or consisting of at least one pastille obtained by the process according to the invention, wherein said pastille comprises or consists of:
  • adhesion agent is preferably selected from the group consisting of fatty acids, fatty alcohols, fatty acid esters or mixtures thereof, such as waxes; and
  • composition has a viscosity q of less than 900 mPa s at 80 °C.
  • compositions prepared according to the inventive process relate to compositions prepared according to the inventive process.
  • the present invention relates to the use of a composition according to the invention for the preparation of consumer products and formulations thereof as well as consumer products and formulations thereof as such comprising or consisting of the composition according to the present invention.
  • compositions according to the present invention allow for an efficient and further improved incorporation of active ingredients in encapsulated form which show excellent release properties (performances) into a broad range of solid consumer product formulations and consumer products as such which simultaneously show excellent olfactory performances, in particular pre-rub performances.
  • the polymeric matrix serves as a buffer protecting the fragile microcapsules during the preparation of the final consumer product (formulation) from mechanical, chemical and/or thermal influences without negatively influencing the performance of the microcapsules within the consumer product (formulation).
  • the present dosage form allows for an efficient incorporation of active ingredients via microcapsules in solid consumer product formulations while simultaneously allowing for an efficient and targeted release of said active ingredients, thus overcoming the drawbacks of the state of the art.
  • the fragile microcapsules are embedded in a protecting matrix which even withstands harsh chemical and physical conditions such as increased temperatures or acidic or basic conditions.
  • the addition of free fragrance substances or fragrance mixtures which are dispersed in said polymer matrix further improve the initial olfactory properties of the solid consumer product (formulation) and allow for a facilitated processing and improved homogeneity by advantageously influencing the viscosity of the compositions according to the invention.
  • Figure 1 shows the results of the sensory evaluation of the performance (i.e. the release properties) of different samples of powder detergent in dependence of the presence of a fragrance emulsifier (i.e. a free fragrance component).
  • a fragrance emulsifier i.e. a free fragrance component
  • Figure 2 shows the viscosity of different samples in dependence of the presence of a fragrance emulsifier (i.e. a free fragrance component).
  • a fragrance emulsifier i.e. a free fragrance component
  • Figure 3 shows the viscosity of different samples in dependence of the type of fragrance emulsifier (polymer matrix: PEG 6,000 g/mol).
  • Figure 4 shows the viscosity of different samples in dependence of the molecular weight of the polymer matrix (PEG 6,000 g/mol; PEG 8,000 g/mol; PEG 10,000 g/mol).
  • Figure 5 Figure 5 shows the results of the sensory evaluation of the performance (i.e. release properties) of different samples in powder detergent for different adhesion agents.
  • Figure 6 Figure 6 shows different samples of compositions comprising or consisting of at least one pastille prepared according to the invention showing the influence of the microcapsule slurry content.
  • Figure 7 shows different samples of compositions comprising or consisting of at least one pastille prepared based on the invention showing the influence of the water content / plasticizer content (without microcapsules).
  • Figure 8 shows different samples of compositions comprising or consisting of at least one pastille prepared according to the invention showing the influence of the water content / plasticizer content (with microcapsules).
  • Figure 10 shows a picture of microcapsules and free fragrance oil in PEG.
  • composition according to the present invention comprises at least one microcapsule encapsulating an active ingredient, wherein said at least one microcapsule is dispersed in a polymeric matrix.
  • microcapsules are used in the printing industry, food industry (vitamins, flavours, plant extracts, enzymes, microorganisms), agricultural chemistry (fertilizers, pesticides), feed industry (minerals, vitamins, enzymes, drugs, microorganisms), pharmaceutical industry, detergent industry, and cosmetic industry, among others.
  • the core material is preferably a hydrophobic active substance, i.e., a substance that has a specific effect or causes a specific reaction, for example, a drug, a pesticide, a cosmetic active ingredient, a food active ingredient, etc.
  • a hydrophobic active substance i.e., a substance that has a specific effect or causes a specific reaction, for example, a drug, a pesticide, a cosmetic active ingredient, a food active ingredient, etc.
  • the microcapsules have a core material comprising or consisting of a hydrophobic single fragrant substance or single odorant substance or a mixture of two or more such substances, i.e. wherein the core material comprises at least one single fragrant substance or single odorant substance or mixtures thereof (i.e. a perfume oil), selected from one or more of the following groups:
  • the molecular weight of the polymer used as component (b) is within the ranges specified above, an efficient protection of the fragile microcapsules can be achieved allowing for an efficient incorporation in solid consumer product formulations which simultaneously allows for an efficient targeted release of the active ingredient(s).
  • a “meltable” polymer is a plastic polymer material that becomes pliable or moldable at a certain elevated temperature and solidifies upon cooling.
  • the polymer used within the context of the present invention can be either a water- soluble or a water-insoluble polymer.
  • component (b) comprises a mixture of one or more water-soluble polymers, a mixture of one or more waterinsoluble polymers, or a mixture of one or more water-soluble polymers and one or more waterinsoluble polymers.
  • the melting point of the polymer according to the present invention preferably having a molecular weight from about 3,000 Da to 20,000 Da
  • suitable waterinsoluble polymers include amongst others classical capsules with coating, waxes such as beeswax, sunflower seed wax, rice bran wax, carnauba wax, pinova wax, rapeseed wax, soywax, candelilla wax, jojoba oil, cork wax, guaruma wax, cotton wax, foxwax, peat wax, rose wax, jasmine wax, peetha-wax from wax gourd, myrtle wax (Myrica cerifera), wax fig wax, berry wax and mixtures of different waxes.
  • waxes such as beeswax, sunflower seed wax, rice bran wax, carnauba wax, pinova wax, rapeseed wax, soywax, candelilla wax, jojoba oil, cork wax, guaruma wax, cotton wax, foxwax, peat wax, rose wax, jasmine wax, peetha-wax from wax gourd,
  • compositions of the present invention according to the second aspect may comprise from 60% to 80% by weight based on the total weight of a pastille of the polymer (component (b)), preferably from 65% to 75% by weight, and even more preferred from 70% to 75% by weight of the pastille.
  • Adhesion agent [0102] Adhesion agent:
  • adhesion agents are for example:
  • Animal and vegetable waxes in particular beeswax, wool wax, China wax, rice bran wax, sunflower seed wax, rice bran wax, carnauba wax, sugarcane wax, pinova wax, rapeseed wax, soy wax, candelilla wax, jojoba oil, cork wax, guaruma wax, ouricury wax (Syagrus coronata), Cuba palm wax (Copernicia hospita), esparto wax (Lygeum spartum, Stipa tenacissima), cotton wax, flax wax, peat wax, rose wax, jasmine wax, peetha wax from wash gourd, and also myrtle wax (Myrica cerifera), wax fig wax, berry wax. as well as mixtures of two or more of the aforementioned adhesion agents.
  • the at least one adhesion agent is selected from the group consisting of animal and/or vegetable waxes, and is preferably (natural) beeswax.
  • the at least one adhesion agent is a vegetable wax, i.e. a wax of plant origin.
  • the at least one adhesion agent is an animal wax, such as beeswax or lanolin (wax obtained from wool).
  • adhesion agent as specified herein can improve the release performance/sensory performance and thus the sensory experience by one unit, i.e. by more than 10% in intensity/efficacy. Accordingly, the adhesion agents as used herein also be considered as “sensory boosters” or “scent boosters”.
  • Biobased materials refer to compounds containing organic carbon of renewable origin such as from agricultural, plant, animal, fungi, microorganism, marine or forestry materials living in a natural environment in equilibrium with the atmosphere, being of non-fossil origin such as petroleum as defined according to the ASTM D6866 standard test.
  • biogenic compounds are compounds containing carbon (organic and inorganic) of renewable origin like agricultural, plant, animal, fungi, microorganisms, microorganisms, marine, or forestry materials.
  • the inventive compositions comprise such biogenic or biobased, i.e., bio-derived materials. Therefore, bioderived materials are preferably used for the preparation of pastilles and thus compositions according to the invention.
  • the at least one adhesion agent is paraffin wax.
  • the adhesion agent component is incorporated into the polymeric matrix.
  • the adhesion agent used as component (c) according to the second aspect of the present invention is comprised in an amount of from 2% to 32% by weight based on the total weight of the pastille, preferably from 3% to 20% by weight, and more preferred from 4% to 17% by weight, and most preferred from 5% to 10% by weight of the pastille.
  • adhesion agent(s) within said ranges allows for an improved balance between microcapsule protection and adhesion promotion as well as scent boost.
  • the density of the polymer matrix ranges from 0.95 g/cm 3 to 1.10 g/cm 3 and preferably from 0.99 g/cm 3 to 1 .05 g/cm 3 .
  • the density is within the above ranges, it was found that the homogeneity of the pastilles according to the invention is improved and that the preparation of the pastilles according to the invention is further facilitated.
  • the density was determined as bulk density which is defined as the mass of particles per volume, of a mixture of the solid bulk material and a continuous fluid / solvent which fills the cavities between the particles.
  • lower amounts of the polymer component implicitly mean higher amounts of the microcapsule component.
  • the microcapsule component is preferably added in the form of an aqueous slurry, the increased amount of water will result in the composition getting softer and stickier thereby rendering the preparation of pastilles more challenging (see Figures 6 and 7). This effect can surprisingly be partially compensated by adding an adhesion agent as specified herein.
  • the overall amount of the adhesion agent is kept low, and preferably below 10% by weight of the pastille in order to avoid potential disadvantages such as the formation of stains on textiles caused by the water-insoluble adhesion agent component (such as a wax) e.g. during the textile washing process.
  • the water-insoluble adhesion agent component such as a wax
  • compositions further comprise free fragrance(s).
  • free fragrance refers to either a single fragrance substance or a mixture of two or more fragrance substances which are dispersed within the polymeric matrix in unencapsulated (or non-encapsulated) form, i.e. this fragrance component is not present in the form of discrete microcapsules.
  • compositions according to the present invention additionally necessarily comprise a single free fragrance substance or a mixture two or more fragrance substances (i.e. a free fragrance mixture or free perfume oil), i.e. the compositions according to the present invention additionally comprise at least one unencapsulated or free fragrance substance as additional component.
  • the sensory data shows that the addition of a free oil / free fragrance component provides a better odour impression.
  • the free fragrance substance or the free fragrance mixture (mixture of two or more fragrance substances) is comprised in amounts of 0.1% by weight to 10% by weight based on the total weight of the pastille, and preferably in amounts of 2% by weight to 8% by weight and further preferred in amounts of 2% by weight to 5% by weight.
  • Suitable fragrance substances and mixtures thereof are described above in the context of microencapsulation.
  • the free fragrance component (either a single free fragrance substance or a mixture of two or more fragrance substances) can either be the same or different compared to the encapsulated fragrance component in terms of amount and/or chemical composition.
  • Said free fragrance component serves as emulsifier (“fragrance emulsifier”) and further facilitates the preparation of the pastilles according to the invention in a more homogenous manner while simultaneously adding olfactory benefits.
  • the comprised free fragrance component further improves the final product properties allowing for an efficient adjustment of the viscosity and flexibility of the polymeric matrix resulting in a less brittle and more flexible matrix with improved buffering effect and thus better protection of the fragile microcapsules and a facilitated incorporation into solid consumer product formulations without altering the fundamental chemical character of the plasticized material (see Figures 1 to 4).
  • the free fragrance component facilitates the pastille formation and significantly improves the miscibility of the microcapsule component and the polymer component and further optional components or additives thereby allowing for achieving a more homogeneous distribution of the microcapsules (and thus the active ingredients) within the polymeric matrix.
  • the presence of free fragrance(s) surprisingly reduces the compositions viscosity and thus positively influences the properties of the composition by allowing a more homogeneous distribution of the pastille components.
  • the processability is facilitated. This allows for the preparation of more stable pastilles with improved release properties.
  • For fragrance microcapsules an improved and more homogeneous scent release was observed when combined with free fragrance(s).
  • the compositions according to the present invention allow for an instantly perceivable scent experience.
  • fragrance substances such as Agrumex LC, Agrunitril, Aldehyd C10, Aldehyd C12 Laurin, Aldehyd C12 MNA, Aldehyd C14 sog., Allylcapronat, Amarocit, Ambrocenide, Amylsalicylat, Benzalydehyd, Benzylacetat, Benzylaceton, Benzylsalicylat, Borneol/lsoborneol 65:35, Bourgeonal, Citronellol 950, Clonal, CM20 Sanjinol Replacer, Coniferan, Cumarin, Cyclamenaldehyd, Cyclohexylsalicylat, Damascenon, Damascene Delta, Decenol, Dihydromrycenol, Dimethylbenzylcarbinol, Dimethylbenzylcarbinylacetat, Diphenyloxid, Dipropyl
  • fragrance substances are selected from the group of hydrocarbons such as Caren Delta-nat, Caryophyllen nat. rekt., Pinen alpha laevo nat., Terpinen Gamma and mixtures thereof.
  • compositions according to the invention can further comprise a certain amount of at least one plasticizer as additive.
  • the compositions according to the present invention can comprise one single plasticizer or a mixture of two or more of such plasticizers.
  • a plasticizer is a substance that is used to increase the flexibility and plasticity of a specific substance or composition and can additionally decrease the viscosity as well as the friction of a substance or composition.
  • Suitable plasticizers are known to the person skilled in the art. Suitable plasticizers are for example water, polyethylene glycol, ortho phthalates, phthalate esters, trimellitates and esters thereof, (organo)phosphates, aliphatic dibasic acid esters, benzoate esters, polyesters, citrates, bioderived plasticizers based on epoxidized soybean oil, epoxidized linseed oil, castor oil, palm oil, other vegetable oils, starches, sugars and the like, chlorinated paraffins, alkyl sulfonic acid esters, dicarbonates, fatty acid esters.
  • the plasticizer(s) is/are selected from amongst others water or polyethylene glycol.
  • the plasticizer water can origin for example from the manufacture process of the pastilles or can be added subsequently.
  • the plasticizer and preferably the plasticizer water, is provided through the addition of an aqueous microcapsule slurry (component (a)), i.e. wherein the aqueous phase of the microcapsule slurry is serving as plasticizer.
  • component (a) i.e. wherein the aqueous phase of the microcapsule slurry is serving as plasticizer.
  • polyethylene glycol is used as the plasticizer component.
  • the molecular weight of the plasticizer polyethylene glycol is below 4,000 Da, further preferred below 3,500 Da and most preferred below 3,000 Da.
  • the plasticizer(s) used as additive(s) according to the present invention is/are comprised in an amount of from 0.5% to 10% by weight based on the total weight of the pastille, preferably from 2% to 8% by weight, and more preferred from 3% to 6% by weight.
  • plasticizer(s) within said ranges allows for efficiently adjusting the viscosity and flexibility of the polymeric matrix resulting in a less brittle and more flexible matrix with improved buffering effect and thus better protection of the fragile microcapsules and a facilitated incorporation into solid consumer product formulations without altering the fundamental chemical character of the plasticized material.
  • compositions according to the present invention can comprise one single structuring agent or a mixture of two or more of such structuring agents.
  • composition according to the first and second aspect of the present invention includes at least a surfactant.
  • Said structuring agent(s) is/are preferably comprised in an amount ranging from 0.1 % to 10% by weight based on the total weight of a pastille, preferably from 1% to 8% by weight and even more preferred from 2% to 7% by weight.
  • Suitable structuring agents are commercially available surfactants or emulsifiers known in the art and esters such as isopropyl myristate.
  • a structuring agent further improves the homogeneity of the inventive compositions, in particular in the presence of waxes. Mixtures of waxes and polyethylene glycol tend to separate and form distinct phases. However, by adding a structuring agent as specified herein a homogeneous formulation can be obtained.
  • the structuring agent can be an emulsifier or surfactant.
  • the addition of surfactants is particularly suitable for compositions comprising an adhesion agent as specified herein.
  • the compositions according to the present invention may comprise any kind of surfactant, namely anionic surfactants, cationic surfactants, non-ionic surfactants, amphoteric / zwitterionic surfactant, and any mixture thereof. Among these surfactants non-ionic surfactants are particularly preferred.
  • Suitable surfactants are for example selected from the group consisting of ammonium derivates, esters, sulfonates, sulfates, sorbates and related surfactants, and mixtures thereof.
  • Non-ionic detergents are particularly beneficial for preparing “green” compositions.
  • surfactants can be used either singular or in the form of mixtures of two, three, or even more surfactants, either from the same surfactant category (anionic, cationic, non-ionic, amphoteric/zwitterionic) or as mixture of surfactants of different surfactant categories.
  • the composition according to the second aspect of the present invention includes at least one surfactant, preferably a non-ionic surfactant.
  • the present invention relates to a composition
  • a composition comprising or consisting of at least one pastille, wherein said pastille comprises or consists of:
  • adhesion agent is preferably selected from the group consisting of fatty acids, fatty alcohols, fatty acid esters or mixtures thereof, such as waxes; based on the total weight of the pastille; and
  • said at least one pastille further comprises or consists of: from 0.1% to 10% by weight of at least one structuring agent, preferably a surfactant and even more preferred a non-ionic surfactant, wherein said structuring agent is preferably selected from the group consisting of esters, such as isopropyl myristate or other emulsifiers; based on the total weight of the pastille.
  • compositions according to the present invention can comprise further suitable additives if required.
  • Further suitable additives are for example dyes, laundry actives etc.
  • compositions according to the present invention comprise or consist of at least one pastille having the compositions specified above.
  • the compositions are present as a plurality of pastilles.
  • the compositions are present as a single pastille of the above-specified compositions according to the first or second aspect.
  • compositions of the present invention comprise or consist of at least one pastille comprising an encapsulated active ingredient, preferably a fragrance (mixture), a polymer forming a polymer matrix, preferably polyethylene glycol, and free fragrance (mixture).
  • an encapsulated active ingredient preferably a fragrance (mixture)
  • a polymer forming a polymer matrix preferably polyethylene glycol
  • free fragrance mixture
  • composition thus comprises or consists of at least one pastille, wherein said pastille comprises or consists of:
  • the pastille of the composition according to the first aspect further comprises or consists of:
  • plasticizer from 0.5% to 10% by weight (based on the total weight of the pastille) of at least one plasticizer, wherein said plasticizer is preferably water or polyethylene glycol.
  • compositions of the present invention comprise or consist of at least one pastille comprising an encapsulated active ingredient, preferably a fragrance (mixture), a polymer forming a polymer matrix, preferably polyethylene glycol, free fragrance (mixture) and optionally at least one adhesion agent.
  • an encapsulated active ingredient preferably a fragrance (mixture)
  • a polymer forming a polymer matrix preferably polyethylene glycol
  • free fragrance mixture
  • adhesion agent optionally at least one adhesion agent
  • composition comprises or consists of at least one pastille, wherein said pastille comprises or consists of:
  • adhesion agent is preferably selected from the group consisting of fatty acids, fatty alcohols, fatty acid esters or mixtures thereof, such as waxes;
  • the pastille of the composition according to the second aspect further optionally comprises or consists of:
  • plasticizer preferably water or polyethylene glycol
  • said structuring agent is preferably selected from the group consisting of esters, such as isopropyl myristate or other emulsifiers; based on the total weight of the pastille.
  • the present invention relates to a composition
  • a composition comprising or consisting of at least one pastille, wherein said pastille comprises or consists of:
  • adhesion agent is preferably selected from the group consisting of fatty acids, fatty alcohols, fatty acid esters or mixtures thereof, such as waxes; based on the total weight of the pastille; and (d) from 0.1% to 10% by weight of free fragrance or free fragrance mixture; based on the total weight of the pastille, wherein said at least one pastille further comprises or consists of: from 0.1% to 10% by weight of at least one structuring agent, preferably a surfactant and even more preferred a non-ionic surfactant, wherein said structuring agent is preferably selected from the group consisting of esters, such as isopropyl myristate or other emulsifiers; based on the total weight of the pastille.
  • compositions according to the second aspect of the present invention further comprising an adhesion agent as specified herein show improved protection and release properties. Moreover, it was found that the preparation of such pastilled compositions can be improved due to the presence of the adhesion agent resulting in more homogeneous, more flexible and less brittle pastilles with an enhanced microcapsule distribution (see also Example 5).
  • compositions and consequently the pastilles according to the present invention have a solidification point from 25 °C to 100 °C, preferably from 30 °C to 90 °C, more preferably from 35 °C to 85 °C and most preferred from 40 °C to 75 °C.
  • a solidification point within this range allows for a facilitated handling of the compositions according to the present invention and the pastilles thereof.
  • compositions according to the present invention and consequently the corresponding pastille have a viscosity q in the range from 500 mPas to 1 ,000 mPas at a temperature of 70 °C and a shear pressure of 6.4 Pa, preferably a viscosity in the range from 760 mPas to 980 mPas, and even more preferred a viscosity in the range from 800 mPas to 950 mPas.
  • the viscosity q is even more preferred in the range from 750 mPas to 1 ,000 mPas at a temperature of 70 °C and a shear pressure of 6.4 Pa, preferably a viscosity in the range from 760 mPas to 980 mPas, and even more preferred a viscosity in the range from 800 mPas to 950 mPas. If the viscosity of the compositions is within the above ranges, the composition is considered “solid” at room temperature. [0183] Thus, preferably, the composition according to the present invention is preferably a solid composition.
  • the viscosity of the composition influences the pastille formation by dripping as such as well as the stability of the pastilles (see Figures 6 and 7). If the viscosity of the compositions is within the above ranges processing of the compositions (in particular in a pastillation process as specified herein) and their incorporation into solid consumer product formulations is facilitated. Additionally, if the viscosity is within the above ranges an ideal balance between microcapsule protection and microcapsule performance can be achieved. Due to the low viscosity, the mixture can be homogenized better, and at the same time the lower viscosity allows for an improved dripping behaviour.
  • the encapsulated actives can be distributed in a more homogeneous manner within the pastilles.
  • such viscosities provide for improved pastille flexibilities, i.e. the pastille are less brittle and simultaneously show an improved buffering effect.
  • the viscosity can be adjusted correspondingly via the content of the adhesion agent as well as the plasticizer content.
  • compositions according to the present invention and consequently the corresponding pastilles have a Young's modulus E of higher than 100 Pa and less than 1 GPa, preferably from 1 kPa to 100 MPa, and even more preferred from 10 kPa to 1 MPa.
  • the Young's modulus E describes the tensile or compressive stiffness of a solid but elastic material when the force is applied lengthwise based on the tensile/compressive stress (force per unit area) and axial strain (proportional deformation) in the linear elastic region of a material.
  • the total water content in the composition according to the present invention and thus of the corresponding pastilles is from 2% to 12% by weight based on the total weight of a pastille.
  • the water content is in the range from 3% to 9% by weight and even more preferred in the range from 4% to 8% by weight.
  • Such amounts of water are advantageous in terms of flexibility as the water component can function as plasticizer and thus is valuable in view of an improved buffering effect and thus better protection of the fragile microcapsules and a facilitated incorporation into solid consumer product formulations without altering the fundamental chemical character of the plasticized material. Higher amounts of water will decrease the viscosity too much making an incorporation into solid formulations more difficult while to low water contents make the pastille material to brittle for an incorporation.
  • compositions according to the present invention can be adjusted based on the specific amounts of the components, the molecular weight of the polymer and the free fragrance component as well as the optional addition of additives such as the plasticizers and structuring agents described above.
  • the particle size of the pastille(s) of the compositions according to the present invention is from 1 pm to 1 cm, preferably from 100 pm to 7 mm and even more preferred from 500 pm to 5 mm in order to achieve an ideal distribution of the pastilles within the final solid consumer product formulation and thus in turn of the microcapsules embedded therein. Too big pastilles result in an inhomogeneous distribution within the final product formulation.
  • the ratio between the size of the microcapsules and the size of the final granules/pastilles is in the range of from 1 : 5 to 1 : 200, preferably from 1 : 10 to 1 : 100.
  • Said pastilles or granules are preferably present in the shape of tablets, pills, spheres, and the like, having a spherical, hemispherical, compressed hemispherical, lentil shaped, and oblong shape and can be prepared by any method known in the art by those skilled in the art (see Figure 6).
  • the composition of the invention and the pastilles thereof may further comprise one or more ingredients which improve the visual aesthetics of the final product such as colourants.
  • the composition can comprise further additives and/or active ingredients such as optical brighteners, cleaning agents, laundry actives and the like.
  • compositions according to the present invention do not comprise a balancing agent and/or do not comprise a filler.
  • the present invention relates to a process for the preparation of a composition comprising or consisting of a plurality of pastilles comprising the following steps of:
  • step (v) forming pastilles by dripping the mixture of step (iv);
  • step (vi) optionally cooling; optionally further comprising the step of adding at least one plasticizer and/or at least one structuring agent in, or after step (ii), (iii) and/or (iv).
  • the components specified above in the context of the first and second aspect likewise apply to the subject of the third aspect, i.e. the terms “microcapsule”, “polymer”, “free fragrance”, “adhesion agent”, “plasticizer”, “pastille”, “structuring agent” etc. as well as the corresponding amounts and properties as specified above.
  • microcapsules as specified herein are provided.
  • Said microcapsules can either be present as such or alternatively in the form of an aqueous dispersion comprising one or more microcapsules and preferably a plurality of microcapsules.
  • the microcapsules are dispersed in an aqueous phase, microcapsules according to the invention dispersed in an aqueous phase, preferably wherein the microcapsule concentration within the aqueous phase is greater than 5% and less than 70% by weight, preferably greater than 20% and less than 60% by weight, most preferably greater than 30% and less than 50% by weight based on the weight of the dispersion.
  • microcapsules in the form of a dispersion is advantageous in terms of a more homogeneous distribution of the microcapsules within the final pastilles.
  • the comprised water of the continuous or outer phase of the dispersion can serve as plasticizer helping to improve the final product properties as specified above, allowing for an efficient adjustment of the viscosity and flexibility of the polymeric matrix resulting in a less brittle and more flexible matrix with improved buffering effect and thus better protection of the fragile microcapsules and a facilitated incorporation into solid consumer product formulations without altering the fundamental chemical character of the plasticized material.
  • microcapsule(s) is/are provided in the form of an aqueous dispersion in step (i) of the process according to the third aspect of the present invention.
  • the at least one polymer is melted.
  • an adhesion agent can be added which is heated and melted together with the polymer as specified herein.
  • both substances can be melted separately and subsequently the resulting corresponding melts can be combined and homogenized.
  • a polymer as specified herein, and preferably polyethylene glycol wherein the melting point of the at least one polymer, and preferably of the polyethylene glycol, is in the range from 25 °C to 100 °C, and preferably from 40 °C to 80 °C.
  • the melting point of the polymer according to the first, second and/or third aspect of the present invention preferably having a molecular weight from about 3,000 Da to 20,000 Da is preferably in the range from 25 °C to 100 °C, and preferably from 40 °C to 80 °C in order to efficiently and homogeneously embed the microcapsules within the polymeric matrix.
  • the melting step (ii) is conducted at a temperature in the range from 25 °C to 100 °C, preferably from 40 °C to 80 °C, and even more preferred at 80 °C in order to achieve a homogeneous distribution of microcapsules in the polymeric buffering matrix.
  • additional additives such as adhesion agents, surfactants, plasticizers and/or structuring agents can be added and mixed to obtain a homogenous mixture.
  • the at least one microcapsule or microcapsule dispersion is mixed into the polymer melt of step (ii) and the resulting mixture homogenized in a further process step (iii) in order to obtain a homogeneous distribution of discrete microcapsules within the melt.
  • the as-prepared polymer composition is then mixed with free, i.e. unencapsulated fragrance component (a single fragrance substance or a mixture of two or more fragrance substances) (step (iv)).
  • free, i.e. unencapsulated fragrance component a single fragrance substance or a mixture of two or more fragrance substances
  • step (v) pastilles are formed by dripping the mixture of step (iv) using state-of-the-art pastillation processes known to those skilled in the art.
  • Pastillation is a particle forming process, where usually a pastille is formed using a droplet former, followed by cooling of the as-obtained discrete particles.
  • Processes for the preparation of pastilles or granules are commercially used methods and the pastilles may be formed into different shapes include tablets, pills, spheres, and the like.
  • up-scaling by dropping using a pulse generator in air or vegetable oil also showed good results.
  • the obtained granules are solidified in an additional cooling step (vi).
  • At least one plasticizer and/or a structuring agent and/or surfactant can be added in or after step (ii), (iii) and/or (iv).
  • the free fragrance component is mixed with the molten polymer and the microcapsules are added afterwards.
  • composition is prepared based on the following steps:
  • step (iii) admixing free fragrance or a free fragrance mixture into the polymer melt of step (ii);
  • step (vi) optionally cooling; optionally further comprising the step of adding at least one plasticizer and/or at least one structuring agent in or after step (ii), (iii) and/or (iv).
  • compositions prepared according to the inventive process relate to compositions prepared according to the inventive process.
  • the additional free fragrance(s) dispersed in the polymeric matrix further improve the processability, homogeneity and release properties. Additionally, it instantly improves the consumer's scent experience from the onset.
  • the present invention also relates to the use of the composition according to the present invention for the preparation of consumer products and formulations thereof, wherein said consumer product or consumer product formulation is a solid product such as a textile care product (such as a powder detergent, laundry soap, solid fabric softener), a solid soap, a household product (such as a solid WC-cleaner, solid allpurpose cleaners, powdered carpet cleaners, powdery washing agents for washing dishes or for cleaning various surfaces), a personal care product (such as a deodorant, soap), scent boosters, fragrance enhancers, a pharmaceutical product, and mixtures thereof.
  • a textile care product such as a powder detergent, laundry soap, solid fabric softener
  • a solid soap such as a solid WC-cleaner, solid allpurpose cleaners, powdered carpet cleaners, powdery washing agents for washing dishes or for cleaning various surfaces
  • a personal care product such as a deodorant, soap
  • scent boosters such as a deodorant, soap
  • fragrance enhancers such as a pharmaceutical product
  • Example 1 Composition comprising microcapsules with and without additional free fragrances in powder detergent - Sensory evaluation.
  • a composition comprising or consisting of at least one pastille comprising microcapsules was prepared as follows: In a first step core-shell microcapsules comprising a melamine-formaldehyde-based shell material and a fragrance core were provided (microcapsule size: 10 to 50 pm). The microcapsules were prepared according to the state of the art. Subsequently, 78.8% by weight of a polymer mixture comprising PEG-150 and PEG-450 were mixed with 7.5% by weight of rapeseed wax was melted at a temperature of 80 °C.
  • a non-ionic surfactant Imbentin AG/168S/500 G
  • free fragrance free fragrance mixture 1 : mixture of aldehydes, alcohols, ketones, and hydrocarbons.
  • 8% by weight of a microcapsule slurry the capsule-to-water ratio of the slurry was 2:3 by weight of the slurry
  • the viscous mixture was dripped a using state-of-the-art pastillation process by dripping the viscous material through small openings in order to form a plurality of pastilles having an average particle size of approximately 2 mm in which the microcapsules are embedded in a polyethylene glycol matrix, followed by cooling for solidification of the pastilles.
  • the portion of the polyethylene glycol of the final pastilles was about 78.8% by weight based on the total weight of each pastille.
  • the amounts of the above-mentioned components are based on the total weight of the final pastille.
  • fragrance composition/mixtures was used as the free fragrance component:
  • the sensory evaluation was performed as follows: Once the composition according to the present invention was prepared the as-obtained pastilles were combined with commercially available powder detergent and homogenized. The final dosage of the microcapsules in 40 g of the powder detergent was 0.5% by weight (corresponding to 6.25% by weight of pastilles in 40 g of the powder detergent).
  • All microcapsules have a particle size in the range of 10 - 50 pm.
  • the fragrance release was carried out in four steps.
  • the first step describes the smelling of a freshly washed, i.e. wet or damp cloth.
  • the second step described the smelling of an untreated dry cloth (“pre-rub”).
  • the third step describes the smelling of a lightly kneaded dry cloth; for this purpose, the cloth was subjected to slight mechanical stress by moving it back and forth between the hands several times, causing the capsules to break.
  • the fourth step describes the smelling after the dry clothes were rubbed strongly and thus the capsules broke.
  • the fragrance intensity was evaluated.
  • 8 to 9 test persons assessed the fragrance intensity on a scale of 1 (no odour) to 9 (very strong odour).
  • the mechanical treatment of the textiles causes a rupture of the fragile microcapsules thereby releasing the active ingredient (here: fragrance composition).
  • active ingredient here: fragrance composition
  • samples comprising the composition according to the present invention comprising the core-shell microcapsules embedded in a polyethylene glycol matrix show a considerably increased performance indicating an efficient protection of the fragile microcapsules within the solid product formulation while simultaneously allowing for an efficient release of the active ingredient.
  • the polymer matrix serves as a shock absorbing layer in the production process of the consumer product. Samples not containing such a shock absorbing layer and such comprising a mere coating do not perform as most of the microcapsules are already destroyed during the preparation of the consumer product.
  • Example 2 Composition comprising microcapsules with and without additional free fragrances - Viscosity in dependence of the presence of free fragrances.
  • composition comprising or consisting of at least one pastille comprising microcapsules was prepared in accordance with Example 1 . Subsequently, the pastilles were analysed using a rheometer (HAAKE Rheometer RS 1 (RheoStress)) and the viscosity was tested at different temperatures.
  • HAAKE Rheometer RS 1 HeoStress
  • Example 3 Composition comprising microcapsules with additional free fragrances - Viscosity in dependence of the type of free fragrance.
  • a composition comprising or consisting of at least one pastille comprising microcapsules was prepared as follows: In a first step core-shell microcapsules comprising a melamine-formaldehyde-based shell material and a fragrance core were provided (microcapsule size: 10 to 50 pm). The microcapsules were prepared according to the state of the art. Subsequently, 78.8% by weight of the polymer PEG-150 were mixed with 7.5% by weight of rapeseed wax was melted at a temperature of 80 °C. Thereafter, 2.5% by weight of a non-ionic surfactant (Imbentin AG/168S/500 G) were added followed by 3.2% by weight of free fragrance and 8% by weight capsule slurry (capsule to water ratio 2:3).
  • a non-ionic surfactant Imbentin AG/168S/500 G
  • fragrance compositions/mixtures were used as the free fragrance component:
  • Free fragrance mixture 1 General fragrance Mixture of: Agrumex LC, Agrunitril, Aldehyd C10, Aldehyd C12 Laurin, Aldehyd C12 MNA, Aldehyd C14 sog., Allylcapronat, Amarocit, Ambrocenide, Amylsalicylat, Benzalydehyd, Benzylacetat, Benzylaceton, Benzylsalicylat, Borneol/lsoborneol 65:35, Bourgeonal, Citronellol 950, Clonal, CM20 Sanjinol Replacer, Coniferan, Cumarin, Cyclamenaldehyd, Cyclohexylsalicylat, Damascenon, Damascene Delta, Decenol, Dihydromrycenol, Dimethylbenzylcarbinol, Dimethylbenzylcarbinylacetat, Diphenyloxid, Dipropylenglycol,
  • Example 4 Composition comprising microcapsules with additional free fragrances - Viscosity in dependence of the molecular weight of the polymer matrix.
  • a composition comprising or consisting of at least one pastille comprising microcapsules was prepared as follows: In a first step core-shell microcapsules comprising a melamine-formaldehyde-based shell material and a fragrance core were provided (microcapsule size: 10 to 50 pm). The microcapsules were prepared according to the state of the art. Subsequently, 78.8% by weight of the polymer PEG were mixed with 7.5% by weight of rapeseed wax was melted at a temperature of 80 °C.

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Abstract

The present invention relates to the field of perfumed particles in particular for solid consumer product formulations such as textile care products and the like. More specifically, the present invention relates to a composition comprising or consisting of at least one pastille, wherein said pastille comprises or consists of at least one microcapsule as well as a polymer matrix embedding said at least one microcapsule, wherein the composition further comprises free fragrance as well as to a composition additionally comprising or consisting of at least one adhesion agent in said matrix. Moreover, the present invention relates to a process for the preparation of a corresponding composition and their use for the preparation of consumer products as well as consumer products as such comprising or consisting of the composition according to the invention.

Description

Perfume oil capsules for solid formulations with fragrance boost
Field of the Invention
[0001 ] The present invention relates to the field of perfumed particles in particular for solid consumer product formulations such as textile care products or the like. More specifically, the present invention relates to a composition comprising or consisting of at least one pastille, wherein said pastille comprises or consists of at least one microcapsule as well as a polymer matrix embedding said at least one microcapsule, wherein the composition further comprises free fragrance as well as to a composition additionally comprising or consisting of at least one adhesion agent in said matrix. Moreover, the present invention relates to a process for the preparation of a corresponding composition and their use for the preparation of consumer products as well as consumer products as such comprising or consisting of the compositions according to the invention.
Background of the Invention
[0002] Nowadays many consumer products such as detergents, fabric softeners, washing powders, deodorants, lotions, etc. are perfumed with fragrance materials or contain cosmetic ingredients to deliver a specific effect.
[0003] Unfortunately, often, for example, the fragrant substances or cosmetic ingredients of such products interact with other components of the product formulation, or the more volatile components of the perfume formulation tend to evaporate prematurely. Consequently, this leads to an undesired change and/or decrease of the fragrance impression or premature “use” of the cosmetic ingredient over time or might even cause disadvantageous reactions with the other ingredients of the product formulation resulting in a reduced product quality and/or stability. In order to prevent possible interactions of the fragrances or other active components with the other ingredients of the product or, for example, to prevent the volatilization of the fragrances and thus not to distort or reduce the desired olfactory impression, the fragrances or other active ingredients can be added to the formulation in encapsulated form. In this way, for example the desired olfactory impression can be guaranteed based on a targeted release of the active component. Moreover, interactions between the product components can be reduced allowing for improved product quality and storage stability. [0004] Therefore, a broad variety of consumer products comprise encapsulated active ingredients such as fragrances in their formulations. For example, textile care formulations such as liquid detergents or fabric softener comprise a plurality of such perfumed microcapsules. Additionally, said formulations require the incorporation of preservatives in order to increase their stability and durability such as methylisothiazolinone (MIT) which can cause allergic reactions or skin irritations, while powdered detergents usually do not require the addition of preservatives and cause a reduced environmental pollution. However, the incorporation of microcapsules into powdered formulations such as powdered detergent is considerably aggravated as a mixing of the microcapsule component and the other detergent components leads to breakage of the fragile microcapsules resulting in a loss of for example olfactory performance.
[0005] It is particularly difficult to produce microcapsules that have both good stability and good release properties. The ability of the capsules to retain the active ingredient and thus to prevent the loss of volatile components depends in particular on the stability of the capsules in the product base. However, very stable microcapsules, e.g. capsules having a comparably thick capsule wall, usually tend to exhibit a low performance as the break of the microcapsules and thus the release of the active ingredient(s) is hindered. However, if they are too unstable, they are already destroyed during storage or result in a leakage of the active ingredient and do not perform either. Thus, an increase of the capsule wall, i.e. a multi-layered microcapsule shell or a thicker shell, respectively, likewise result in a decreased performance as the targeted release of the active ingredient is aggravated and said microcapsules usually require a complex multi-step preparation process.
[0006] In addition, there is a new and increasing trend towards solid consumer products such as solid hair care products, soaps and solid body wash in view of the public's increased ecological awareness (less waste, less preservatives, etc.), so that solid consumer products will become more and more relevant not only in the cosmetic industry but also in other industries. However, as indicated above, the incorporation of microcapsules into powdered formulations is considerably aggravated as a mixing of the microcapsule component and the other usually solid detergent components leads to breakage of the fragile microcapsules.
[0007] Consequently, there is a need to improve the efficient incorporation of actives such as perfuming ingredients into solid consumer product formulations, which however, simultaneously allow for an efficient and targeted release of said active. [0008] Particularly, there is a need to provide compositions comprising said actives for use in such consumer product formulations, in particular textile treatment compositions, with improved olfactory performances and stabilities.
[0009] Simultaneously, in order to cover the high demand, the compositions for solid consumer product formulations should be obtained more easily and the resulting compositions should show improved properties, e.g. in terms of their olfactory qualities.
Summary of the Invention
[0010] The present invention was made in view of the disadvantages described above. To solve the above-mentioned drawbacks, the present invention provides a composition and a method for the preparation thereof, allowing for the efficient incorporation of active ingredients with improved olfactory performances and stabilities into solid consumer product formulations and/or for the preparation of consumer products as such.
[0011 ] More specifically, the present invention provides a process allowing for the facilitated processing of corresponding compositions, simultaneously showing improved olfactory properties.
[0012] Thus, in a first aspect the present invention relates to a composition comprising or consisting of at least one pastille, wherein said pastille (based on the total weight of the pastille) comprises or consists of:
(a) from 0.5% to 10% by weight of at least one microcapsule encapsulating an active ingredient, wherein said active ingredient is preferably a single fragrance or a fragrance mixture;
(b) from 92% to 98% by weight of a polymer, wherein said polymer is preferably polyethylene glycol; and
(c) from 0.1% to 10% by weight of free fragrance or a free fragrance mixture, and preferably a hydrophobic fragrance or fragrance mixture (i.e. a hydrophobic free fragrance component); based on the total weight of the pastille.
[0013] Preferably said composition is used for the preparation of perfumed consumer product formulations, in particular perfumed textile treatment compositions. [0014] In a preferred embodiment of the composition, the polymer is preferably polyethylene glycol.
[0015] According to a second aspect the present invention relates to a composition comprising or consisting of at least one pastille, wherein said pastille (based on the total weight of the pastille) comprises or consists of:
(a) from 0.5% to 10% by weight of at least one microcapsule encapsulating an active ingredient, wherein said active ingredient is preferably a fragrance or fragrance mixture;
(b) from 60% to 80% by weight of at least one polymer, wherein said polymer is preferably polyethylene glycol;
(c) from 2% to 32% by weight of at least one adhesion agent, wherein said adhesion agent is preferably selected from the group consisting of fatty acids, fatty alcohols, fatty acid esters or mixtures thereof, such as waxes; and
(d) from 0.1% to 10% by weight of free fragrance or a free fragrance mixture, and preferably a hydrophobic fragrance or fragrance mixture (i.e. a hydrophobic free fragrance component).
[0016] In a preferred embodiment of said composition, the polymer is preferably polyethylene glycol, and/or the adhesion agent is preferably selected from the group consisting of animal and/or vegetable waxes, and is preferably beeswax.
[0017] According to a third aspect the present invention relates to a process for the preparation of a composition comprising or consisting of a plurality of pastilles, comprising the following steps of:
(i) providing at least one microcapsule or an aqueous dispersion comprising at least one microcapsule;
(ii) melting of at least one polymer and optionally an adhesion agent;
(iii) mixing the at least one microcapsule into the polymer melt of step (ii);
(iv) admixing a free fragrance or a free fragrance mixture;
(v) forming pastilles by dripping the mixture of step (iv); and
(vi) optionally cooling; optionally further comprising the step of adding at least one plasticizer and/or at least one structuring agent in, or after step (ii), (iii) and/or (iv). [0018] Furthermore, the present invention relates to a composition comprising or consisting of at least one pastille obtained by the process according to the invention, wherein said pastille comprises or consists of:
(a) at least one microcapsule encapsulating an active ingredient, wherein said active ingredient is preferably a fragrance or a fragrance mixture;
(b) at least one polymer, preferably polyethylene glycol;
(c) optionally at least one adhesion agent, wherein said adhesion agent is preferably selected from the group consisting of fatty acids, fatty alcohols, fatty acid esters or mixtures thereof, such as waxes; and
(d) a free fragrance or a free fragrance mixture, and preferably a hydrophobic fragrance or fragrance mixture (i.e. a hydrophobic free fragrance component); wherein the composition has a viscosity q of less than 900 mPa s at 80 °C.
[0019] Additionally, in a further aspect the present invention relates to compositions prepared according to the inventive process.
[0020] Finally, the present invention relates to the use of a composition according to the invention for the preparation of consumer products and formulations thereof as well as consumer products and formulations thereof as such comprising or consisting of the composition according to the present invention.
[0021 ] That is, the present inventors have found that the compositions according to the present invention allow for an efficient and further improved incorporation of active ingredients in encapsulated form which show excellent release properties (performances) into a broad range of solid consumer product formulations and consumer products as such which simultaneously show excellent olfactory performances, in particular pre-rub performances. Thereby, the polymeric matrix serves as a buffer protecting the fragile microcapsules during the preparation of the final consumer product (formulation) from mechanical, chemical and/or thermal influences without negatively influencing the performance of the microcapsules within the consumer product (formulation). Based thereon the present dosage form allows for an efficient incorporation of active ingredients via microcapsules in solid consumer product formulations while simultaneously allowing for an efficient and targeted release of said active ingredients, thus overcoming the drawbacks of the state of the art. The fragile microcapsules are embedded in a protecting matrix which even withstands harsh chemical and physical conditions such as increased temperatures or acidic or basic conditions. The addition of free fragrance substances or fragrance mixtures which are dispersed in said polymer matrix further improve the initial olfactory properties of the solid consumer product (formulation) and allow for a facilitated processing and improved homogeneity by advantageously influencing the viscosity of the compositions according to the invention.
[0022] The present problem is solved by the objects of the independent patent claims. Preferred embodiments are apparent from the wording of the dependent patent claims as well as the following description.
[0023] All percentages are by weight unless otherwise indicated. Numeric examples given in the form "x to y" include the values given. When multiple preferred numeric ranges are specified in this format, all ranges created by combining the various endpoints are also included.
[0024] The terms "at least one" or "one or more" as used herein refers to 1 or more, for example 2, 3, 4, 5, 6, 7, 8, 9 or more.
[0025] The term "and/or" expresses that a linkage exists, or an alternative is provided.
Brief Description of Drawings
[0026] Figure 1 : Figure 1 shows the results of the sensory evaluation of the performance (i.e. the release properties) of different samples of powder detergent in dependence of the presence of a fragrance emulsifier (i.e. a free fragrance component).
[0027] Figure 2: Figure 2 shows the viscosity of different samples in dependence of the presence of a fragrance emulsifier (i.e. a free fragrance component).
[0028] Figure 3: Figure 3 shows the viscosity of different samples in dependence of the type of fragrance emulsifier (polymer matrix: PEG 6,000 g/mol).
[0029] Figure 4: Figure 4 shows the viscosity of different samples in dependence of the molecular weight of the polymer matrix (PEG 6,000 g/mol; PEG 8,000 g/mol; PEG 10,000 g/mol).
[0030] Figure 5: Figure 5 shows the results of the sensory evaluation of the performance (i.e. release properties) of different samples in powder detergent for different adhesion agents. [0031 ] Figure 6: Figure 6 shows different samples of compositions comprising or consisting of at least one pastille prepared according to the invention showing the influence of the microcapsule slurry content.
[0032] Figure 7: Figure 7 shows different samples of compositions comprising or consisting of at least one pastille prepared based on the invention showing the influence of the water content / plasticizer content (without microcapsules).
[0033] Figure 8: Figure 8 shows different samples of compositions comprising or consisting of at least one pastille prepared according to the invention showing the influence of the water content / plasticizer content (with microcapsules).
[0034] Figure 9: Figure 9 shows a picture of microcapsules and free fragrance oil in laundry soap.
[0035] Figure 10: Figure 10 shows a picture of microcapsules and free fragrance oil in PEG.
[0036] Figure 11 : Figure 11 shows the results of the sensory evaluation of the performance (i.e. the release properties) of a laundry soap according to the present invention.
Detailed Description of the Invention
[0037] Hereinafter, the present invention is described in more detail.
[0038] The compositions of the present invention comprise or consist of at least one pastille comprising an encapsulated active ingredient, preferably a fragrance (or a fragrance mixture), a polymer forming a polymer matrix, preferably polyethylene glycol, free fragrance (or a free fragrance mixture) and optionally at least one adhesion agent.
[0039] In a first aspect the present invention relates to a composition comprising or consisting of at least one pastille, wherein said pastille comprises or consists of:
(a) from 0.5% to 10% by weight based on the total weight of the pastille of at least one microcapsule encapsulating an active ingredient, wherein said active ingredient is preferably a fragrance or fragrance mixture;
(b) from 92% to 98% by weight based on the total weight of the pastille of a polymer, wherein the polymer is preferably polyethylene glycol (PEG); and (c) from 0.1% to 10% by weight of free fragrance or a free fragrance mixture (i.e. a free fragrance component), and preferably a hydrophobic fragrance or fragrance mixture (i.e. a hydrophobic free fragrance component); based on the total weight of the pastille.
[0040] Optionally, in a further preferred embodiment the pastille of the composition according to the first aspect further comprises or consists of:
(d) from 0.5% to 10% by weight (based on the total weight of the pastille) of at least one plasticizer, wherein said plasticizer is preferably water or polyethylene glycol; based on the total weight of the pastille.
[0041 ] In a second aspect the present invention relates to a composition comprising or consisting of at least one pastille, wherein said pastille comprises or consists of:
(a) from 0.5% to 10% by weight based on the total weight of the pastille of at least one microcapsule encapsulating an active ingredient, wherein said active ingredient is preferably a fragrance or a fragrance mixture;
(b) from 60% to 80% by weight based on the total weight of the pastille of at least one polymer, preferably polyethylene glycol;
(c) from 2% to 32% by weight of based on the total weight of the pastille at least one adhesion agent, wherein said adhesion agent is preferably selected from the group consisting of fatty acids, fatty alcohols, fatty acid esters or mixtures thereof, such as waxes; and
(d) from 0.1% to 10% by weight of free fragrance or free fragrance mixture; based on the total weight of the pastille.
[0042] According to a further preferred embodiment, the pastille of the composition according to the second aspect further optionally comprises or consists of:
(e) from 0.5% to 10% by weight based on the total weight of the pastille of at least one plasticizer, wherein said plasticizer is preferably water or polyethylene glycol; and/or
(f) from 0.1% to 10% by weight based on the total weight of the pastille of a structuring agent, wherein said structuring agent is preferably selected from the group consisting of esters, such as isopropyl myristate or other emulsifiers; based on the total weight of the pastille. [0043] Based on the above compositions an efficient buffer or bumper system was developed which efficiently combines short-term and long-term release properties, in particular perfuming properties, based on a combination of free and encapsulated fragrances for a wide range of products, in particular (solid) textile care products.
[0044] Preferably, the composition does not contain any inorganic or organic salts. These might negatively influence the viscosity and thus the processability and stability of the resulting pastilles.
[0045] Microcapsules and active ingredients, component (a):
[0046] The composition according to the present invention comprises at least one microcapsule encapsulating an active ingredient, wherein said at least one microcapsule is dispersed in a polymeric matrix.
[0047] In general, microcapsules are particles comprising a core and a wall material surrounding the core, wherein the core may be a solid, liquid or gaseous substance or substance mixture (and preferably at least one active substance) surrounded by a polymeric dense, permeable or semi-permeable wall material. The wall is usually formed by precipitation of the polymers upon emulsification and coacervation or interfacial polymerization. The core is also referred to as the inner phase. Other names used for the wall include outer phase, shell or coating. The shell wall can comprise one or more (different) layers and can comprise an additional coating with a coating substance. The diameter of the microcapsules typically varies in the range of 1 to 1 ,000 pm. The wall thickness is typically 0.5 pm to 150 pm but can be varied in the range of 5 ■ 10'9 m to 5 ■ 10'6 m. Typically loadings of 25 wt.-% to 95 wt.-% with core material, but also those of 1 wt.-% to 99 wt.-% are possible.
[0048] For example, hydrophobic active ingredients, such as single fragrances (also referred to as fragrant/odorous substances or fragrance substances), fragrance mixtures (also referred to as mixtures of fragrant/odorous substances or mixtures of fragrance substances or perfume oils), aroma substances or mixtures of aroma substances, can be easily incorporated into numerous and diverse application formulations through encapsulation.
[0049] Based on their properties, microcapsules are used in the printing industry, food industry (vitamins, flavours, plant extracts, enzymes, microorganisms), agricultural chemistry (fertilizers, pesticides), feed industry (minerals, vitamins, enzymes, drugs, microorganisms), pharmaceutical industry, detergent industry, and cosmetic industry, among others.
[0050] A variety of capsule wall or coating materials are known for the manufacture of microcapsules. The capsule wall can be made of either natural, semi-synthetic or synthetic materials. Natural shell materials include gum arabic, agar-agar, agarose, maltodextrins, alginic acid or its salts, e.g., sodium alginate or calcium alginate, fats and fatty acids, cetyl alcohol, collagen, chitosan, lecithins, gelatine, albumin, shellac, polysaccharides such as starch or dextran, polypeptides, protein hydrolysates, sucrose, and waxes. Semisynthetic capsule wall materials include chemically modified celluloses, especially cellulose esters, and cellulose ethers, e.g., cellulose acetate, ethyl cellulose, hydroxypropyl cellulose, hydroxypropyl methyl cellulose, and carboxymethyl cellulose, as well as starch derivatives, in particular starch ethers and starch esters. Synthetic shell materials are, for example, polymers such as polyacrylates, polyamides, polyvinyl alcohol or polyvinylpyrrolidone.
[0051 ] Depending on the type of capsule wall material and manufacturing process thereof, microcapsules with different properties in terms of diameter, size distribution, and physical and/or chemical properties are formed in each case.
[0052] The microcapsules according to component (a) of the composition according to the present invention can be any of those known to the person skilled in the art.
[0053] Preferably, the microcapsules used within the scope of the present invention are such microcapsules, wherein the shell of the at least one microcapsule comprises or consists of a shell material selected from the group consisting of: sol-gel polymer (e.g., silica), polysiloxane, polyacrylate, polyacrylamide, poly(acrylate-co-acrylamide), polyurea, polyurethane, polyamide, polypeptide, polysulfonate, polysaccharide, polyphenolic polymers, poly(melamine-formaldehyde), poly(resorcinol-formaldehyde), poly(urea-formaldehyde), poly(melamine-urea), or combinations thereof, and preferably selected from the group consisting of sol-gel polymer, polyacrylate, polyacrylamide, poly(acrylate-co-acrylamide), polyurea, polyurethane, polypeptide, polysaccharide, polyphenolic polymers, poly(melamine- formaldehyde), poly(resorcinol-formaldehyde), poly(urea-formaldehyde), or combinations thereof.
[0054] The compositions according to the present invention comprise at least one of said microcapsules, i.e. either a single of the above mentioned types of microcapsules is embedded in the polymer matrix of the invention, or two or more different microcapsules up to a plurality of microcapsules can be embedded in the polymer matrix. Thereby, all microcapsules can be of the same type, i.e. all microcapsules are for example poly(melamine-formaldehyde)-based, or some of the microcapsules of component (a) are for example poly(melamine-formaldehyde)- based and others are polyurea-based, i.e. component (a) can comprise or consist of a mixture of different types of microcapsules being based on different encapsulation materials/shell materials.
[0055] Moreover, the microcapsules used within the compositions according of the present invention can be loaded with different materials, such as with different active ingredients, i.e. the compositions according to the invention comprise different microcapsules differing in their core material.
[0056] According to a further preferred variant, the compositions according to the invention comprise different microcapsules both differing in their core material as well as their shell material.
[0057] Preferably, however, the microcapsules according to component (a) of the present invention are selected from the following group of capsule types consisting of: poly(melamine- formaldehyde)-based microcapsules and isocyanate-based microcapsules such as polyurea- based and/or polyurethane-based microcapsules and mixtures thereof and which are preferably biodegradable.
[0058] Biodegradable microcapsule-technologies are known to those skilled in the art and are particularly suitable within the context of the present invention in terms of environmental sustainability. Examples of such biodegradable microcapsules are some isocyanate-based microcapsules or polysaccharide-based microcapsules.
[0059] The biodegradation of the microcapsule slurry in the environment involves the biological breakdown of the polymeric shell as per the invention. Measurement of biological activity or decomposition of the shell material could be determined under different environments in soil, ocean water, or sludge notably under OECD guidelines. The OECD tests which can be used to determine the ready biodegradability of organic chemicals include the six test methods described in the OECD Test Guidelines No. 301 A-F: DOC Die-Away Test (TG 301 A), CO2 Evolution Test (TG 301 B), Modified MITI Test (I) (TG 301 C), Closed Bottle Test (TG 301 D), Modified OECD Screening Test (TG 301 E) and Manometric Respirometry Test (TG 301 F). More details can be found in the official OECD Guideline for the testing of chemicals: OECD (2006), Revised Introduction to the OECD Guidelines for Testing of Chemicals, Section 3, OECD Guidelines for the Testing of Chemicals, Section 3, OECD Publishing, Paris.
[0060] Within the context of the present invention a microcapsule is considered to be biodegradable if the requirements according to the OECD 301 F biodegradability standard are fulfilled (standardized OECD 301 F test procedure: manometric respirometry test). According to OECD 301 F, a microcapsule is considered readily biodegradable if more than 60% of the wall material has degraded after 28 days.
[0061 ] Consequently, in the composition according to the present invention, the at least one microcapsule is preferably biodegradable according to OECD 301 F.
[0062] In the context of the present invention, microcapsules are understood to be microparticles comprising at least one or more active ingredient(s) as core material inside the capsule and which are enclosed by a capsule shell or capsule wall as specified above. As active ingredient to be encapsulated according to the invention, basically any material suitable for inclusion in microcapsules can be considered in the process according to the invention. Preferably, hydrophobic or lipophilic, i.e. , water-insoluble, or water-immiscible liquids or solids as well as suspensions can be considered as active ingredients to be encapsulated. These are predominantly non-polar substances. Such hydrophobic substances are almost always lipophilic, i.e., they dissolve well in fat and oil.
[0063] The terms "microcapsule" and "capsule" or "hydrophobic" and “lipophilic" are used synonymously within the context of the present invention.
[0064] In the context of the present description, the core material is preferably a hydrophobic active substance, i.e., a substance that has a specific effect or causes a specific reaction, for example, a drug, a pesticide, a cosmetic active ingredient, a food active ingredient, etc.
[0065] Preferably, the at least one lipophilic or hydrophobic active ingredient or substance is a single lipophilic or hydrophobic fragrance substance or aroma substance or a lipophilic or hydrophobic perfume oil or aroma (i.e. a mixture of two or more fragrance substances or of two or more aroma substances, respectively), a cooling agent, a TRPV1 or a TRPV3 modulator, a substance that produces a pungent taste or a warmth or heat sensation on the skin or mucous membranes or a tingling sensation in the mouth or throat, or active ingredients with astringent effect, a pesticide, a biocide, an insecticide, a substance from the group of repellents, a food additive, a cosmetic active ingredient, a pharmaceutical active ingredient, a dye, a dye precursor; an agrochemical, a dye, a luminous paint, an optical brightener, a solvent, a wax, a silicone oil, a lubricant, a print coating for paper, or a mixture of two or more of the aforementioned active ingredients.
[0066] In a preferred embodiment according to the present invention, the microcapsules have a core material comprising or consisting of a hydrophobic single fragrant substance or single odorant substance or a mixture of two or more such substances, i.e. wherein the core material comprises at least one single fragrant substance or single odorant substance or mixtures thereof (i.e. a perfume oil), selected from one or more of the following groups:
Extracts of natural raw materials and also fractions thereof or components isolated therefrom; single fragrance substances from a group of hydrocarbons; aliphatic alcohols; aliphatic aldehydes and acetals; aliphatic ketones and oximes; aliphatic sulfur-containing compounds; aliphatic nitriles; esters of aliphatic carboxylic acids; formates, acetates, propionates, isobutyrates, butyrates, isovalerates, pentanoates, hexanoates, crotonates, tiglinates and 3- methyl-2-butenoates of acyclic terpene alcohols; acyclic terpene aldehydes and ketones as well as their dimethyl and diethyl acetals; formates, acetates, propionates, isobutyrates, butyrates, isovalerates, pentanoates, hexanoates, crotonates, tiglinates and 3-methyl-2- butenoates of cyclic terpene alcohols; cyclic terpene aldehydes and ketones; cyclic alcohols; cyclic and cycloaliphatic ethers; cyclic and macrocyclic ketones; cycloaliphatic aldehydes; cycloaliphatic ketones; esters of cyclic alcohols; esters of cycloaliphatic carboxylic acids; aromatic hydrocarbons; araliphatic alcohols; esters of araliphatic alcohols and aliphatic carboxylic acids; araliphatic ethers; aromatic and araliphatic aldehydes; aromatic and araliphatic ketones; aromatic and araliphatic carboxylic acids and their esters; nitrogencontaining aromatic compounds; phenyl ethers and phenyl esters; heterocyclic compounds; lactones; and mixtures of the above active ingredients.
[0067] The terms "fragrance" and "fragrant substance" or "fragrance substance" or “odorant (substance)” or “odorous substance” are used synonymously within the context of the present invention.
[0068] Specific examples of the abovementioned substances are known to the person skilled in the art. Fragrant substances or odorant substances and mixtures of two or more of said substances are chemical substances or compositions which are used to confer, impart and/or modulate a specific odour or odour impression. Preferably, said odour (impression) is considered as being pleasant.
[0069] In an alternative embodiment according to the present invention, the microcapsules according to the invention use a fragrance substance or a perfume oil, respectively, or an aroma substance or an aroma as the active ingredient to be encapsulated or as the core material. These are compositions containing at least one fragrance substance or at least one aroma substance. Such compositions, in particular mixtures of fragrance substances or perfume oils, preferably comprise two, three, four, five, six, seven, eight, nine, ten or more fragrance substances. The fragrance mixtures or perfume oils, respectively, are preferably selected from the group consisting of: extracts from natural raw materials, such as essential oils, concretes, absolutes, resins, resinoids, balsams, tinctures such as e.g., Ambergris oil; Amyris oil; Angelica seed oil; Angelica root oil; Anise oil; Valerian oil; Basil oil; Tree moss absolute; Bay oil; Mugwort oil; Benzoin resin; Bergamot oil; Beeswax absolute; Birch tar oil; Bitter almond oil; Savory oil; Bucco leaf oil; Cabreuva oil; Cade oil; Calmus oil; Camphor oil; Cananga oil; Cardamom oil; Cascarilla oil; Cassia oil; Cassie absolute; Castoreum absolute; Cedar leaf oil; Cedarwood oil; Cistus oil; Citronella oil; Citron oil; Copaiva balsam; Copaiva balsam oil; Coriander oil; Costus root oil; Cumin oil; Cypress oil; Davana oil; Dill herb oil; Dill seed oil; Eau de brouts absolute; Oak moss absolute; Elemi oil; Tarragon oil; Eucalyptus citriodora oil; Eucalyptus oil; Fennel oil; Spruce needle oil; Galbanum oil; Galbanum resin; Geranium oil; Grapefruit oil; Guaiac wood oil; Gurjun balsam; Gurjun balsam oil, Helichrysum absolute; Helichrysum oil; Ginger oil; Iris root absolute; Iris root oil; Jasmine absolute; Calamus oil; Chamomile oil blue; Chamomile oil Roman; Carrot seed oil; Cascarilla oil; Pine needle oil; Curly mint oil; Caraway seed oil; Labdanum oil; Labdanum absolute; Labdanum resin; Lavandin absolute; Lavandin oil; Lavender absolute; Lavender oil; Lemongrass oil; Lovage oil; Lime oil distilled; Lime oil pressed; Linal oil; Litsea cubeba oil; Bay leaf oil; Macis oil; Marjoram oil; Mandarin oil; Masso bark oil; Mimosa absolute; Musk grain oil; Musk tincture; Muscat sage oil; Muscat oil; Myrrh absolute; Myrrh oil; Myrtle oil; Clove leaf oil; Clove flower oil; Neroli oil; Olibanum absolute; Olibanum oil; Opopanax oil; Orange flower absolute; Orange oil; Origanum oil; Palmarosa oil; Patchouli oil; Perilla oil; Perubalsam oil; Parsley leaf oil; Parsley seed oil; Petitgrain oil; Peppermint oil; Pepper oil; Pimento oil; Pine oil; Poley oil; Rose absolute; Rosewood oil; Rose oil; Rosemary oil; Sage oil Dalmatian; Sage oil Spanish; Sandalwood oil; Celery seed oil; Spicy lavender oil; Star anise oil; Styrax oil; Tagetes oil; Fir needle oil; Tea tree oil; Turpentine oil; Thyme oil; Tolu balsam; Tonka absolute; Tuberose absolute; Vanilla extract; Violet leaf absolute; Verbena oil; Vetiver oil; Juniper berry oil; Wine yeast oil; Wormwood oil; Wintergreen oil; Ylang oil; Hyssop oil; Civet absolute; Cinnamon leaf oil; Cinnamon bark oil; and fractions thereof or ingredients isolated therefrom, as well as mixtures of the aforementioned substances.
[0070] In a further variant of the invention aroma substances can also be encapsulated as a core material, wherein the core material comprises at least one single aroma substance or mixtures of two or more different aroma substances as active ingredient.
[0071 ] However, preferably a single fragrant substance or odorous substance (i.e. , chemical compounds having a smell or odour and thus all natural and synthetic substances that impart an olfactorily perceptible odour) or alternatively a mixture of fragrant substances or odorous substances (so-called perfume oil) is used as the active ingredient enclosed by the microcapsule shell. More preferably, said substances and mixtures of substances are imparting a pleasant odour to a consumer product.
[0072] In a preferred variant of the present invention, all microcapsules of component (a) are loaded with the same active ingredient(s), for example all of the microcapsules are comprising a fragrance substance and even more preferred the same fragrance substance.
[0073] According to an alternative embodiment, the microcapsules according to component (a) of the invention are encapsulating different classes of active ingredients or different substances among the same class of active ingredients. For example, some of the microcapsule comprise a specific fragrance substance while other microcapsules enclose another fragrance substance.
[0074] Thereby, preferably the core material is selected irrespective of the shell material.
[0075] Thus, according to a further preferred variant of the present invention, the pastilles of the present invention can comprise one type of microcapsules or a mixture of two or more different types of microcapsules. Thereby, the microcapsules can vary in terms of the active ingredient composition (i.e. the microcapsule core) and/or the wall composition (i.e. the material of the capsule shell).
[0076] According to the invention, the compositions comprise at least one microcapsule dispersed within the polymer component (b), which is preferably a water-soluble polymer matrix. [0077] Between 0.5% by weight to 10% by weight of microcapsules can be incorporated into the final composition based on the total weight of the pastille, i.e. a single pastille of the composition according to the present invention comprises between 0.5% by weight to 10% by weight of microcapsule(s) as specified above. If the amount of the microcapsule component (a) is kept within these ranges, a homogeneous distribution of the microcapsules within the pastille(s) can be achieved. Moreover, if the amount of component (a) is within the above ranges the active ingredients can efficiently be incorporated into the final solid consumer product formulation due to an efficient protection by the surrounding polymeric matrix, i.e. the microcapsules do not break open during the preparation process of the solid consumer product and thus can effectively retain the encapsulated active ingredient(s) without loss, resulting in a significantly improved microcapsule performance as shown in the experimental section.
[0078] Thus, according to a preferred embodiment, the amount of the microcapsule(s) ranges from 0.5% by weight to 10% by weight based on the total weight of the pastille and even more preferred from 3% by weight to 8% by weight based on the total weight of the pastille.
[0079] According to the present invention, the at least one microcapsule encapsulating an active ingredient is dispersed in a polymer matrix (or polymeric matrix).
[0080] Thereby, the inventive compositions comprising the microcapsules encapsulating the active ingredient(s) can be efficiently incorporated into a variety of solid consumer product formulations allowing for an efficient and targeted release of the active ingredient(s). Thereby the surrounding polymeric matrix acts as kind of a shock absorbing layer protecting the microcapsules from damage due to mechanical, chemical and/or thermal influences and thus premature release and degradation of the active ingredient(s) during the preparation process of the consumer product.
[0081 ] Polymer or polymer matrix, component (b):
[0082] As specified above, the compositions/pastilles according to the present invention comprise or consist of from 92% to 98% by weight or from 60% to 80% by weight (based on the total weight of a pastille), respectively, of at least one polymer.
[0083] Suitable polymers according to the present invention are meltable polymers, such as for example polyethylene glycol (“PEG”) having a molecular weight from about 3,000 Da to 20,000 Da, preferably from about 4,000 Da to 12,000 Da, and even more preferred from about 5,000 Da to 8,000 Da.
[0084] Component (b) can comprise either one specific polymer having a molecular weight within the ranges specified above, or two or more different polymers. Said different polymers can be either the same substance differing in their molecular weight within the specified ranges (such as PEG 3,000 and PEG 4,000) or can be different chemical substances having either the same or different molecular weights.
[0085] If the molecular weight of the polymer used as component (b) is within the ranges specified above, an efficient protection of the fragile microcapsules can be achieved allowing for an efficient incorporation in solid consumer product formulations which simultaneously allows for an efficient targeted release of the active ingredient(s).
[0086] The polymeric matrix protects the microcapsules towards chemical and mechanical influences while allowing for high release performances. Said protection allows an efficient incorporation of the loaded microcapsules into a broad range of consumer product formulations and in particular solid consumer product formulations. In the manufacture of such compositions the fragile microcapsules are subject to high shearing which causes a breakage of the microcapsules and thus a premature release of the active ingredients. It was surprisingly found that the compositions according to the present invention can be advantageously incorporated into such formulations thereby showing improved performances and chemical and mechanicals stabilities within these formulations, during their manufacture and towards the other ingredients.
[0087] In the context of the present invention, a “meltable” polymer is a plastic polymer material that becomes pliable or moldable at a certain elevated temperature and solidifies upon cooling.
[0088] The polymer used within the context of the present invention can be either a water- soluble or a water-insoluble polymer. According to an alternative embodiment component (b) comprises a mixture of one or more water-soluble polymers, a mixture of one or more waterinsoluble polymers, or a mixture of one or more water-soluble polymers and one or more waterinsoluble polymers. [0089] In a preferred variant of the present invention the melting point of the polymer according to the present invention (preferably having a molecular weight from about 3,000 Da to 20,000 Da) is preferably in the range from 25 °C to 100 °C, and preferably from 40 °C to 80 °C.
[0090] Preferably however, the polymer used in the context of the present invention as component (b) is water-soluble. For example, when incorporated in textile care formulations, such as powder detergents, the polymeric protecting matrix will be dissolved thereby releasing the microcapsules which thus can be efficiently applied to the textile. This has the additional advantage, that the microcapsules will not be destroyed upon storing, processing, product preparation and the like, thereby preventing a premature release of the active ingredient(s). The water-soluble polymeric matrix will dissolve during the washing process and efficiently release the encapsulated fragrance components as well as the free, i.e. unencapsulated, fragrance component(s) without leaving an unacceptable residue on the fabric being treated.
[0091 ] Examples of suitable water-soluble polymers are for example polyvinyl alcohol, derivatives of polyvinyl alcohol (such as quaternary amine derivatives), polyethylene glycol (of varying molecular weight), polyvinyl pyrrolidone, (poly)acrylates, polyacrylic acid, acrylamides, polyamino acids and amine-functional polymers, saccharides and polysaccharides such as starch, modified starch, maltodextrins, carbohydrates, chitosan, and gum arabic, maleic anhydride copolymers, vinyl acids and ethers, styrenes, polystyrene sulfonates, ethylene glycol-propylene glycol block copolymers and mixtures thereof. Examples of suitable waterinsoluble polymers include amongst others classical capsules with coating, waxes such as beeswax, sunflower seed wax, rice bran wax, carnauba wax, pinova wax, rapeseed wax, soywax, candelilla wax, jojoba oil, cork wax, guaruma wax, cotton wax, foxwax, peat wax, rose wax, jasmine wax, peetha-wax from wax gourd, myrtle wax (Myrica cerifera), wax fig wax, berry wax and mixtures of different waxes.
[0092] In a preferred embodiment according to the present invention, the polymer is preferably polyethylene glycol (PEG, also known as polyethylene oxide (PEG) or polyoxyethylene (POE)) having a molecular weight from about 3,000 Da to 20,000 Da, preferably from about 3,000 Da to 12,000 Da, and even more preferred from about 4,000 Da to 9,000 Da.
[0093] According to an alternative preferred embodiment component (b) comprises a mixture of two or more polyethylene glycols differing in their molecular weight. [0094] Polyethylene glycol is a cheap, synthetic, hydrophilic, biocompatible polymer with widespread use in biomedical and other applications such as in pharmaceutical compositions as excipient or as laxative, in the chemical industry e.g. as lubricating coating, and in cosmetic formulations as a basis for creams or as dispersant. Polyethylene glycol is a flexible, water- soluble polymer having a low toxicity which can be incorporated into a broad variety of formulations and having the general formula: C2nH4n+2On+i.
[0095] The compositions of the present invention according to the first aspect may comprise from 91% to 98% by weight based on the total weight of a pastille of the polymer (component (b)), preferably from 92% to 98% by weight, and even more preferred from 92% to 96% by weight of the pastille.
[0096] Lower amounts of the polymer component implicitly mean higher amounts of the microcapsule component. As the microcapsule component is preferably added in the form of an aqueous slurry, the increased amount of water will result in the composition getting softer and stickier thereby rendering the preparation of pastilles more challenging (see Figures 6 and 7).
[0097] The compositions of the present invention according to the second aspect may comprise from 60% to 80% by weight based on the total weight of a pastille of the polymer (component (b)), preferably from 65% to 75% by weight, and even more preferred from 70% to 75% by weight of the pastille.
[0098] It was further found that lower contents of the polymer component (i.e. below 60% by weight based on the total weight of a pastille) result in a decreased water solubility e.g. of the pastilles in a solid detergent formulation. In this case the intended effect is not achieved anymore and the composition according to the present invention does not show the intended release performance. On the other hand, if the content of the polymer component is too high, i.e. above 80% by weight based on the total weight of a pastille, the composition gets to hard thereby rendering the pastillation process more difficult.
[0099] If the polymer specified above is comprised within said ranges in the compositions according to the present invention an efficient protection of the fragile microcapsules within said polymeric matrix can be achieved while simultaneously allowing for an efficient targeted release of the active ingredients. [0100] According to another preferred variant of the present invention the polymer(s) exhibit(s) a specific solidification point: The minimum solidification point of the water-soluble polymer-like particles, i.e. the final pastilles, is preferably above 0 °C, preferably above 20 °C, and particularly preferably above 35 °C, while the minimum solidification point of the non- water-soluble polymer-like particles is at above 0 °C, preferably above 20 °C, and particularly preferably above 35 °C. Solidification points within said ranges allow a facilitated formation of the pastilles according to the present invention, without requiring low temperatures for the pastille preparation process and their subsequent processing.
[0101 ] According to the present invention and a preferred embodiment, no additional solid carrier is required in order to incorporate the compositions according to the present invention into product formulations. Thereby, it is possible to further reduce the overall amount of ingredients and waste products without negatively influencing the intended efficacy.
[0102] Adhesion agent:
[0103] Interestingly it was further found that a combination of a polymer as specified above with an additional adhesion agent as specified herein likewise results in an efficient protection of the microcapsules upon incorporation into solid consumer product formulations.
[0104] Thus, in a second aspect the present invention relates to a composition comprising or consisting of a microcapsule component (component (a)), a polymer component (component (b)); an adhesion agent component (component (c)) and a free fragrance component (component (d)) in specific ratios. Thereby the components (b) and (c) are forming the protective matrix surrounding, i.e. embedding the fragile microcapsules.
[0105] An adhesion agent according to the present invention is defined as a substance allowing for an increased adhesion of the microcapsules on external materials and their surfaces such as textiles (adhesion promoter or deposition aid). The adhesion is based on mechanical bonding, hydrogen bonding, chemical or covalent bonding, thermodynamic bonding, etc.
[0106] Preferably the adhesion agent used as component (c) according to the second aspect of the present invention is a substance selected from the group consisting of fatty acids, fatty alcohols, fatty acid esters or mixtures thereof, such as natural and synthetic waxes. Thereby the composition according to the second aspect of the present invention can comprise one or a mixture of two or more of such adhesion agents as component (c).
[0107] Further suitable adhesion agents are for example:
Long-chain, aliphatic, linear or branched, saturated or unsaturated carboxylic acids with 12 to 30 carbon atoms (fatty acids), in particular lauric acid (12:0), tridecanoic acid (13:0), myristic acid (14:0), pentadecanoic acid (15:0), palmitic acid (16:0), margaric acid (17:0), stearic acid (18:0), nonadecanoic acid (19:0), arachidic acid (20:0), heneicosanoic acid (21 :0), behenic acid (22:0), lignoceric acid (24:0), cerotinic acid (26:0), montanic acid (28:0), and melissic acid (30:0); myristoleic acid (14:1), palmitoleic acid (16:1), margaroleic acid (17: 1), petroselinic acid (18:1), oleic acid (18:1), elaidic acid (18:1), vaccenic acid (18:1), gadoleic acid (20:1), gondoic acid (20:1), cetoleic acid (22:1), erucic acid 822:1), nervonic acid (24:1), linoleic acid (18:2), alpha-linolenic acid (18:3), gamma-linolenic acid (18:3), calendulic acid (18:3), punicic acid (18:3), alpha-eloeostearic acid (18:3), beta-eloeostearic acid (18:3), stearidonic acid (18: 4), arachidonic acid (20:4), eicosapentaenoic acid (20:5), docosatetraenoic acid (ADA) (22:4), docosapentaenoic acid (DPA-3) (22:5), docosahexaenoic acid (22:6), and tetracosahexaenoic acid (24:6), phytanic acid;
Long-chain, aliphatic, linear or branched, saturated or unsaturated primary alcohols with 12 to 30 carbon atoms (fatty alcohols), in particular lauryl alcohol (12:0), myristyl alcohol (14:0), palmityl alcohol (16:0), margaryl alcohol (17:0), stearyl alcohol (18: 0), arachidyl alcohol (20:0), behenyl alcohol (22:0), lignoceryl alcohol (24:0), ceryl alcohol (26:0), montanyl alcohol (28:0), and melissyl alcohol (30: 0); palmitoleyl alcohol (16:1), oleyl alcohol (18:1), elaedyl alcohol (18:1), linoleyl alcohol (18:2), gamma-linolenyl alcohol (18:3);
Esters of long-chain, aliphatic saturated carboxylic acids containing 12 to 30 carbon atoms with long-chain, aliphatic primary alcohols containing 12 to 30 carbon atoms, in particular lauryl palmitate, myricyl palmitate, cetylarachinate and stearyl behenate;
Animal and vegetable waxes, in particular beeswax, wool wax, China wax, rice bran wax, sunflower seed wax, rice bran wax, carnauba wax, sugarcane wax, pinova wax, rapeseed wax, soy wax, candelilla wax, jojoba oil, cork wax, guaruma wax, ouricury wax (Syagrus coronata), Cuba palm wax (Copernicia hospita), esparto wax (Lygeum spartum, Stipa tenacissima), cotton wax, flax wax, peat wax, rose wax, jasmine wax, peetha wax from wash gourd, and also myrtle wax (Myrica cerifera), wax fig wax, berry wax. as well as mixtures of two or more of the aforementioned adhesion agents.
[0108] Of the carboxylic acids listed above, the saturated fatty acids are particularly preferred. Most preferred in the context of the invention is the use of the animal and vegetable waxes as specified above due to their lower melting points, which facilitate their incorporation into the composition.
[0109] According to another preferred embodiment, the at least one adhesion agent is selected from the group consisting of animal and/or vegetable waxes, and is preferably (natural) beeswax.
[01 10] In another preferred variant the at least one agent is selected from animal and/or vegetable waxes and is preferably selected from the group consisting of beeswax, wool wax, China wax, rice bran wax, sunflower seed wax, rice bran wax, carnauba wax, sugarcane wax, pinova wax, rapeseed wax, soy wax, candelilla wax, jojoba oil, cork wax, guaruma wax, ouricury wax (Syagrus coronata), Cuba palm wax (Copernicia hospita), esparto wax (Lygeum spartum, Stipa tenacissima), cotton wax, flax wax, peat wax, rose wax, jasmine wax, peetha wax from wash gourd, and also myrtle wax (Myrica cerifera), wax fig wax, berry wax, and mixtures thereof.
[01 11 ] In addition, it was surprisingly found that adhesion agents as specified herein such as animal and/or vegetable waxes positively influence the performance of the pastilles, i.e. the pastilles comprising animal and/or vegetable waxes show improved protective properties in view of the microcapsules embedded therein as well as improved release properties allowing for a more efficient protection as well as targeted release of the active ingredients.
[01 12] Moreover, it was found that adhesion agents as specified herein, and particularly animal and/or vegetable waxes, positively influence the initial odour impression of formulations comprising fragrant active components.
[01 13] Surprisingly, it was found that such natural or synthetic animal and/or vegetable waxes can be efficiently incorporated into the composition according to the second aspect. Moreover, these substances allow for an improved adhesion of the microcapsules onto the surface of other materials such as textile fibres and simultaneously support the protecting effect of the polymeric matrix thus showing multiple advantages. In other words, the adhesion agents as specified herein not only improve the adhesion of the active ingredients to the respective surfaces but simultaneously improve the protection of the fragile microcapsules and even allow for an improved performance.
[01 14] According to a further preferred embodiment, the at least one adhesion agent is a vegetable wax, i.e. a wax of plant origin.
[01 15] Alternatively, according to another further preferred embodiment, the at least one adhesion agent is an animal wax, such as beeswax or lanolin (wax obtained from wool).
[01 16] Additionally, it was observed, that the combination of the polymer (e.g. polyethylene glycol) with an adhesion agent as specified herein (e.g. beeswax) results in a considerable performance improvement compared to compositions comprising a pure polyethylene glycol matrix, indicating an improved shock absorbing and protective effect. The use of microcapsules embedded in a polymer-adhesion agent-matrix result in an even more improved performance of the consumer product.
[01 17] In addition, it was found that a comparison of the samples with and without an additional adhesion agent shows that the addition of an adhesion agent not only improves the manufacturing and preparation of more homogeneous pastilles but also results in an improvement of the sensory experience by allowing for a more efficient protection of the fragile microcapsules and thus a more targeted fragrance release. Accordingly, based on their sensory enhancing properties, it was found that the adhesion agents additionally can act as "scent booster”.
[01 18] It was found that the addition of an adhesion agent as specified herein can improve the release performance/sensory performance and thus the sensory experience by one unit, i.e. by more than 10% in intensity/efficacy. Accordingly, the adhesion agents as used herein also be considered as “sensory boosters” or “scent boosters”.
[01 19] It was further found that different types of waxes can suitably be used as such adhesion agents.
[0120] Thereby biobased or bio-derived reagents are preferred in view of health and environmental aspects. Biobased materials (bio-derived materials) refer to compounds containing organic carbon of renewable origin such as from agricultural, plant, animal, fungi, microorganism, marine or forestry materials living in a natural environment in equilibrium with the atmosphere, being of non-fossil origin such as petroleum as defined according to the ASTM D6866 standard test. Further it is defined that such biogenic compounds are compounds containing carbon (organic and inorganic) of renewable origin like agricultural, plant, animal, fungi, microorganisms, microorganisms, marine, or forestry materials. Preferably, the inventive compositions comprise such biogenic or biobased, i.e., bio-derived materials. Therefore, bioderived materials are preferably used for the preparation of pastilles and thus compositions according to the invention.
[0121 ] Thus, in a further preferred variant of the present invention preferably, the at least one adhesion agent is selected from the group of bio-based materials such as naturally occurring animal and/or vegetable waxes.
[0122] According to an alternative preferred variant, the at least one adhesion agent is paraffin wax.
[0123] The adhesion agent component is incorporated into the polymeric matrix.
[0124] Preferably the adhesion agent used as component (c) according to the second aspect of the present invention is comprised in an amount of from 2% to 32% by weight based on the total weight of the pastille, preferably from 3% to 20% by weight, and more preferred from 4% to 17% by weight, and most preferred from 5% to 10% by weight of the pastille.
[0125] The addition of the adhesion agent(s) within said ranges allows for an improved balance between microcapsule protection and adhesion promotion as well as scent boost.
[0126] Furthermore, it was found that a further improved balance between microcapsule protection and release properties could be achieved if the density of the polymer matrix (preferably the PEG matrix) ranges from 0.95 g/cm3 to 1.10 g/cm3 and preferably from 0.99 g/cm3 to 1 .05 g/cm3. Moreover, if the density is within the above ranges, it was found that the homogeneity of the pastilles according to the invention is improved and that the preparation of the pastilles according to the invention is further facilitated.
[0127] The density was determined as bulk density which is defined as the mass of particles per volume, of a mixture of the solid bulk material and a continuous fluid / solvent which fills the cavities between the particles. [0128] As explained above, lower amounts of the polymer component implicitly mean higher amounts of the microcapsule component. As the microcapsule component is preferably added in the form of an aqueous slurry, the increased amount of water will result in the composition getting softer and stickier thereby rendering the preparation of pastilles more challenging (see Figures 6 and 7). This effect can surprisingly be partially compensated by adding an adhesion agent as specified herein. However, it is preferred that the overall amount of the adhesion agent is kept low, and preferably below 10% by weight of the pastille in order to avoid potential disadvantages such as the formation of stains on textiles caused by the water-insoluble adhesion agent component (such as a wax) e.g. during the textile washing process.
[0129] Free fragrance or unencapsulated fragrance (fragrance emulsifier):
[0130] According to the invention, the compositions further comprise free fragrance(s). The term “free fragrance” refers to either a single fragrance substance or a mixture of two or more fragrance substances which are dispersed within the polymeric matrix in unencapsulated (or non-encapsulated) form, i.e. this fragrance component is not present in the form of discrete microcapsules.
[0131 ] The compositions according to the present invention additionally necessarily comprise a single free fragrance substance or a mixture two or more fragrance substances (i.e. a free fragrance mixture or free perfume oil), i.e. the compositions according to the present invention additionally comprise at least one unencapsulated or free fragrance substance as additional component. The sensory data shows that the addition of a free oil / free fragrance component provides a better odour impression.
[0132] Thereby, the olfactory performance can be further increased, and the final product as well as the freshly treated textile immediately shows perceivable olfactory performance. A rupture of the microcapsules adds additional intense scent in the case of encapsulated fragrance(s).
[0133] Preferably, the free fragrance substance or the free fragrance mixture (mixture of two or more fragrance substances) is comprised in amounts of 0.1% by weight to 10% by weight based on the total weight of the pastille, and preferably in amounts of 2% by weight to 8% by weight and further preferred in amounts of 2% by weight to 5% by weight. [0134] Suitable fragrance substances and mixtures thereof are described above in the context of microencapsulation.
[0135] In case that the encapsulated active ingredient is a fragrance or mixture of fragrance substances, then the free fragrance component (either a single free fragrance substance or a mixture of two or more fragrance substances) can either be the same or different compared to the encapsulated fragrance component in terms of amount and/or chemical composition.
[0136] Said free fragrance component serves as emulsifier (“fragrance emulsifier”) and further facilitates the preparation of the pastilles according to the invention in a more homogenous manner while simultaneously adding olfactory benefits.
[0137] It was surprisingly found that the presence of a free fragrance component dispersed within the polymer matrix results in further improved release properties (Figure 1). Moreover, it was possible to achieve a comparably high initial scent experience, i.e. before mechanically rupturing the microcapsules and thereby releasing the encapsulated fragrances (Figure 1). The scent experience achieved by compositions according to the present invention is thus (i) prolonged and present from the onset (i.e. directly after the treatment), and (ii) intensified and more homogeneous over time.
[0138] Surprisingly, the comprised free fragrance component further improves the final product properties allowing for an efficient adjustment of the viscosity and flexibility of the polymeric matrix resulting in a less brittle and more flexible matrix with improved buffering effect and thus better protection of the fragile microcapsules and a facilitated incorporation into solid consumer product formulations without altering the fundamental chemical character of the plasticized material (see Figures 1 to 4).
[0139] Additionally, it was surprisingly found that the free fragrance component facilitates the pastille formation and significantly improves the miscibility of the microcapsule component and the polymer component and further optional components or additives thereby allowing for achieving a more homogeneous distribution of the microcapsules (and thus the active ingredients) within the polymeric matrix. The presence of free fragrance(s) surprisingly reduces the compositions viscosity and thus positively influences the properties of the composition by allowing a more homogeneous distribution of the pastille components. In addition, the processability is facilitated. This allows for the preparation of more stable pastilles with improved release properties. For fragrance microcapsules an improved and more homogeneous scent release was observed when combined with free fragrance(s). Additionally, the compositions according to the present invention allow for an instantly perceivable scent experience.
[0140] Even more surprising, it was found that the above-mentioned advantageous effects cannot be achieved by merely using a common plasticizer and/or structuring agent such as isopropyl myristate, which is no fragrance substance.
[0141 ] These advantageous effects mentioned above could be observed for a broad range of fragrance substances and mixtures thereof, not being limited to specific chemical classes of fragrance substances.
[0142] However, particularly good results were achieved for fragrance substances such as Agrumex LC, Agrunitril, Aldehyd C10, Aldehyd C12 Laurin, Aldehyd C12 MNA, Aldehyd C14 sog., Allylcapronat, Amarocit, Ambrocenide, Amylsalicylat, Benzalydehyd, Benzylacetat, Benzylaceton, Benzylsalicylat, Borneol/lsoborneol 65:35, Bourgeonal, Citronellol 950, Clonal, CM20 Sanjinol Replacer, Coniferan, Cumarin, Cyclamenaldehyd, Cyclohexylsalicylat, Damascenon, Damascene Delta, Decenol, Dihydromrycenol, Dimethylbenzylcarbinol, Dimethylbenzylcarbinylacetat, Diphenyloxid, Dipropylenglycol, Dynascone, Ethylcaprinat, Eucalyptusoil, Eugenol, Florazon, Florosa BM/Pyranol, Geraniol Supra, Geranylacetat 60, Hexylacetat, Hexylsalicylat, Hexylzimtaldehyd alpha, Isobornylacetat, Isooctanon, Isodralein 70, Kresolmethylether para, Labienoxime, Lemonile, Lilial, Linalool, Linaylacetat, Manzanate, Melonaol, Methyloctincarbonat, Mugenal, Mugetaoil, Orangeoil, Patchoulioil, Peonile, Phenylethylacetat, Phenylethylalkohol, Phenylethylmethylether, Pinoacetataldehyd, Rosenoxid High Cis, Stemone, Stryolacetat, Tamarine Type Base BHT Free, Terpineol Rein, Timbersilk, Undecanon-2, Undecavertol, Vertofix, Vertroprenal, Ylang Colipa Base and mixtures thereof.
[0143] Further particularly suitable fragrance substances are selected from the group of hydrocarbons such as Caren Delta-nat, Caryophyllen nat. rekt., Pinen alpha laevo nat., Terpinen Gamma and mixtures thereof.
[0144] Further suitable free fragrance substances are selected from the group consisting of esters such as Benzylbutyrat and/or aldehydes such Aldehyde C10 and mixtures thereof (Figures 3 and 4). [0145] Plasticizer:
[0146] The compositions according to the invention can further comprise a certain amount of at least one plasticizer as additive. Thereby the compositions according to the present invention can comprise one single plasticizer or a mixture of two or more of such plasticizers.
[0147] A plasticizer is a substance that is used to increase the flexibility and plasticity of a specific substance or composition and can additionally decrease the viscosity as well as the friction of a substance or composition.
[0148] Suitable plasticizers are known to the person skilled in the art. Suitable plasticizers are for example water, polyethylene glycol, ortho phthalates, phthalate esters, trimellitates and esters thereof, (organo)phosphates, aliphatic dibasic acid esters, benzoate esters, polyesters, citrates, bioderived plasticizers based on epoxidized soybean oil, epoxidized linseed oil, castor oil, palm oil, other vegetable oils, starches, sugars and the like, chlorinated paraffins, alkyl sulfonic acid esters, dicarbonates, fatty acid esters.
[0149] Preferably the plasticizer(s) is/are selected from amongst others water or polyethylene glycol. The plasticizer water can origin for example from the manufacture process of the pastilles or can be added subsequently.
[0150] According to a preferred variant the plasticizer, and preferably the plasticizer water, is provided through the addition of an aqueous microcapsule slurry (component (a)), i.e. wherein the aqueous phase of the microcapsule slurry is serving as plasticizer.
[0151 ] According to an alternative preferred variant polyethylene glycol is used as the plasticizer component. Preferably, in this case, the molecular weight of the plasticizer polyethylene glycol is below 4,000 Da, further preferred below 3,500 Da and most preferred below 3,000 Da.
[0152] Preferably the plasticizer(s) used as additive(s) according to the present invention is/are comprised in an amount of from 0.5% to 10% by weight based on the total weight of the pastille, preferably from 2% to 8% by weight, and more preferred from 3% to 6% by weight.
[0153] The addition of the plasticizer(s) within said ranges allows for efficiently adjusting the viscosity and flexibility of the polymeric matrix resulting in a less brittle and more flexible matrix with improved buffering effect and thus better protection of the fragile microcapsules and a facilitated incorporation into solid consumer product formulations without altering the fundamental chemical character of the plasticized material.
[0154] Structuring agent:
[0155] Additionally, or alternatively, it is possible to add one or more structuring agents to the compositions according to the present invention as specified above as additional component or additive. Thereby the composition according to the present invention can comprise one single structuring agent or a mixture of two or more of such structuring agents.
[0156] Thus, according to a further preferred embodiment the composition according to the first and second aspect of the present invention includes at least a surfactant.
[0157] Said structuring agent(s) is/are preferably comprised in an amount ranging from 0.1 % to 10% by weight based on the total weight of a pastille, preferably from 1% to 8% by weight and even more preferred from 2% to 7% by weight.
[0158] Suitable structuring agents are commercially available surfactants or emulsifiers known in the art and esters such as isopropyl myristate.
[0159] The addition of such structuring substance results in an improved sphere formation during droplet formation. Based thereon the incorporation of the microcapsules/pastilles into the final product formulation is enhanced in a homogeneous manner. These substances are for example an additive that increases the viscosity of the composition to a thick liquid, semisolid, or solid state.
[0160] Furthermore, it was surprisingly found that the addition of a structuring agent further improves the homogeneity of the inventive compositions, in particular in the presence of waxes. Mixtures of waxes and polyethylene glycol tend to separate and form distinct phases. However, by adding a structuring agent as specified herein a homogeneous formulation can be obtained.
[0161 ] Accordingly, the structuring agent can be an emulsifier or surfactant. [0162] The addition of surfactants is particularly suitable for compositions comprising an adhesion agent as specified herein. The compositions according to the present invention may comprise any kind of surfactant, namely anionic surfactants, cationic surfactants, non-ionic surfactants, amphoteric / zwitterionic surfactant, and any mixture thereof. Among these surfactants non-ionic surfactants are particularly preferred.
[0163] Suitable surfactants are for example selected from the group consisting of ammonium derivates, esters, sulfonates, sulfates, sorbates and related surfactants, and mixtures thereof.
[0164] Non-ionic detergents are particularly beneficial for preparing “green” compositions.
[0165] The above specified surfactants can be used either singular or in the form of mixtures of two, three, or even more surfactants, either from the same surfactant category (anionic, cationic, non-ionic, amphoteric/zwitterionic) or as mixture of surfactants of different surfactant categories.
[0166] Preferably, the composition according to the second aspect of the present invention includes at least one surfactant, preferably a non-ionic surfactant.
[0167] Accordingly, in another referred variant the present invention relates to a composition comprising or consisting of at least one pastille, wherein said pastille comprises or consists of:
(a) from 0.5% to 10% by weight of at least one microcapsule encapsulating an active ingredient, wherein said active ingredient is preferably a fragrance or fragrance mixture;
(b) from 60% to 80% by weight of at least one polymer, preferably polyethylene glycol;
(c) from 2% to 32% by weight of at least one adhesion agent, wherein said adhesion agent is preferably selected from the group consisting of fatty acids, fatty alcohols, fatty acid esters or mixtures thereof, such as waxes; based on the total weight of the pastille; and
(d) from 0.1% to 10% by weight of free fragrance or free fragrance mixture; based on the total weight of the pastille, wherein said at least one pastille further comprises or consists of: from 0.1% to 10% by weight of at least one structuring agent, preferably a surfactant and even more preferred a non-ionic surfactant, wherein said structuring agent is preferably selected from the group consisting of esters, such as isopropyl myristate or other emulsifiers; based on the total weight of the pastille.
[0168] Additionally, the compositions according to the present invention can comprise further suitable additives if required. Further suitable additives are for example dyes, laundry actives etc.
[0169] Composition/Pastille:
[0170] The compositions according to the present invention comprise or consist of at least one pastille having the compositions specified above. Preferably the compositions are present as a plurality of pastilles. Alternatively, the compositions are present as a single pastille of the above-specified compositions according to the first or second aspect.
[0171 ] According to a first aspect of the present invention the compositions of the present invention comprise or consist of at least one pastille comprising an encapsulated active ingredient, preferably a fragrance (mixture), a polymer forming a polymer matrix, preferably polyethylene glycol, and free fragrance (mixture).
[0172] According to a first aspect the composition thus comprises or consists of at least one pastille, wherein said pastille comprises or consists of:
(a) from 0.5% to 10% by weight based on the total weight of the pastille of at least one microcapsule encapsulating an active ingredient, wherein said active ingredient is preferably a fragrance or fragrance mixture;
(b) from 92% to 98% by weight based on the total weight of the pastille of a polymer, wherein the polymer is preferably polyethylene glycol (PEG); and
(c) from 0.1% to 10% by weight of free fragrance or a free fragrance mixture; based on the total weight of the pastille.
[0173] Optionally, in a further preferred embodiment the pastille of the composition according to the first aspect further comprises or consists of:
(d) from 0.5% to 10% by weight (based on the total weight of the pastille) of at least one plasticizer, wherein said plasticizer is preferably water or polyethylene glycol.
[0174] According to another embodiment the compositions of the present invention comprise or consist of at least one pastille comprising an encapsulated active ingredient, preferably a fragrance (mixture), a polymer forming a polymer matrix, preferably polyethylene glycol, free fragrance (mixture) and optionally at least one adhesion agent.
[0175] Thus, according to a second aspect the composition comprises or consists of at least one pastille, wherein said pastille comprises or consists of:
(a) from 0.5% to 10% by weight based on the total weight of the pastille of at least one microcapsule encapsulating an active ingredient, wherein said active ingredient is preferably a fragrance or fragrance mixture;
(b) from 60% to 80% by weight based on the total weight of the pastille of at least one polymer, preferably polyethylene glycol;
(c) from 2% to 32% by weight of based on the total weight of the pastille at least one adhesion agent, wherein said adhesion agent is preferably selected from the group consisting of fatty acids, fatty alcohols, fatty acid esters or mixtures thereof, such as waxes; and
(d) from 0.1% to 10% by weight of free fragrance or free fragrance mixture; based on the total weight of the pastille.
[0176] Optionally, the pastille of the composition according to the second aspect further optionally comprises or consists of:
(e) from 0.5% to 10% by weight based on the total weight of the pastille of at least one plasticizer, wherein said plasticizer is preferably water or polyethylene glycol; and/or
(f) from 0.1 % to 10% by weight based on the total weight of the pastille of at least one structuring agent, wherein said structuring agent is preferably selected from the group consisting of esters, such as isopropyl myristate or other emulsifiers; based on the total weight of the pastille.
[0177] Accordingly, in another referred variant the present invention relates to a composition comprising or consisting of at least one pastille, wherein said pastille comprises or consists of:
(a) from 0.5% to 10% by weight of at least one microcapsule encapsulating an active ingredient, wherein said active ingredient is preferably a fragrance or fragrance mixture;
(b) from 60% to 80% by weight of at least one polymer, preferably polyethylene glycol;
(c) from 2% to 32% by weight of at least one adhesion agent, wherein said adhesion agent is preferably selected from the group consisting of fatty acids, fatty alcohols, fatty acid esters or mixtures thereof, such as waxes; based on the total weight of the pastille; and (d) from 0.1% to 10% by weight of free fragrance or free fragrance mixture; based on the total weight of the pastille, wherein said at least one pastille further comprises or consists of: from 0.1% to 10% by weight of at least one structuring agent, preferably a surfactant and even more preferred a non-ionic surfactant, wherein said structuring agent is preferably selected from the group consisting of esters, such as isopropyl myristate or other emulsifiers; based on the total weight of the pastille.
[0178] It was found that the compositions according to the second aspect of the present invention further comprising an adhesion agent as specified herein show improved protection and release properties. Moreover, it was found that the preparation of such pastilled compositions can be improved due to the presence of the adhesion agent resulting in more homogeneous, more flexible and less brittle pastilles with an enhanced microcapsule distribution (see also Example 5).
[0179] In a preferred embodiment according to the present invention, the compositions and consequently the pastilles according to the present invention have a solidification point from 25 °C to 100 °C, preferably from 30 °C to 90 °C, more preferably from 35 °C to 85 °C and most preferred from 40 °C to 75 °C.
[0180] A solidification point within this range allows for a facilitated handling of the compositions according to the present invention and the pastilles thereof.
[0181 ] According to another preferred embodiment the compositions according to the present invention and consequently the corresponding pastille have a viscosity q in the range from 500 mPas to 1 ,000 mPas at a temperature of 70 °C and a shear pressure of 6.4 Pa, preferably a viscosity in the range from 760 mPas to 980 mPas, and even more preferred a viscosity in the range from 800 mPas to 950 mPas.
[0182] For compositions according to the present invention the viscosity q is even more preferred in the range from 750 mPas to 1 ,000 mPas at a temperature of 70 °C and a shear pressure of 6.4 Pa, preferably a viscosity in the range from 760 mPas to 980 mPas, and even more preferred a viscosity in the range from 800 mPas to 950 mPas. If the viscosity of the compositions is within the above ranges, the composition is considered “solid” at room temperature. [0183] Thus, preferably, the composition according to the present invention is preferably a solid composition.
[0184] In addition, it was found that the viscosity of the composition influences the pastille formation by dripping as such as well as the stability of the pastilles (see Figures 6 and 7). If the viscosity of the compositions is within the above ranges processing of the compositions (in particular in a pastillation process as specified herein) and their incorporation into solid consumer product formulations is facilitated. Additionally, if the viscosity is within the above ranges an ideal balance between microcapsule protection and microcapsule performance can be achieved. Due to the low viscosity, the mixture can be homogenized better, and at the same time the lower viscosity allows for an improved dripping behaviour. Furthermore, if the viscosity of the compositions is within the above ranges the encapsulated actives can be distributed in a more homogeneous manner within the pastilles. In addition, such viscosities provide for improved pastille flexibilities, i.e. the pastille are less brittle and simultaneously show an improved buffering effect.
[0185] The viscosity can be adjusted correspondingly via the content of the adhesion agent as well as the plasticizer content.
[0186] As the shear rate increases, the viscosity decreases within a range with which dripping is still possible, thereby further improving the final product properties, in particular the pastille stability, the homogeneity as well as the processability of the pastille formulations.
[0187] Based on another preferred variant of the present invention, the compositions according to the present invention and consequently the corresponding pastilles, have a Young's modulus E of higher than 100 Pa and less than 1 GPa, preferably from 1 kPa to 100 MPa, and even more preferred from 10 kPa to 1 MPa.
[0188] The Young's modulus E describes the tensile or compressive stiffness of a solid but elastic material when the force is applied lengthwise based on the tensile/compressive stress (force per unit area) and axial strain (proportional deformation) in the linear elastic region of a material.
[0189] An elasticity within said ranges allows for ideal balance between microcapsule protection and their efficient incorporation into solid consumer product formulations while allowing for excellent release properties. [0190] In another preferred variant the total water content in the composition according to the present invention and thus of the corresponding pastilles is from 2% to 12% by weight based on the total weight of a pastille. Preferably the water content is in the range from 3% to 9% by weight and even more preferred in the range from 4% to 8% by weight.
[0191 ] Such amounts of water are advantageous in terms of flexibility as the water component can function as plasticizer and thus is valuable in view of an improved buffering effect and thus better protection of the fragile microcapsules and a facilitated incorporation into solid consumer product formulations without altering the fundamental chemical character of the plasticized material. Higher amounts of water will decrease the viscosity too much making an incorporation into solid formulations more difficult while to low water contents make the pastille material to brittle for an incorporation.
[0192] In addition, it was found that if the overall water content is within the ranges specified above, the pastille preparation is facilitated resulting in homogeneous pastille shapes.
[0193] The abovementioned properties of the compositions according to the present invention can be adjusted based on the specific amounts of the components, the molecular weight of the polymer and the free fragrance component as well as the optional addition of additives such as the plasticizers and structuring agents described above.
[0194] It is additionally advantageous if the particle size of the pastille(s) of the compositions according to the present invention is from 1 pm to 1 cm, preferably from 100 pm to 7 mm and even more preferred from 500 pm to 5 mm in order to achieve an ideal distribution of the pastilles within the final solid consumer product formulation and thus in turn of the microcapsules embedded therein. Too big pastilles result in an inhomogeneous distribution within the final product formulation.
[0195] In a further preferred variant of the present invention the ratio between the size of the microcapsules and the size of the final granules/pastilles is in the range of from 1 : 5 to 1 : 200, preferably from 1 : 10 to 1 : 100.
[0196] Said pastilles or granules are preferably present in the shape of tablets, pills, spheres, and the like, having a spherical, hemispherical, compressed hemispherical, lentil shaped, and oblong shape and can be prepared by any method known in the art by those skilled in the art (see Figure 6). [0197] Moreover, the composition of the invention and the pastilles thereof may further comprise one or more ingredients which improve the visual aesthetics of the final product such as colourants. In addition, the composition can comprise further additives and/or active ingredients such as optical brighteners, cleaning agents, laundry actives and the like.
[0198] Further additives such as balancing agents such as glycerine or alkanediols or fillers can be added if required. However, preferably the compositions according to the present invention do not comprise a balancing agent and/or do not comprise a filler.
[0199] Process for the preparation of the inventive compositions:
[0200] According to a third aspect the present invention relates to a process for the preparation of a composition comprising or consisting of a plurality of pastilles comprising the following steps of:
(i) providing at least one microcapsule or an aqueous dispersion comprising at least one microcapsule;
(ii) melting of at least one polymer and optionally at least one adhesion agent;
(iii) mixing the at least one microcapsule into the polymer melt of step (ii);
(iv) admixing free fragrance or a free fragrance mixture;
(v) forming pastilles by dripping the mixture of step (iv); and
(vi) optionally cooling; optionally further comprising the step of adding at least one plasticizer and/or at least one structuring agent in, or after step (ii), (iii) and/or (iv).
[0201 ] In the context of the present invention, the components specified above in the context of the first and second aspect likewise apply to the subject of the third aspect, i.e. the terms “microcapsule”, “polymer”, “free fragrance”, “adhesion agent”, “plasticizer”, “pastille”, “structuring agent” etc. as well as the corresponding amounts and properties as specified above.
[0202] The process according to the third aspect as specified herein is suitable for the preparation of the compositions according to the first and second aspect of the present invention based on the corresponding adjustment of the required amounts.
[0203] In a first step (i) of the process according to the present invention microcapsules as specified herein are provided. Said microcapsules can either be present as such or alternatively in the form of an aqueous dispersion comprising one or more microcapsules and preferably a plurality of microcapsules.
[0204] Preferably, the microcapsules are dispersed in an aqueous phase, microcapsules according to the invention dispersed in an aqueous phase, preferably wherein the microcapsule concentration within the aqueous phase is greater than 5% and less than 70% by weight, preferably greater than 20% and less than 60% by weight, most preferably greater than 30% and less than 50% by weight based on the weight of the dispersion.
[0205] It was further found, that advantageously amounts of 30% by weight or less of such an aqueous microcapsule slurry are employed in the process of the present invention (see Figure 6 and Example 6), and further preferred amounts of 20% by weight or less and even more preferred of 15% by weight or less. Ideal results in terms of stability, flexibility and performance were observed for additions of 5% to 10% by weight of such aqueous microcapsule dispersions (“microcapsule slurry”, preferably the capsule- to- water ratio of such a slurry is 2:3 by weight of the slurry).
[0206] The provision of microcapsules in the form of a dispersion is advantageous in terms of a more homogeneous distribution of the microcapsules within the final pastilles. Additionally, the comprised water of the continuous or outer phase of the dispersion can serve as plasticizer helping to improve the final product properties as specified above, allowing for an efficient adjustment of the viscosity and flexibility of the polymeric matrix resulting in a less brittle and more flexible matrix with improved buffering effect and thus better protection of the fragile microcapsules and a facilitated incorporation into solid consumer product formulations without altering the fundamental chemical character of the plasticized material.
[0207] Therefore, preferably the microcapsule(s) is/are provided in the form of an aqueous dispersion in step (i) of the process according to the third aspect of the present invention.
[0208] In a subsequent step (ii) of the process according to the invention, the at least one polymer is melted. Depending on the approach an adhesion agent can be added which is heated and melted together with the polymer as specified herein. Alternatively, both substances can be melted separately and subsequently the resulting corresponding melts can be combined and homogenized. [0209] In order to achieve a homogeneous distribution of microcapsules within the polymeric matrix it is further preferred to use a polymer as specified herein, and preferably polyethylene glycol, wherein the melting point of the at least one polymer, and preferably of the polyethylene glycol, is in the range from 25 °C to 100 °C, and preferably from 40 °C to 80 °C.
[0210] Thus, according to a further preferred variant of the present invention the melting point of the polymer according to the first, second and/or third aspect of the present invention preferably having a molecular weight from about 3,000 Da to 20,000 Da is preferably in the range from 25 °C to 100 °C, and preferably from 40 °C to 80 °C in order to efficiently and homogeneously embed the microcapsules within the polymeric matrix.
[0211 ] In a preferred variant of the process according to the invention correspondingly the melting step (ii) is conducted at a temperature in the range from 25 °C to 100 °C, preferably from 40 °C to 80 °C, and even more preferred at 80 °C in order to achieve a homogeneous distribution of microcapsules in the polymeric buffering matrix.
[0212] In this step, additional additives such as adhesion agents, surfactants, plasticizers and/or structuring agents can be added and mixed to obtain a homogenous mixture.
[0213] The at least one microcapsule or microcapsule dispersion is mixed into the polymer melt of step (ii) and the resulting mixture homogenized in a further process step (iii) in order to obtain a homogeneous distribution of discrete microcapsules within the melt.
[0214] The as-prepared polymer composition is then mixed with free, i.e. unencapsulated fragrance component (a single fragrance substance or a mixture of two or more fragrance substances) (step (iv)).
[0215] The resulting mixture homogenized in order to obtain a homogeneous distribution of the components.
[0216] Finally, in a subsequent step (v) pastilles are formed by dripping the mixture of step (iv) using state-of-the-art pastillation processes known to those skilled in the art.
[0217] Pastillation is a particle forming process, where usually a pastille is formed using a droplet former, followed by cooling of the as-obtained discrete particles. Processes for the preparation of pastilles or granules are commercially used methods and the pastilles may be formed into different shapes include tablets, pills, spheres, and the like. Moreover, up-scaling by dropping using a pulse generator in air or vegetable oil also showed good results.
[0218] Optionally the obtained granules are solidified in an additional cooling step (vi).
[0219] If required, at least one plasticizer and/or a structuring agent and/or surfactant can be added in or after step (ii), (iii) and/or (iv).
[0220] Alternatively, according to another preferred embodiment of the process according to the present invention, the free fragrance component is mixed with the molten polymer and the microcapsules are added afterwards.
[0221 ] According to this embodiment the composition is prepared based on the following steps:
(i) providing at least one microcapsule or an aqueous dispersion comprising at least one microcapsule;
(ii) melting of at least one polymer and optionally at least one adhesion agent;
(iii) admixing free fragrance or a free fragrance mixture into the polymer melt of step (ii);
(iv) mixing the at least one microcapsule into the mixture of step (iii)
(v) forming pastilles by dripping the mixture of step (iv); and
(vi) optionally cooling; optionally further comprising the step of adding at least one plasticizer and/or at least one structuring agent in or after step (ii), (iii) and/or (iv).
[0222] According to an alternative embodiment the free fragrance component and the microcapsule component are added simultaneously to the molten polymer.
[0223] It was surprisingly found, that the order of mixing does not influence the final product properties. This means that the molten polymer, the microcapsule component, the free fragrance component and, if present, any further (optional) ingredients can be admixed in any order or simultaneously.
[0224] In order to achieve a homogeneous distribution of microcapsules within the protecting matrix it is advantageous to use microcapsules having a particle size ranging from 150 pm to 5 mm, preferably in the rage from 500 pm to 3 mm. [0225] Thus, according to a preferred variant of the present invention the particle size of the microcapsule(s) according to the first, second and/or third aspect of the present invention is preferably in the range from 150 pm to 5 mm, preferably in the rage from 500 pm to 3 mm.
[0226] According to another aspect the present invention further relates to a composition comprising or consisting of at least one pastille obtained by the process according to the invention, wherein said at least one pastille comprises or consists of:
(a) at least one microcapsule encapsulating an active ingredient which is preferably dispersed in a polymer matrix, and wherein said active ingredient is preferably a fragrance or fragrance mixture;
(b) at least one polymer (forming said polymer matrix), wherein said polymer is preferably polyethylene glycol;
(c) optionally at least one adhesion agent, wherein said adhesion agent is preferably selected from the group consisting of fatty acids, fatty alcohols, fatty acid esters or mixtures thereof, such as waxes; and
(d) free fragrance or free fragrance mixture which a preferably dispersed in said polymer matrix; wherein the composition has a viscosity q of less than 900 mPa s at 80 °C.
[0227] Due to the reduction of the viscosity the formulation can be prepared in a manner more homogenous. At the same time the lower viscosity leads to a better dripping behaviour and thus to the facilitated and more homogeneous formation of homogeneous pastilles.
[0228] It was surprisingly found that the viscosity can positively be influenced both by the free fragrance component as well as the matrix component (such as the PEG matrix).
[0229] Additionally, in a further aspect of the present invention relates to compositions prepared according to the inventive process.
[0230] Consumer products:
[0231 ] Additionally, in another aspect, the present invention relates to the use of the compositions according to the invention for the preparation of consumer product formulations. The terms "consumer product formulation" and "consumer product" are used synonymously within the context of the present invention. [0232] Thereby, any of the abovementioned compositions is suitable for the preparation of consumer product formulations, i.e. compositions according to the first aspect of the present invention, compositions according to the second aspect of the present invention and/or compositions obtained based on the process according to the third aspect of the present invention, as well as mixtures thereof.
[0233] Moreover, a consumer product can advantageously comprise two or more different compositions according to the present invention, which differ for example in the composition and/or amounts of the encapsulated active ingredient/fragrance component, the free fragrance component and/or the composition of the polymeric matrix. This allows for a further improvement in the olfactory performance and its complexity. Additionally, this approach allows for the combination of different active ingredients which otherwise would not be compatible.
[0234] Particular advantages of the inventive pastille compositions were found in view of the preparation of solid consumer products such as powder detergents, laundry soaps, solid fabric softeners, deo sticks and the like. Thus, preferably the consumer product according to the present invention is a solid consumer product.
[0235] When incorporated into consumer product formulations, microcapsules have to be chemically stable in a rather aggressive environment but simultaneously also be mechanically stable when subjected to mechanical stress such as during the mixing and optionally pressing of a solid consumer product formulation. However, an increase in the shell thickness usually will result in worsened release properties (release of the active ingredient) due to a high capsule breakage during the processing caused by shearing. It was surprisingly found that the compositions according to the present invention, which are based on microcapsules embedded in a polymeric matrix in combination with free fragrance dispersed in said matrix, are particularly suitable for the incorporation in solid consumer product formulations. The polymeric matrix protects the microcapsules while allowing for high release performances.
[0236] The additional free fragrance(s) dispersed in the polymeric matrix further improve the processability, homogeneity and release properties. Additionally, it instantly improves the consumer's scent experience from the onset.
[0237] Therefore, in another preferred variant the present invention also relates to the use of the composition according to the present invention for the preparation of consumer products and formulations thereof, wherein said consumer product or consumer product formulation is a solid product such as a textile care product (such as a powder detergent, laundry soap, solid fabric softener), a solid soap, a household product (such as a solid WC-cleaner, solid allpurpose cleaners, powdered carpet cleaners, powdery washing agents for washing dishes or for cleaning various surfaces), a personal care product (such as a deodorant, soap), scent boosters, fragrance enhancers, a pharmaceutical product, and mixtures thereof.
[0238] Finally, in another aspect the present invention relates to the consumer product or consumer product formulation as such comprising or consisting of the composition according to the invention, i.e. the composition according to the first aspect of the present invention, the composition according to the second aspect of the present invention and/or the composition obtained based on the process according to the third aspect of the present invention, and mixtures thereof.
[0239] The inventive compositions allow for the efficient incorporation of active ingredients into solid product formulations allowing for an efficient and targeted release of said active ingredients.
Examples
[0240] Hereinafter, the present invention is described in more detail and specifically with reference to the examples, which however are not intended to limit the present invention.
[0241 ] Example 1 : Composition comprising microcapsules with and without additional free fragrances in powder detergent - Sensory evaluation.
[0242] According to a first example a composition comprising or consisting of at least one pastille comprising microcapsules was prepared as follows: In a first step core-shell microcapsules comprising a melamine-formaldehyde-based shell material and a fragrance core were provided (microcapsule size: 10 to 50 pm). The microcapsules were prepared according to the state of the art. Subsequently, 78.8% by weight of a polymer mixture comprising PEG-150 and PEG-450 were mixed with 7.5% by weight of rapeseed wax was melted at a temperature of 80 °C. Thereafter, 2.5% by weight of a non-ionic surfactant (Imbentin AG/168S/500 G) were added followed by 3.2% by weight of free fragrance (free fragrance mixture 1 : mixture of aldehydes, alcohols, ketones, and hydrocarbons). In a next step, 8% by weight of a microcapsule slurry (the capsule-to-water ratio of the slurry was 2:3 by weight of the slurry) were mixed with the as-obtained polymer melt. Finally, the viscous mixture was dripped a using state-of-the-art pastillation process by dripping the viscous material through small openings in order to form a plurality of pastilles having an average particle size of approximately 2 mm in which the microcapsules are embedded in a polyethylene glycol matrix, followed by cooling for solidification of the pastilles. The portion of the polyethylene glycol of the final pastilles was about 78.8% by weight based on the total weight of each pastille. The amounts of the above-mentioned components are based on the total weight of the final pastille.
[0243] The following fragrance composition/mixtures was used as the free fragrance component:
Free fragrance mixture 1 : General fragrance
Mixture of: Agrumex LC, Agrunitril, Aldehyd C10, Aldehyd C12 Laurin, Aldehyd C12 MNA, Aldehyd C14 sog., Allylcapronat, Amarocit, Ambrocenide, Amylsalicylat, Benzalydehyd, Benzylacetat, Benzylaceton, Benzylsalicylat, Borneol/lsoborneol 65:35, Bourgeonal, Citronellol 950, Clonal, CM20 Sanjinol Replacer, Coniferan, Cumarin, Cyclamenaldehyd, Cyclohexylsalicylat, Damascenon, Damascene Delta, Decenol, Dihydromrycenol, Dimethylbenzylcarbinol, Dimethylbenzylcarbinylacetat, Diphenyloxid, Dipropylenglycol, Dynascone, Ethylcaprinat, Eucalyptusoil, Eugenol, Florazon, Florosa BM/Pyranol, Geraniol Supra, Geranylacetat 60, Hexylacetat, Hexylsalicylat, Hexylzimtaldehyd alpha, Isobornylacetat, Isooctanon, Isodralein 70, Kresolmethylether para, Labienoxime, Lemonile, Lilial, Linalool, Linaylacetat, Manzanate, Melonaol, Methyloctincarbonat, Mugenal, Mugetaoil, Orangeoil, Patchoulioil, Peonile, Phenylethylacetat, Phenylethylalkohol, Phenylethylmethylether, Pinoacetataldehyd, Rosenoxid High Cis, Stemone, Stryolacetat, Tamarine Type Base BHT Free, Terpineol Rein, Timbersilk, Undecanon-2, Undecavertol, Vertofix, Vertroprenal, Ylang Colipa Base.
[0244] The sensory evaluation was performed as follows: Once the composition according to the present invention was prepared the as-obtained pastilles were combined with commercially available powder detergent and homogenized. The final dosage of the microcapsules in 40 g of the powder detergent was 0.5% by weight (corresponding to 6.25% by weight of pastilles in 40 g of the powder detergent).
[0245] Finally, the product was added to the laundry machine and the fabrics (terry cloth) washed at 30 °C.
[0246] After rinsing the fabrics were air dried at room temperature (line-dried).
[0247] A corresponding powder detergent was used as reference. Thereby, comparative pastilles were prepared in an analogous manner which did not contain any free fragrance component.
[0248] All microcapsules have a particle size in the range of 10 - 50 pm.
[0249] The fragrance release was carried out in four steps. The first step describes the smelling of a freshly washed, i.e. wet or damp cloth. The second step described the smelling of an untreated dry cloth (“pre-rub”). The third step describes the smelling of a lightly kneaded dry cloth; for this purpose, the cloth was subjected to slight mechanical stress by moving it back and forth between the hands several times, causing the capsules to break. The fourth step describes the smelling after the dry clothes were rubbed strongly and thus the capsules broke. After each step, the fragrance intensity was evaluated. [0250] In order to evaluate the sensory performance, 8 to 9 test persons assessed the fragrance intensity on a scale of 1 (no odour) to 9 (very strong odour).
[0251 ] The results of the sensory evaluation are shown in Figure 1.
[0252] The mechanical treatment of the textiles causes a rupture of the fragile microcapsules thereby releasing the active ingredient (here: fragrance composition). It was surprisingly found that samples comprising the composition according to the present invention comprising the core-shell microcapsules embedded in a polyethylene glycol matrix show a considerably increased performance indicating an efficient protection of the fragile microcapsules within the solid product formulation while simultaneously allowing for an efficient release of the active ingredient. The polymer matrix serves as a shock absorbing layer in the production process of the consumer product. Samples not containing such a shock absorbing layer and such comprising a mere coating do not perform as most of the microcapsules are already destroyed during the preparation of the consumer product.
[0253] Additionally, it was surprisingly found that the presence of a free fragrance component dispersed within the polymer matrix results in further improved release properties (Figure 1 : “pre” (pre-rub), “kneaded”, “post” (post-rub)). Moreover, it was possible to achieve a comparably high initial scent experience, i.e. before mechanically rupturing the microcapsules and thereby releasing the encapsulated fragrances (Figure 1 : “wet”, i.e. freshly washed textile). The scent experience achieved by compositions according to the present invention is thus (i) prolonged and present from the onset (i.e. directly after the treatment), and (ii) intensified thereby achieving a long-lasting and intense olfactive perception during and after application.
[0254] Example 2: Composition comprising microcapsules with and without additional free fragrances - Viscosity in dependence of the presence of free fragrances.
[0255] According to a second example a composition comprising or consisting of at least one pastille comprising microcapsules was prepared in accordance with Example 1 . Subsequently, the pastilles were analysed using a rheometer (HAAKE Rheometer RS 1 (RheoStress)) and the viscosity was tested at different temperatures.
[0256] Again, a composition of pastilles without an additional free fragrance component served as reference. [0257] The results of the viscosity analysis are shown in Figure 2.
[0258] The analysed samples show that the viscosity decreases with increasing temperature. In a conventional emulsion, the addition of oil droplets (e.g., free perfume oil) is associated with a sharp increase in viscosity and the appearance of shear-thinning flow behaviour. Similar behaviour would be expected for the compositions of the present invention. However, for the compositions according to the present invention, it was surprisingly found that the viscosity is lower for samples comprising an additional free fragrance component dispersed in the polymeric matrix, i.e. the flowability is increased.
[0259] It was surprisingly found that the low viscosity allows for a better homogenization of the composition mixture while simultaneously allowing for a better dripping and thus the formation of more homogenous pastilles. In addition, the sensory data shows that the addition of free oil further provides a better sensory experience from the onset.
[0260] Moreover, it was surprisingly found that the viscosity reproducibly decreases independently of the functional groups of the free fragrance component. Accordingly, this viscosity reducing effect can be achieved with any fragrance substance / fragrance mixture.
[0261 ] Example 3: Composition comprising microcapsules with additional free fragrances - Viscosity in dependence of the type of free fragrance.
[0262] According to another example a composition comprising or consisting of at least one pastille comprising microcapsules was prepared as follows: In a first step core-shell microcapsules comprising a melamine-formaldehyde-based shell material and a fragrance core were provided (microcapsule size: 10 to 50 pm). The microcapsules were prepared according to the state of the art. Subsequently, 78.8% by weight of the polymer PEG-150 were mixed with 7.5% by weight of rapeseed wax was melted at a temperature of 80 °C. Thereafter, 2.5% by weight of a non-ionic surfactant (Imbentin AG/168S/500 G) were added followed by 3.2% by weight of free fragrance and 8% by weight capsule slurry (capsule to water ratio 2:3).
[0263] The following fragrance compositions/mixtures were used as the free fragrance component:
Free fragrance mixture 1 : General fragrance Mixture of: Agrumex LC, Agrunitril, Aldehyd C10, Aldehyd C12 Laurin, Aldehyd C12 MNA, Aldehyd C14 sog., Allylcapronat, Amarocit, Ambrocenide, Amylsalicylat, Benzalydehyd, Benzylacetat, Benzylaceton, Benzylsalicylat, Borneol/lsoborneol 65:35, Bourgeonal, Citronellol 950, Clonal, CM20 Sanjinol Replacer, Coniferan, Cumarin, Cyclamenaldehyd, Cyclohexylsalicylat, Damascenon, Damascene Delta, Decenol, Dihydromrycenol, Dimethylbenzylcarbinol, Dimethylbenzylcarbinylacetat, Diphenyloxid, Dipropylenglycol, Dynascone, Ethylcaprinat, Eucalyptusoil, Eugenol, Florazon, Florosa BM/Pyranol, Geraniol Supra, Geranylacetat 60, Hexylacetat, Hexylsalicylat, Hexylzimtaldehyd alpha, Isobornylacetat, Isooctanon, Isodralein 70, Kresolmethylether para, Labienoxime, Lemonile, Lilial, Linalool, Linaylacetat, Manzanate, Melonaol, Methyloctincarbonat, Mugenal, Mugetaoil, Orangeoil, Patchoulioil, Peonile, Phenylethylacetat, Phenylethylalkohol, Phenylethylmethylether, Pinoacetataldehyd, Rosenoxid High Cis, Stemone, Stryolacetat, Tamarine Type Base BHT Free, Terpineol Rein, Timbersilk, Undecanon-2, Undecavertol, Vertofix, Vertroprenal, Ylang Colipa Base.
Free fragrance mixture 2: Hydrocarbon mixture
Mixture of: Caren Delta-nat., Caryophyllen nat. rekt., Pinen alpha laevo nat., Terpinen Gamma.
Free fragrance mixture 3: Hydrocarbon mixture (= free fragrance mixture 2) + Ester, wherein the ester component is Benzylbutyrat.
Free fragrance mixture 4: Hydrocarbon mixture (= free fragrance mixture 2) + Aldehyde, wherein the aldehyde component is Aldehyde C10.
[0264] Subseguently, the pastilles were analysed using a rheometer (HAAKE Rheometer RS 1 (RheoStress)) and the viscosity was tested at different temperatures.
[0265] Again, a composition of pastilles without an additional free fragrance component served as reference.
[0266] The results of the viscosity analysis are shown in Figure 3.
[0267] The analysed samples show that the viscosity decreases with increasing temperature. In addition, it was found that hydrocarbon compounds have a stronger influence on the viscosity. Further decreases of the viscosity were in dependence of further fragrance additives such as esters and aldehydes. This leads to the conclusion, that the viscosity can be influenced by the selection of the fragrance component, i.e. the fragrance emulsifier. This makes the sample more homogenizable, resulting in a more uniform particle.
[0268] Example 4: Composition comprising microcapsules with additional free fragrances - Viscosity in dependence of the molecular weight of the polymer matrix.
[0269] According to a fourth example a composition comprising or consisting of at least one pastille comprising microcapsules was prepared as follows: In a first step core-shell microcapsules comprising a melamine-formaldehyde-based shell material and a fragrance core were provided (microcapsule size: 10 to 50 pm). The microcapsules were prepared according to the state of the art. Subsequently, 78.8% by weight of the polymer PEG were mixed with 7.5% by weight of rapeseed wax was melted at a temperature of 80 °C. Thereafter, 2.5% by weight of a non-ionic surfactant (Imbentin AG/168S/500 G) were added followed by 3.2% by weight of free fragrance and 8% by weight capsule slurry (capsule to water ratio 2:3) (free fragrance mixture 1).
[0270] The PEG component was varied by using polymers having different molecular weights. The following PEG compounds were used: PEG 10,000 g/mol PEG 8,000 g/mol PEG 6,000 g/mol
[0271 ] Subsequently, the pastilles were analysed using a rheometer rheometer (HAAKE Rheometer RS 1 (RheoStress)) and the viscosity was tested at different temperatures.
[0272] Again, a composition of pastilles without an additional free fragrance component served as reference in combination with the different polymer components.
[0273] The results of the viscosity analysis are shown in Figure 4.
[0274] The analysed samples show the beneficial effect of the presence of free fragrance components, i.e. the fragrance emulsifier. Additionally, it was surprisingly found that lower molecular weight PEGs lead to lower viscosities. Mixtures of different PEGs lead to lower viscosities, which means that both the mixture with free fragrance oils and the pure addition of PEG both result in a decrease of the viscosity and the resulting advantages specified above. The additional addition of free fragrance however has a surprising double advantage with improved odour and viscosity decrease.
[0275] Usually, PEGs having molecular weights of above 3,000 g/mol are solids with rather comparable melting ranges. However, it was surprisingly found that the molecular weight has a considerable influence on the melting behaviour and he viscosities of the resulting compositions.
[0276] The results show that the use of microcapsules embedded in a polymer-adhesion agent-matrix in combination with specific amounts of free fragrance components result in an even more improved performance of the consumer product.
[0277] Example 5: Composition comprising microcapsules with additional free fragrances for different adhesion agents - Sensory evaluation.
[0278] According to a fifth example different compositions comprising or consisting of at least one pastille comprising microcapsules were prepared. Said different samples comprising an adhesion agent were prepared as follows: In a first step core-shell microcapsules comprising a melamine-formaldehyde-based shell material and a fragrance core were provided (microcapsule size: 10 to 50 pm). The microcapsules were prepared according to the state of the art. Subsequently, 78.8% by weight of a polymer mixture comprising PEG-150 and PEG- 450 were mixed with 7.5% by weight of adhesion agent (see Figure 5) was melted at a temperature of 80 °C. Thereafter 2.5% by weight of a non-ionic surfactant (Imbentin AG/168S/500 G) were added followed by 3.2% by weight of free fragrance (free fragrance mixture 1 : mixture of aldehydes, alcohols, ketones and hydrocarbons). In a next step, 8.0% by weight of a microcapsule slurry (the capsule-to-water ratio of the slurry was 2:3 by weight of the slurry) were mixed with the as-obtained polymer melt. Finally, the viscous mixture was dripped a using state-of-the-art pastillation process by dripping the viscous material through small openings in order to form a plurality of pastilles having an average particle size of approximately 2 mm in which the microcapsules are embedded in a polyethylene glycol matrix, followed by cooling for solidification of the pastilles. The portion of the polyethylene glycol of the final pastilles was about 78.8% by weight based on the total weight of each pastille. The amounts of the above-mentioned components are based on the total weight of the final pastille.
[0279] The PEG to adhesion agent ratio was approximately 10:1 in all of said samples. [0280] Additionally, as a reference, comparative pastilles were prepared in an analogous manner which did not contain any adhesion agent (“capsule in PEG” -without adhesion agent). Said pastilles were prepared as follows: In a first step core-shell microcapsules comprising a melamine-formaldehyde-based shell material and a fragrance core were provided (microcapsule size: 10 to 50 pm). The microcapsules were prepared according to the state of the art. Subsequently, 86.3% by weight of a polymer mixture comprising PEG-150 and PEG- 450 was melted at a temperature of 80 °C. Thereafter, 2.5% by weight of a non-ionic surfactant (Imbentin AG/168S/500 G) were added followed by 3.2% by weight of free fragrance (free fragrance mixture 1 : mixture of aldehydes, alcohols, ketones and hydrocarbons). In a next step, 8.0% by weight of a microcapsule slurry (the capsule-to-water ratio of the slurry was 2:3 by weight of the slurry) were mixed with the as-obtained polymer melt. Finally, the viscous mixture was dripped a using state-of-the-art pastillation process by dripping the viscous material through small openings in order to form a plurality of pastilles having an average particle size of approximately 2 mm in which the microcapsules are embedded in a polyethylene glycol matrix, followed by cooling for solidification of the pastilles. The portion of the polyethylene glycol of the final pastilles was about 86.3% by weight based on the total weight of each pastille. The amounts of the above-mentioned components are based on the total weight of the final pastille.
[0281 ] In order to evaluate the sensory performance, 8 to 9 test persons assessed the fragrance intensity on a scale of 1 (no odour) to 9 (very strong odour) according to the method of Example 1 .
[0282] The results of the sensory evaluation are shown in Figure 5. In order to evaluate the sensory performance, the particles were incorporated in a standard powder detergent which was subsequently dissolved in water. Subsequently, terry cloths were washed in the obtained solution. After air drying at room temperature the sensory evaluation was determined according to the method of Example 1.
[0283] A comparison of the samples with and without an additional adhesion agent show that the addition of an adhesion agent not only improves the manufacturing and preparation of more homogeneous pastilles but also results in an improvement of the sensory experience by allowing for a more efficient protection of the fragile microcapsules and thus a more targeted fragrance release. It was further found that different types of waxes can suitably be used as adhesion agents. [0284] Additionally, it was found that both animal and vegetable waxes are suitable as adhesion agents for use within the compositions of the present invention.
[0285] Example 6: Compositions comprising microcapsules with additional free fragrances according to the invention - influence of the microcapsule slurry content.
[0286] According to a sixth example a composition comprising or consisting of at least one pastille comprising microcapsules was prepared in accordance with Example 1. Accordingly, the pastilles are based on PEG, rapeseed wax and a microcapsule slurry (the capsule-to-water ratio of the slurry was 2:3 by weight of the slurry). However, the amount of capsule slurry used for the preparation of the corresponding pastilled compositions was varied.
[0287] The composition of the single samples is shown in Table 1.
[0288] Table 1 : Composition of five different samples.
Figure imgf000053_0001
Capsule-to-water ratio of 2:3 by weight in the slurry
[0289] Figure 6 shows pictures of these different samples of compositions differing in the amount of capsule slurry used, thereby showing the influence of the microcapsule slurry content on the final pastilles.
[0290] The amount of the microcapsule slurry used in the preparation was varied as follows: The first sample (Figure 6, left) was prepared using 8% of microcapsule slurry by weight (the capsule-to-water ratio of the slurry was 2:3 by weight of the slurry). This amount is considered ideal in terms of flexibility, protective properties and performance, i.e. release properties. Further samples were prepared using 15%, 20%, 30%, and 40% of microcapsule slurry, respectively (from left to right in Figure 6). [0291 ] It was found that an increase in the capsule slurry content in the process according to the invention results in an increased stickiness of the pastilles, resulting in a less homogenous and stable products for amounts of 30% and higher. Best results were found if the amount of slurry was within a range of 0.5% to 10% by weight based on the total pastille composition. This corresponds to a corresponding pure microcapsule content within the same range of 0.5% to 10% by weight, and preferably from 3% by weight to 8% by weight based on the total weight of the pastille.
[0292] Example 7: Compositions with additional free fragrances - influence of the plasticizer I water content.
[0293] According to a seventh example a composition comprising or consisting of at least one pastille was prepared in analogy to Example 1. The pastilles are based on PEG, rapeseed wax and water. However, the pastilles did not comprise microcapsules to show the influence of the water content as such. However, the amount of plasticizer / water used for the preparation of the corresponding pastilled compositions was varied from 0% to 30% by weight (see Figure 7 from left to right). No plasticizer was used in the first sample (0%, left)
[0294] The composition of the single samples is shown in Table 2.
[0295] Table 2: Composition of five different samples.
Figure imgf000054_0001
[0296] Figure 7 shows pictures of these different samples of compositions differing in the amount of the plasticizer water used, thereby showing the influence of the water content / plasticizer content.
[0297] It was found that an increase in the capsule slurry content in the process according to the invention results in an increased stickiness of the pastilles for water amount of 10% or more by weight, resulting in a less homogenous and stable product for amounts of 30% and higher.
[0298] Accordingly, Figure 7 demonstrates that a very high water content, in addition to plasticizing properties, leads to increasing stickiness.
[0299] Moreover, it was found that stickiness leads to increased residues (e.g. wax residues) on the textiles treated with the corresponding laundry formulation.
[0300] Example 8: Compositions with additional free fragrances - influence of the plasticizer I water content.
[0301 ] According to an eighth example a composition comprising or consisting of at least one pastille comprising microcapsules was prepared in accordance with the present invention.
[0302] The composition of the single samples is shown in Table 3.
[0303] Table 3: Composition of five different samples with increasing plasticizer / water content.
Figure imgf000055_0001
Capsule-to-water ratio of 2:3 by weight in the slurry
[0304] The results of the pastillation are shown in Figure 8. Figure 8 demonstrates that an increasing amount of the plasticizer component / water content does not allow for the preparation of suitable pastilles. One effect that is not seen in sample 1 is that the water is used as a "plasticizer", so a small amount, as used in samples 2 to 4, is ideal. In sample 5, on the other hand, we are at a level of water that causes the pellet to have less volume and at the same time be very sticky after evaluation with an expert panel. [0305] Best results were achieved for a plasticizer content in the range of 0.5% to 10% by weight based on the total weight of the pastille. Already small amounts of plasticizer are sufficient to provide for a sufficient flexibility of the pastilles. This guarantees their stability upon mixing with other components of the final formulation such as other detergent components without crumbling. However, too high amounts of the plasticizer do not result in pastilles and show a higher degree of stickiness. This stickiness is disadvantageous when mixing the pastilles according to the present invention with other components of the final formulation such as other detergent components and might result in sticking the single components together thereby reducing the stability of e.g. a detergent powder.
[0306] In addition, the examples show, that a polymer content between 60% and 80% by weight is required in order to provide for ideal pastilles according to the present invention.
[0307] Example 9: Laundry soap
[0308] In addition, a laundry soap was prepared by directly incorporating fragrance microcapsules (0.1% by weight of the final product) and free (unencapsulated) fragrance (0.7% by weight of the product) into a commercially available soap base during the extrusion process. The resulting laundry soap is shown in Figure 9. Accordingly, Figure 9 shows the direct incorporation of microcapsules without the use of the inventive protective system.
[0309] Furthermore, a composition according to the present invention was prepared based on the following formulation: 72% PEG-150, 7.5% rapeseed wax, 2.5% Imbentin, 8% capsule slurry (2:3 fragrance capsules to water), and 10% free (unencapsulated) fragrance. The as- obtained product is shown in Figure 10. Accordingly, Figure 10 shows microcapsules and free fragrance oil incorporated in a protective polymeric matrix.
[0310] It was found that it is possible to efficiently incorporate the inventive compositions/pastilles into solid consumer products such as laundry soaps.
[0311 ] Laundry soap - Sensory evaluation
[0312] In order to evaluate the sensory performance of a laundry soap according to the invention and prepared according to Example 9, 8 to 9 test persons assessed the fragrance intensity on a scale of 1 (no odour) to 9 (very strong odour). [0313] The results of the sensory evaluation are shown in Figure 11 . The sensory evaluation was conducted in the same manner as has been described in Example 1.
[0314] The pastilles according to the present invention as described above (72% PEG-150, 7.5% rapeseed wax, 2.5% Imbentin, 8% capsule slurry (2:3 capsules to water), and 10% free (unencapsulated) fragrance) were incorporated into a soap base in order to obtain a laundry soap.
[0315] Subsequently, the release properties of the as-obtained laundry soap were tested and compared with the release properties of a laundry soap based on the direct incorporation of the fragrance components.
[0316] The results confirm that a direct incorporation of the components into a product does not show the desired release properties, indicating an insufficient homogeneity, stability and incorporation of the decisive components. The unprotected fragile microcapsules are crushed and destroyed during the manufacturing of the final consumer product (i.e. the laundry soap).
[0317] On the other hand, an incorporation of free fragrance oil and encapsulated fragrance components via pastilles according to the present invention in a protective polymeric matrix results in an efficient protection of the fragile microcapsules during the manufacturing process while simultaneously allowing for an efficient and targeted release of the active ingredients, i.e. the encapsulated fragrances. This is reflected by the efficient release properties as shown in Figure 11.
[0318] It was further found that the addition of an adhesion agent as specified herein is decisive for formulating such solid consumer products, especially extruded products such as laundry soaps, in order to ensure efficient incorporation of the actives and in order to provide for a suitable consistency as well as an efficient release of the actives encapsulated in the microcapsules.
Based on the results, it can be concluded that microcapsules and free oil can only be efficiently incorporated into a laundry soap (or comparable solid consumer products) when providing these components in the form of pastilles according to the present invention. In addition, it was found that additional adhesion agents as specified herein are beneficial or even required in order to achieve an efficient, homogeneous and stable incorporation of the components mentioned above. This allows for the preparation of a product with high efficiency and longterm stability.

Claims

Claims
1. Composition comprising or consisting of at least one pastille, wherein said pastille comprises or consists of:
(a) from 0.5% to 10% by weight of at least one microcapsule encapsulating an active ingredient, wherein said active ingredient is preferably a fragrance or fragrance mixture;
(b) from 92% to 98% by weight of a polymer, preferably polyethylene glycol; and
(c) from 0.1% to 10% by weight of free fragrance or a free fragrance mixture; based on the total weight of the pastille.
2. Composition according to claim 1 , wherein said at least one pastille further comprises or consists of:
(d) from 0.5% to 10% by weight of at least one plasticizer, based on the total weight of the pastille, wherein said plasticizer is preferably water or polyethylene glycol.
3. Composition comprising or consisting of at least one pastille, wherein said pastille comprises or consists of:
(a) from 0.5% to 10% by weight of at least one microcapsule encapsulating an active ingredient, wherein said active ingredient is preferably a fragrance or fragrance mixture;
(b) from 60% to 80% by weight of at least one polymer, preferably polyethylene glycol;
(c) from 2% to 32% by weight of at least one adhesion agent, wherein said adhesion agent is preferably selected from the group consisting of fatty acids, fatty alcohols, fatty acid esters or mixtures thereof, such as waxes; based on the total weight of the pastille; and
(d) from 0.1% to 10% by weight of free fragrance or free fragrance mixture; based on the total weight of the pastille.
4. Composition according to claim 3, wherein said at least one pastille further comprises or consists of:
(e) from 0.5% to 10% by weight of at least one plasticizer, wherein said plasticizer is preferably water or polyethylene glycol; and/or
(f) from 0.1% to 10% by weight of a structuring agent, wherein said structuring agent is preferably selected from the group consisting of esters, such as isopropyl myristate or other emulsifiers; based on the total weight of the pastille.
5. Composition according to any one of the preceding claims, wherein the at least one polymer is water-soluble and/or wherein the composition does not contain any inorganic or organic salts.
6. Composition according to any one of the preceding claims, wherein the at least one polymer, and preferably polyethylene glycol, has a molecular weight from about 3,000 to 20,000 Da.
7. Composition according to any one of the preceding claims, wherein the shell of the at least one microcapsule comprises or consists of a shell material selected from the group consisting of sol-gel polymer, polyacrylate, polyacrylamide, poly(acrylate-co-acrylamide), polyurea, polyurethane, polypeptide, polysaccharide, polyphenolic polymers, poly(melamine- formaldehyde), poly(resorcinol-formaldehyde), poly(urea-formaldehyde), or combinations thereof.
8. Composition according to any one of the preceding claims, wherein the at least one adhesion agent is selected from the group consisting of animal and/or vegetable waxes, preferably beeswax.
9. Process for the preparation of a composition comprising or consisting of a plurality of pastilles, comprising the following steps of:
(i) providing at least one microcapsule or an aqueous dispersion comprising at least one microcapsule;
(ii) melting of at least one polymer and optionally an adhesion agent;
(iii) mixing the at least one microcapsule into the polymer melt of step (ii);
(iv) admixing free fragrance or a free fragrance mixture;
(v) forming pastilles by dripping the mixture of step (iv); and
(vi) optionally cooling; optionally further comprising the step of adding at least one plasticizer and/or at least one structuring agent in or after step (ii), (iii) and/or (iv).
10. Process for the preparation of a composition according to the preceding claim, wherein the melting point of the at least one polymer, preferably of polyethylene glycol, is in the range from 25 °C to 100 °C, preferably from 40 °C to 80 °C.
11. Process for the preparation of a composition according to any one of claims 9 or 10, wherein the melting step (ii) is conducted at a temperature in the range from 25 °C to 100 °C, preferably from 40 °C to 80 °C, and even more preferred at 80 °C and/or wherein the particle size of the microcapsule(s) is in the range from 150 pm to 5 mm and/or wherein the microcapsule(s) is/are provided in the form of an aqueous dispersion.
12. Composition comprising or consisting of at least one pastille obtained by the process according to any one of claims 9 to 11, wherein said pastille comprises or consists of:
(a) at least one microcapsule encapsulating an active ingredient, wherein said active ingredient is preferably a fragrance or fragrance mixture;
(b) at least one polymer, preferably polyethylene glycol;
(c) optionally at least one adhesion agent, wherein said adhesion agent is preferably selected from the group consisting of fatty acids, fatty alcohols, fatty acid esters or mixtures thereof, such as waxes; and
(d) free fragrance or free fragrance mixture; wherein the composition has a viscosity q of less than 900 mPa s at 80 °C.
13. Use of the composition according to any one of the claims 1 to 8 or 12 for the preparation of consumer product formulations.
14. Use of the composition according to claims 13, wherein said consumer product formulation is a solid product such as a textile care product, a household product, a personal care product, a cosmetic product, a pharmaceutical product, and mixtures thereof.
15. Consumer product formulation comprising or consisting of the composition according to any one of the claims 1 to 8 or 12.
PCT/EP2023/072855 2023-08-18 2023-08-18 Perfume oil capsules for solid formulations with fragrance boost WO2025040240A1 (en)

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WO2011056938A1 (en) * 2009-11-05 2011-05-12 The Procter & Gamble Company Laundry scent additive
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