DK152293B - IN A CONTAINER PACKAGED PARTICULATE DETERGENT - Google Patents

Description

DK 152293 B

The invention relates to a container packed portion in cold-formed detergent manufactured on the basis of non-sticky or liquid non-ionic surfactants having, as appropriate, smaller proportions of anionic surfactants, with the surfactants being applied to structural carrier particles.

Particulate detergents or so-called universal detergents based on surfactants and structural substances are known. The detergent particles are round or spherical and frequently consist of aggregates of a small number of spherical particles, as obtained by spray-drying a detergent mixture on a soap mix of subsequent classification. It is also known afterwards to spray the surfaces of the spray-dried pellets with liquid, especially heat-sensitive components, such as perfume. Furthermore, detergent powder is known on the basis of nonionic surfactants, e.g. according to DE Publication 25 14 675, which still contains anionic detergents and is mixed with conventional structural substances such as alpha 1k1 iphosphates or zeolites having a particle size of 0.1 to 100 µm.

Either the non-ionic surfactants are sprayed onto the carriers or the surfactants and structural fabrics are spray-dried jointly, in which connection the detergent contains 6 to a maximum of 30% by weight of non-ionic surfactants, up to 15% by weight of anionic surfactants and relative to the non-ionic surfactants. -ionic surfactants 2 to 15 times the amount of structural substance. Furthermore, from DE publication 22 04 842 and 25 07 926 rice-resistant premixtures are known as detergents containing 1 non-ionic surfactants containing microfibre in divided silicic acid particles, on which the surfactants deposit on the outside or bond as an outer layer. These are then added to the spray-dried detergent components or mixed with structural fabrics or builder salts for finished detergents. No references to any particle size, density, and detergent structure required are provided in this literature.

In the detergent industry, it has so far been common to market pourable wash powders that were more available

DK 152293 B

2 or less rice-resistant with substantial dust parts, in cardboard boxes or large cardboard drums. The nuisance dust of the fine parts was included in these detergents, regardless of whether these detergents were poured from the carton into the washing machine or if the detergent was extracted with a measuring cup. In addition, these universal detergents were mostly formulated so that, for a normal washing process for a normal washing machine, they were sufficient in an amount of approx. 100 g.

The detergent industry, in its efforts to make highly concentrated detergents available to the user, is the only resort marketed liquid detergents dispensed from bottles, but which has the disadvantage that these mostly viscous products can only be difficult to drain and not. j- is dispensed in the right ratio and produces sticky edges and greased shutters.

SUMMARY OF THE INVENTION It is an object of the present invention to provide a rice-resistant or pourable, highly concentrated detergent which, apart from the sufficient washing power, is present in an easily manageable dry rice-resistant form, has no fine particles and can be easily filled into the container, and can be taken out by the user in a simple way.

Therefore, in order to meet this purpose, a container 25 with particulate detergent of the type mentioned initially according to the invention is used as the combination of a very specific detergent with a bottle with handles and according to the characterizing part of claim 1.

Further advantageous embodiments are described in the independent claims.

Surprisingly, it has been found that the new detergent with detergent particles contained in the determined particle size, having the small density of at least 0.5 g / cm 3 and a rice 1 edible in total corresponding to at least 70% of dry sand in silica can be dispensed in an excellent way from the bottle thus described, without the presence of an adhesive.

DK 152293 B

Washing of the detergent particles, which is otherwise the case with detergents based on nonionic surfactants. This means that the detergent can be easily dispensed without the presence of annoying dust and without any residue remaining in the bottle 5 or the bottle used as a measuring cup, respectively. In addition, both the particulate detergent as well as the container are easily manageable, in which connection the container does not show too large a bottle neck opening and can be filled 10 without difficulty and, in addition, has an aesthetic appearance and in which the inner volume of the container closure cap is filled with detergent is sufficient for a washing machine filling.

Particularly advantageous is a packed detergent in which the detergent mixture contains approx. 60 to 98% of spherical detergent spheres with a porous outer surface and a lower skeleton and approx. 2 to 40% by weight of a liquid and tacky surfactant below 40 ° C deposited in the inner region of the ball, while the outer surface of the ball is substantially free of surfactant.

2Q These detergent mixtures - especially when containing the preferred range of 70 to 95% structural spheres and 5 to 30% surfactant - exhibit a particularly good rice performance which is important both in the filling of the container and in the detergent dispenser in ng.

Particularly good particulate detergents are those based on non-ionic surfactants of ethoxylated aliphatic Gg to C22 fatty alcohols with 5 to 30 ethylene oxide units per minute. molecule produced. The structural spheres preferably consist of 45 to 85% by weight of a phosphate salt, 5 to 15% by weight of an alkali salt, and about 30% by weight. 5 to 15% by weight of water, the phosphate salt being advantageously present as a mixture of hydrated and anhydrous salt in a weight ratio of 0.3 to approx. 0.7.

A particularly favorable combination exists when the cross-section of the bottle neck of the container is in the range of 3 to 20 cm 2 and that of the handle in a range of 2 to 5 cm 2, and when further the detergent mixture has a particle size such that 95% of the particles pass through a sieve. a mesh width of 0.42 mm i

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4 and retained on a sieve with a mesh width of 0.075 mm and the density ranges from 0.55 to 0.8 g / cm 3.

Containers with the selected detergent can be particularly well filled 5 and also dispense these well when the upper wall of the bottle wall at the bottle neck opening is almost vertical and that which is closer to the handle extends at an angle of 30 to 60 °. Preferably, the bottleneck has an outer thread, while the closure cap has an internal thread and is sized in size as measuring cups which take up half and one-third and one-fourth, respectively, of the amount needed to wash a washing machine's wash.

The subject matter of the present invention is explained in more detail below on the basis of the drawing. On this, FIG. 1 is a side view of a partially formed detergent product loaded onto an un-sealed container; FIG. 2 shows the product from above; FIG. 3 shows the product from the handle side, fig. 4 is a section along the plane 4-4 of FIG. 1, FIG. 5 is a side view of a portion of the device shown in FIG. 1-4 with a closure cap; FIG. 6 is a photograph of a larger portion of a spray-dried builder ball or particle prior to spraying with a surfactant to obtain a free-flowing detergent, magnified 200 times; FIG. 7 is a sectional view of the one shown in FIG. 6 is enlarged 2000 times and FIG. 8 is a schematic representation of the order of the filling operations and stages.

In FIG. 1 shows a bottle 11 of transparent polyvinyl chloride plastic with a body part 13 with a handle 15, which is blow molded in one

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s with the body, and a neck portion 17. Preferably, the bottle has a substantially oval cross section, at least in the upper and lower regions. The bottleneck is positioned at the top of the bottle and towards one of the ends of the oval horizontal main axis, and the handle is at or near the opposite end of the main axis. Preferably, the upper part 14 of the body wall 12, namely the part which is closer to the bottle neck opening, extends almost vertically, namely at an angle from 70 ° to 90 ° relative to the horizontal. The upper portion 16 near the handle end may extend less vertically, namely at an angle of 30 to 60 °. In the bottle 11 there are detergent particles 19 which can be easily poured through an opening 21 in the bottle neck by tilting the bottle.

In FIG. 4, a portion of the main volume 23 of the bottle is illustrated, as well as a portion of the internal flow path 25 through the handle 15. As shown, both are filled with particulate detergent 19.

In FIG. 1 through 4, the bottle is shown without a cap. For normal closure and shipment use a screw cap 27, shown in FIG. 5, 20 on the threaded neck 17. Normally the material of the cap is sufficiently elastic so that sealing discs are not needed. Frequently, sealing inserts are sufficient.

In FIG. 6 and 7 are the bright areas reflections from the skeletal areas of the pellet whose inner and outer parts help to stabilize it. The dark areas show voids in the sphere into which liquid or dissolved surfactants can penetrate after they are sprayed or otherwise applied to the structural fabric beads to produce a sphere surface substantially free of detergent and which .g. has less than 10% detergent in the outer areas. The ball illustrated in FIG. 6 and 7 is one obtained by spray drying. It contains approx. 18.8 parts of pentane sodium tripolyphosphate hexahydrate, 7.6 parts of sodium silicate (Na 2 O: SiO 2 = 2.4), 28.3 parts of pentane sodium tripolyphosphate (anhydrous) and 49.6 parts of water. Spray-dried, the moisture content is approx. 10%.

In FIG. 8, six steps are shown when filling the bottle 11 with the detergent 19. A filling head 29 has a retractable filling nozzle - 6

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31 with a control valve 33. In the first step, the filling head is placed over the empty bottle 11. In the next step, the nozzle 31 is partially lowered into the bottle neck 17, but the filling with detergent has not yet begun. The next step illustrates the filling of detergent 19 in the bottle 11. The filling level is approx. half the height at which the handle mouths the bottle's main compartment. The filling level 37 in the handle 15 is lower at this time. In the fourth step, the filling height is increased. The detergent is now above the flow opening 25 and the detergent 19 fills the flow opening to the filling level 39. In the fifth step, the particles 19 have been filled to the final filling level 41. In the sixth step, the nozzle 31 is pulled out. In a subsequent step, the bottle is closed automatically or manually.

15

The bottle used for the present product may be of any suitable material, although synthetic organic polymeric plastic materials such as polyvinyl chloride, polymethyl methacrylate, polyethylene terephthalate, poly-2Q ethylene, polypropylene, polystyrene, polyesters and polyethers, preferably fiberglass, is preferred. Glass bottles can also be used. It is preferred that the bottles used are transparent, but it is within the present invention to use opaque and transparent plastic varieties. A significant advantage of said bottle

Δ O

materials are that they are substantially or completely water resistant and that they also impede the transmission of organic volatile substances such as perfumes even with relatively thin walls, ie. ca. 1 to 3 mm thick walls.

3 0

The bottles may have different shapes. Unlike other containers, they have a relatively narrow neck portion which has a small opening relative to the average cross-sectional area of the bottle. Generally, such a cross-sectional area is less than 40¾ of the average bottle cross-section, preferably less than 30% of this and especially less than 25% of this. To facilitate easy pouring and good control of the dispensing, the bottleneck cross section should be from 2 to 40 cm 2, preferably 3 7

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to 20 cm 2 and in particular 5 to 15 cm 2. The neck is usually oriented such that its flow opening and walls are parallel to the vertical axis of the bottle, but it may also have a slope, usually no more than 30 ° from the vertical, but larger slopes also work. The size of the neck is partly dependent on the volume of the bottle and partly on the cap size desired for dispensing the detergent. For 1/4 or 1 liter bottles, neck heights of 1 to 5 cm can be used, but these heights will usually range from 1.5 to 3 cm. For larger sizes 10 such as 2 and 4 liter bottles, the necks may also be from 1 to 2 cm high, but preferably from 2 to 5 cm. Other bottle dimensions are adapted to the volume of the bottle if the bottle is of the illustrated or modified design.

Various designs and cross-sectional shapes can be used for the bottle, but the most preferred cross-section is substantially oval, and the bottles illustrated in the drawing are considered to belong to this category. Occasionally, it is desirable to transform the round curves of such an oval into an approximately four-2Q angular shape. Such altered forms are also considered oval. Instead of oval cross-sections one can use other waveforms such as circular, elliptical (considered oval in bottles), regularly polygonal, e.g. rectangular, square, or polygonal with round corners.

25

Although not an essential feature of the present invention, with the bottle in one shaped hollow handle that is frequently blow molded or otherwise conveniently formed in one piece with the neck and main areas of the bottle, a very important characteristic of the bottle is compatible with the present detergent composition. The handle of the handle is in conjunction with other inner areas of the bottle so that the detergent can be filled in and flow from it. The handle is located at a bottle side opposite to the neck or pour spout and does not extend beyond the normal bottle wall. The handle is not formed outside of the bottle, but is formed by omitting material within the general circumference of the bottle. The handle need not have a regular cross-section or an inner 8

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flow area, but a substantially regular or uniform flow path is preferred. The hollow handle must have at least one internal cross-sectional area in the range of 1 to 10 cm 2, preferably 2 to 5 cm 2. Normally, the handle has a comfortable length to be easily grasped, which length has been determined to be from approx. 8 to 12 cm, preferably 9 to 11 cm. Such a height for a hollow handle section is easily filled by the high-density flowable, dust-free particulate detergent of the present invention, and this will readily flow from the handle when dispensed.

In this regard, it is desirable to have a free height above the top of the handle flow opening, between the desired level of loading of the particles and the top of the handle flow opening of at least 1 cm and preferably at least 5 15 cm, heights up to 10 or 15 cm being useful. connection with larger containers. The inclination angle of the wall 16 is greater than or about equal to the normal frictional angle of the particulate detergent at rest after storage during filling or after pouring, and consequently facilitates filling of 20 and emptying from the handle's orifice opening.

The detergent in the bottle has an improved flowability, increased bulk density and a particle size distribution to promote flow and venting of gases, thereby reducing the tendency for bridging in the container or in narrow areas thereof. The detergent composition of the particles contains a surfactant and a structural substance or builder for such detergent and may comprise usual additives.

As surfactant, anionic, nonionic, cationic, ampholytic or amphoteric surfactants can be used. Of these, the anionic and nonionic surfactants are particularly preferred, the nonionic being most suitable for the present composition. Generally, cationic surfactants are not used for the present products, and this is especially true when anionic substances are present. Although nonionic surfactants are preferred, mixtures of nonionic and anionic surfactants are sometimes preferred.

9

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The nonionic surfactants may be liquid or semi-solid at room temperature and will usually be liquid or sticky at a temperature below 40 ° C. Preferred nonionic surfactants are ethoxylated aliphatic alcohols having especially straight but also branched chain having from about 8 to 22 carbon atoms with approx. 5 to approx. 30 ethylene oxide units per molecule. Particularly convenient nonionic surfactants of this kind are based on a higher alcohol of 12-15, especially 14-15 carbon atoms, which are condensed with an average of 7-11 ethylene oxide units. Another suitable class 10 of ethoxylated aliphatic alcohols consists of a mixture of primary alcohols having 16-18 carbon atoms which is ethoxylated and contains 65 mole% ethylene oxide.

Further examples of non-ionic surfactants are those marketed by BASF Wyandotte under the trademark "Pluronic" ®. Such compounds are prepared by condensing ethylene oxide with a hydrophobic base formed by condensing propylene oxide with propylene glycol. The hydrophobic portion of the molecule has a molecular weight of from ca. 1500 to approx. 1800, and the addition of polyoxy-2g ethylene (or ethylene oxide) to such a hydrophobic moiety improves as a whole the solubility of the molecule, whereby the detergent remains liquid at room temperatures up to a polyoxyethylene content greater than ca. 50%. Useful nonionic surfactants are also the polyethylene oxide condensates with the alkyl phenols, such as condensation products, wherein the alkyl group contains from ca.

2 to 6 to 12 carbon atoms, in either a straight or a branched chain form, with 5 to 25 moles of ethylene oxide per liter. mole of alkylphenol. The ΑΊ-cooling substituents can e.g. be polyroerized propylene, diisobutylene, octene or nonen.

3 0

Suitable anionic surfactants are the higher fatty acid soaps obtained from natural or synthetic higher fatty acids having from 8 to 20 carbon atoms or from triglycerides, e.g. coconut oil, sebum, hydrogenated coconut oil, hydrogenated sebum and mixtures thereof, further linear linear alkylbenzene sulfonate,

3 S

wherein the alkyl group has 10 to 18 carbon atoms, preferably 12 to 15 carbon atoms, e.g. linear sodium tridecylbenzenesulfonate, paraffin sulfonates, olefin sulfonates and other organic 10

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sulfonates and sulfates in which a lipophilic group is present, usually with a chain of 10 to 18 carbon atoms. The described nonionic compounds can be converted to anionic compounds by sulfation or sulfonation. Usually, this occurs in advance on the terminal hydroxyl groups. In such cases, the proportion of ethylene oxide to produce the primary nonionic condensate product decreases such that there will be from 3 to 12 moles, preferably 5 to 10 moles of ethylene oxide per liter. moles of anionic surfactant present.

10

The anionic surfactants are preferably used as sodium salts, although potassium salts and in some cases small proportions of ammonium or triethanolamine salts can also be used.

Representative cationic surfactants generally also have 15 fabric softening and antibacterial properties. This is especially true for Quaternary compounds. Examples of such compounds are distearyl dimethyl ammonium chloride and 2-hepta-decyl-1-methyl-1 - [(2-stereoylamino) ethyl] -imidazolinium methyl sulfate. Various amphoteric surfactants are also marketed. These are generally higher carboxyl atoms, phosphates, sulfates or sulfonates containing a cationic substituent such as an amino group quaternized with a low chain alkyl group or with a condensate product thereof on the amino group by condensation with a low chain alkylene oxide.

25

Further proper surfactants are described in McCutcheon's "Detergents and Emulsifiers," 1973 Annual, and in "Surface Active Agents," Volume II, by Schwartz, Perry, and Berch (Interscience Publishers, 1958).

30

It is particularly preferred that the builder or structural substance be made up of inorganic substances, especially water-soluble salts, especially phosphates. However, organic structural substances such as sodium citrate, sodium gluconate, trisodium nitrite acetate and other organic compounds having structural activity are also frequently found in admixture with inorganic substances and may be processed into a free flowing detergent. Generally, the organic compounds will be present as sodium

DK 152293 B

11 µm or other alkali metal salts, but sometimes the free acids can be used. Although the phosphates are highly preferred for the production of exceptionally free-flowing particles in large bulk weight-containing materials and containing large amounts of surfactant, which are preferably later added to the said phosphate-based pellets, other inorganic substances can also be used as structural substances or in combination with these, such as silicates, borates, carbonates and bicarbonates. Ion-exchanging clays that act as detergents in the detergent mixture to remove hard water inducing ions from the water, such as type A (preferably 4A) molecular sieves and other suitable molecular sieves, can be used as structural substances in combination with a suitable phosphate. However, with non-phosphate-containing detergents, they can be used with other non-phosphate-containing structural substances, alone or with other ion-exchange zeolites.

In the case of phosphates and the other inorganic water-soluble structural salts, sodium salts are normally used, but potassium salts can be used. Specific examples of phosphate structural salt are pentane sodium tripolyphosphate, other sodium tripolyphosphates such as trisodium tripolyphosphate, trisodium phosphate, disodium phosphate, monosodium phosphate, tetrasodium pyrophosphate and disodium pyrophosphate. The corresponding potassium salts may also be used, but are preferably used in combination with the sodium salts.

Preferred adjunct structural substances which also have anti-corrosion properties in the disclosed detergent and assist in forming the desired beads in the preparation of the structural substances subjected to subsequent spraying or spraying of surfactant are the alkali metal silicates commonly applied in form of aqueous solutions containing approx. 40 to 60% by weight, typically approx. 50% by weight of solid silica ter. Such silicates are preferably sodium silicates having the ratio of Na 2 O: SiO 2 from 1: 1.6 to about 1: 3.4, preferably 1: 2 to 1: 3 and especially about 1: 2.35 or 1: 2.4.

Along with the detergent composition and in addition to the surfactants and structural components, various adjuvants may be

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12, usually preferably incorporated into the structures of the particles, either by spray drying them with the particles of a common mixture in a soap mixer or, when heat sensitive, by adding them afterwards. Among such auxiliaries are known functional and aesthetic agents such as bleaching agents, e.g. sodium perborate, coloring agents, e.g. pigments, dyes and optical brighteners, perfumes, foam stabilizers, e.g. alkanolamides such as laurine myristine diethanolamide, enzymes, e.g. proteases, amylases, skin protection and conditioning agents, e.g. low molecular weight water-soluble proteins made by the hydrolysis of protein-containing materials such as animal hair, hides, gelatine, collagen, foam-destroying agents, e.g. silicones, fabric softeners, e.g. ethoxylated lanolins, bactericides, e.g. hexachlorophen, buffering agents, e.g. alkali metal acetates and bisulfates and flow enhancers, e.g. painted clays. In addition, filling salts such as sodium sulfate, generally anhydrous, and sodium chloride may be present, but it is currently best to avoid them.

20

Detergent party in the clothes in the holder usually approx. 50 to 98% of structural substances and the rest are surfactants except for other substances, including water. Considering the presence of other substances in products, it will normally contain from 30 to 80% structural materials, 2 to 35% or 40% surfactant, 10 to 20% additives other than fillers, 0 to 50% fillers and 3 to 15 % moisture. The detergent of the invention may be prepared in the desired manner (including spray drying of the entire composition of heat-stable substances. However, to obtain the 3Q best flowability, least dust and maximum bulk weight and least possible undesirable chemical reactions and decompositions of the components, it is preferred to prepare a ground ball These surfactants are liquid non-ionic or mixtures of anionic and non-ionic surfactants, although anionic surfactants can sometimes advantageously be spray dried with the structural substance. preparation of the particles of about 60 to

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13 approx. 98¾ of the structural materials and have porous outer surfaces and spherical inner structures. They consist of approx. 2 to approx. 40% by weight of surfactants, such as those which are liquid or sticky at a temperature below 40 ° C. These are incorporated into the beads 5 so that these outer surfaces are substantially free of surfactant and therefore free flowing. In the preferred embodiment of the present invention, the detergent consists of 70 to 75% base beads and 5 to 30% surfactants, and the base beads consist of 45 to 85% of a phosphate structure salt of ca. 10 to approx. 15% alkali metal silicate and of approx. 5 to approx. 15% water. In particularly preferred embodiments of the present invention, the surfactants are a nonionic polyethoxylated surfactant derived from aliphatic alcohol having from about 8 to approx. 22 carbon atoms in a chain and condensed with from approx. 5 to approx. 15 moles of ethylene oxide per moth. The phosphates are preferably a mixture of hydrated and anhydrous salts with the weight ratio of hydrate in serous phosphate, generally pentane sodium tripolyphosphate hexahydrate and anhydrous phosphate, usually pentane sodium tripolyphosphate, anhydrous, in the range of about 0.3 to about 20 0.7, preferably 0.4 to 0.6.

The particles are usually dust-free. Even after being shaken in a transparent container, the space above the product will be clearly as short as 1 or 2 seconds after cessation of shaking and none of the product will adhere to the inner walls of the container. Such desirable non-dusting properties can be partly attributed to the content of nonionic surfactant, which is normally present in a sufficient ratio to bind the dust and to prevent it from forming by the movement of the particles. Thus, the amount of nonionic surfactant used can range from 12 to 40% of the product, and sometimes the ratio used will be as much as 20 or 25 to 40% of the final product. This proportion is sorbed in the interior of the detergent particles described, without the surfaces becoming sticky or having poor flowability. Representative for

ISLAND ISLAND

Particularly preferred nonionic surfactants used are the condensation product of an aliphatic alcohol having from 10 to 18 carbon atoms in the chain, with 6 to 14 moles of ethylene oxide per liter. mol 11

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product. Especially with a content of 20 to 40% in the detergent, the percentage of particulate detergent passing a sieve with a mesh width of 0.045 or 0.075 mm is frequently zero. The presence of a more sorbable surfactant in the particulate product and the resulting high density naturally leads to a smaller consumption of the product per unit weight. wash. This makes it easier to pack in bottles and dispense smaller amounts of detergent and measure them in the bottle cap.

In cases where the dust formation is noticed only in very small quantities, the interior of the bottle can be coated with a thin layer of silicone and / or said quaternary ammonium salt to smooth the inner bottle surface and promote the diffusion of any electrostatic charge present in the bottle , that fine particles bond to the inside of the bottle. Normally, the amount of such materials used will be sufficient to form a thin layer on the inside of the bottle, often only 1 to 10 molecules thick.

The cap of the bottle may be of any suitable construction and any suitable material, but it is preferred to use screw caps as they are readily available, close easily and have good measurement properties. Since the product contained in the bottle is a particulate solid and not a liquid, complete sealing is not always necessary. He can therefore use other cap forms that do not have the sealing properties of the normal screw caps. Eg. For example, one can use caps that are inserted into the press fit, as well as ones that include a sliding valve to open a dispensing flow opening. In such and other cases, the neck portion can be made flatter than that of screw caps and can be reduced to an opening in a bottle wall. The material for constructing the cap can be any suitable material, including synthetic organic polymeric plastics, rubber, especially hard rubber, metals and metal alloys. Among the uses-35. ,.

deuge synthetic organic polymers include melamine formaldehydes, phenol formaldehydes, polystyrols, (dense or from foamy beads), fiberglass reinforced polyesters, polypropylene and polyethylene.

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15

The internally threaded caps preferably form a tight closure with the neck of the bottle when screwed into place. They prevent loss of content and prevent the ingress of moisture or other external contaminants into the contents or transmission of moisture vapors from the bottle. Due to the screw type structure and the barrier properties of the bottle, an effective and inexpensive seal is obtained.

Therefore, special barrier linings or coatings normally used on permeable containers to pack detergent powders are superfluous. Furthermore, although the cap is relatively small, it can be used to measure desired amounts of detergent particles. In practice, screw caps are of such size that they can be used to seal openings in bottles of usable size, e.g. from 1 to 4 liters, not big enough

1 O

for example, a cap-filled or even four-cap can contain the volume of ordinary detergent particles to be filled in an automatic washing machine for one wash. With a known spray-dried detergent powder with a room weight of approx. 0.3 20 g / cm 3, after which a small amount of non-ionic surfactants is sprayed, should be approx. 90 g or 300 cm 3 of detergent particles are loaded into a 64.4 liter washer. The normal bottle cap only has a volume of 5 to 15 cm3. Even with a volume of 15 cm3, one should measure approx. 20 full caps of such a normally low-density powder detergent. This would not be acceptable to the user, nor would it be advantageous to follow such a method instead of using a regular measuring cup. However, according to the invention, a package with a slightly larger cap can be used and make metering possible. With the larger amount of surfactant, such as a liquid nonionic surfactant which can be incorporated into the present small balls, it is possible to halve the required amount of detergent product needed per wash. With larger space-weight balls e.g. 0.6, an additional 35 halves of the required volume are obtained. By simply making the cap slightly larger so that it gives a volume of approx. 20 cm3 instead of 15 cm3, the measurement of four hooded detergent powders will provide sufficient for a regular wash in

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16 a machine filled from above. For machines that are filled from the side, where generally half of the amount of detergent is used, the measurement of two hoods will suffice. By further regulating the product's body weight, its content and surfactant and the cap size, it is possible to use as little as one cap detergent per unit. wash or as much as three hoods. Thus, the present invention provides a convenient means for easily measuring an amount of particulate detergent in a bottle cap of the bottle-filled particulate detergent to provide the desired amount of detergent for a common wash.

Methods for preparing free-flowing particle-sized detergents of high bulk weight and desired particle size 10 are known and can be used in accordance with the present invention. Controlled spray drying, spray cooling, agglomeration, solidification, sanding of crystalline materials, etc. are known and suitable. Nonionic surfactants can be incorporated into bases spared in kels or formed together with the particles as long as the particles have a desired, sufficiently rounded or rounded structure to be free flowing and contain any liquid or sticky surfactant material internally in the interstices. in the interior of the particle and not on this surface.

Usually less than 20% will be on the surface and preferably less than 10%. After preparation of the detergent particles, they are filled into bottles and the bottles are closed with a cap by a method similar to that illustrated in FIG.

8, but other more complicated and less satisfactory filling methods may also be used. After the bottle is

O U

closed tightly, the product's shelf life is almost unlimited, in most cases in practice for at least three years, without any unwanted changes.

The product of the present invention has a large number of advantages, many of which have already been mentioned. A relatively inexpensive and easily obtainable container with a built-in hollow handle can be used with known sealing means, which 17

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results in the product having excellent storage properties. The particles are rounded in an attractive way, have a uniform shape and flow like a liquid. They are heavy enough that they can be measured in a relatively small cap, and have a many-five-fold washing power at reasonable bottle size. 1 liter of detergent is e.g. enough for approx. 10 to 20 washes, usually approx. 12, while marketed liquid detergents are only enough for approx. 8 washes per liter. In addition, the cap can be divided for finer measurements. The product is easily manufactured and enables a simple way to incorporate normally heat ustabi 1 e components therein. Since it is not in a liquid phase, storage stability is also improved.

This makes it possible to use certain less stable and more effective cleaning ingredients in the composition.

The following examples illustrate, but do not limit, the present invention. Unless otherwise stated, all parts are parts by weight and all temperatures are in ° C.

Example 1

An aqueous slurry is made up of 14.5 parts of anhydrous pentane sodium tripolyphosphate powder, 15.2 parts of 50% aqueous solution of sodium silicate (Na 2 O: SiO 2 = 1: 2.4) and 21 parts of demineralized water. The slurry is brought to a temperature of approx. 60 ° C and mixed well in a soap mixer to form the hexahydrate salt of pentane sodium tripolyphosphate. The starting mixture thus prepared in the soap mixer is then heated to 88 ° C and maintained between 88 ° C and 93 ° C to prevent the hydration of anhydrous sodium tripolyphosphate powder, which is then dried.

v U

utes are added. The total mixture in the soap mixer is then prepared by adding 28.3 parts of anhydrous pentane sodium tripolyphosphate powder and 21 parts of deminera 1 in serified water at said temperature range between 88 and 93 ° C. The resulting mixture contains from ca. 45 to approx. 50% by weight of solids due to the hydration of small amounts of the anhydrous tripolyphosphate and moisture loss.

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18

The mixture is pumped to a 2.8 m high counterflow spray drying tower and sprayed at a diffuser temperature of 82 ° C and at a pressure of approx. 54 kg / cm2 (absolute) through a Whirljet 15-1 spray nozzle into the dry air having an outlet temperature of 5 approx. 315 ° C as it flows into the spray tower.

The spray-dried base balls produced have an internal structure and outer surface characteristics like the balls shown in FIG. 6 and 7, and rounded, irregularly-shaped solid particles are formed with sponge-like porous outer surfaces and spherical inner structures, unlike known spray-dried detergent bodies having a substantially continuous outer surface and a hollow core.

The spray-dried base balls consist of 77% sodium tripolyphosphate, 13% sodium silicate and 10% moisture. The bulk weight is 0.55 g / cm3 and the flowability is 86% of the dry sand flowability and the product is not sticky.

These base balls are introduced into a rotary batch drum mixer 20 and post-sprayed at 49 ° C with an anionic surfactant based on a 7 to 11 ethylene oxide units condensed with C₂₂_c1515 alcohol and minor amounts of a coloring agent, perfume and clarifier to produce a final product consisting of 78% base balls, 19.7% of the anionic surfactant and 2.3% other components. In other experiments, the liquid anionic surfactants were applied and the other components present in smaller proportions or aqueous solutions or dispersions thereof in the form of fine droplets or mist on the shaken base balls in mixers.

30

The obtained products had a density of 0.68 g / cm 3 and a flowability of 79% and did not show any stickiness. The structural analysis of the spheres of the spheres and detergent spheres was as follows:

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19

Sieve passage Structural-Detergent- with mesh width_beads_beads_ of 0.8 mm 1% 1% through 0.8 and 0.45 mm 19% 20% 5 through 0.45 and 0.25 mm 50% 52% through 0, 25 and 0.18 mm 20% 20% through 0.18 and 0.15 mm 6% 5% through 0.15 and 0.075 mm 3% 2% through 0.007 mm 1% 0% 10

The finished product obtained after only 10 minutes of mixing is filled at room temperature to bottles of the kind illustrated in FIG. 1 - 4 and in the manner shown in FIG. 8th

The bottles are clear polyvinyl chloride bottles and have a volume of approx. 2 liters. They are filled by gravity with the product without damage, with the average filling time being approx. 5 seconds per bottle or smaller, and also filling the hollow handle without encountering any problems. After filling, the bottles are appropriately supplied by mechanical means with 20 caps, and the manufactured products are packed in boxes and shipped in stock. Based on previous experience with storing powerful detergents and experiments carried out on these, it is assumed that the products have a storage stability of more than 3 years.

25

Sufficient product to cause a concentration of 0.075% in a 64.4 liter wash tank is provided with 75 cm 3 of detergent which can be measured in a cap of approx. 5 cm and 4 cm high or by means of two full caps with a diameter of 30 cm and 3 cm high. The former cap size is used with the bottle illustrated and described herein.

When the detergent is used in a top-loading washer which has a capacity of approx. 64.4 liters, to wash 35 a normal amount of washing (about 4 kg), a good washing result is obtained. Similarly, the laundry is effectively washed when using half as much in a front-loading washer. In use, the product flows freely out of the bottle and out

DK 152293 B

20 the hollow handle and is not easily spilled, as is the case with liquids, leaving no unwanted gel or binder-like coatings on the cap or thread of the bottle.

The product produced is attractive and can easily be identified by staining some or all of the particles in it by post-spraying some particles of color.

Instead of producing the detergent particles in accordance with the process described above, products of the same density, particle size and flowability, which are also non-sticky, can be prepared by spray cooling, agglomeration and abrasive methods known in the manufacture of particulate molds. detergents. There are useful particulate detergents having the desired washing properties. However, the detergents produced by the method described earlier in this example are better than the products made by the other methods, being generally more attractive, 20 streams freer, and having a larger volume weight than products of similar size. materials.

Example 2 A product such as that described in Example 1 is prepared essentially by the same process, using an initial mixture of 25 parts hot water (60 ° C), 3.5 parts solid sodium silicate and 13 parts anhydrous pentane sodium tripolyphosphate powder. and mixing the slurry well in a double-walled vapor sheath vessel to hydrate the phosphate to hexahydrate and then heat at steam to 93 ° C, at which temperature 13 parts of anhydrous tripolyphosphate, 25 parts of water, an additional 13 parts of anhydrous tripolyphosphate are then added. and 7.5 parts of anhydrous sodium carbonate 35 for the mixture in the soap mixer. During mixing, the temperature should not fall below 82 ° C to prevent hydration of the then anhydride tripolyphosphate added. The mixture is sprayed at a pressure of 57 bar (absolute) into a spray tower

DK 152293 B

21 with a temperature of 343 ° C for the introduced dry air and a temperature of approx. 113 ° C for departure 1 night. The fabric particles produced have a particle size distribution such that 90% by weight passes through a screen having a mesh width of 0.8 mm and is retained on a screen having a mesh size of 0.075 mm.

78 parts of the spray-dried spheres are then sprayed by the procedure described in Example 1 with 19.5 parts of surfactant and 2.5 parts of less abundant ingredients (optical preparations and perfumes) while shaking in an inclined manner. cylindrical shaking means for approx. 5 minutes. The extracted product has a space weight of approx. 0.75 g / cm3, a flowability of 75% and a moisture content of approx. 5%. It is charged to the bottles described by the method described in Example 1 and tested for its suitability as a coarse detergent. It was found to be very satisfactory in that it had the desired properties previously discussed for the product of Example 1.

Example 3 20

The procedures of Examples 1 and 2 are followed to prepare a base ball from 13 parts of sodium tripolyphosphate hexahydrate, 26 parts of anhydrous sodium tripolyphosphate, 47 parts of demineralized water, 7.5 parts of organic structure, and 6.5 parts of solid sodium silicate (Na : SiO 2 = 1: 2.4). Eighty-five parts 9c of the resulting spray-dried structural spheres are sprayed with 12 parts of surfactants and in minor amounts (fluorescent preparations and perfumes). The resulting detergent passes the samples mentioned in Examples 1 and 2 and is a free-flowing, dust-free, attractive detergent-30 part with high room weight and good washability.

Example 4

The experiment described in Example 1 is repeated using "Alpha-nic" 1618-65 as the non-ionic surfactant to prepare a granular detergent having a non-ionic surfactant content of 30%, the proportions of the other components being reduced accordingly. . the product obtained is an excellent detergent, and!

DK 152293 B

22 the corresponding bottle-shaped particulate detergent has excellent stability and usage characteristics.

Example 5 5

The experiments of Examples 1-4 above are repeated with various bottles and detergents. The component proportions are varied by ± 10%, ± 20% and ± 30% while maintaining the proportions and ratios required by the invention. Filling in different bottles with caps of different materials and constructions was also made within the limitations thus given. Together! Iqninasforsøq

A bottle of detergent packaged in Example 1 and FIG. 1C was subjected to a consumer survey on the characteristics below, with the product most commonly used by the consumer concerned being drawn up for comparison. Hereby the following values were obtained in two different geographical areas, as indicated in the table: 20 25 30 35

DK 152293B

23

Table 1_

Geographical Features- Geographical Advice Chicago Advice Minnesota Product Together- St. Paul according to the equation product invention according to the equation product invention the product

Good outflow conditions 59 25 56 27 easy dosing 51 29 56 27 simple handling 52 30 58 27 10 well visible in the container 47 22 46 20 pure textile odor 48 30 41 27 no residues 34 25 29 24 suitable for all textiles 36 33 32 25 removal of aim . dirt 39 30 29 21 washing effect with 1/4 closing volume per. washing 34 21 24 17 economic use 30 28 27 25 1 clearing effect on colored textiles 24 24 10 15 bleaching effect in connection with white text in clay 26 24 17 24 removal of body stains 23 22 15 18 removal of food stains 17 22 6 14 20 removal of fat and oils 18 18 8 16 In a further comparative experiment, marketed detergents were loaded into a bottle of FIG. 1 and examined in terms of outflow capability. The comparison products flowed out of the bottle more slowly, had dust generation and flowed uniformly, so that a correct measurement in a measuring cup was hardly possible.

In a further experiment, the product of application 30 was compared to five of the most well-known products on the US market. Determining the density of the detergent, when used in practice, is the scale ratio of the detergent's weight in grams taken from a measuring cup or screw cap. The following Table 2 shows that the comparator products have a lower "cup" weight and a lower density than the product of the invention, which in turn means that a larger detergent volume is used to provide the corresponding amount of detergent . The difference between the

Claims (9)

10 VP-AP 111 - 148 3/4 - 1 140 110.3-147 3/4 - 1 147 Product according to the invention 38.8 1/4 155 Patent claims. 15 1. In a container packed particulate detergent characterized by the combination that a) the container is a transparent plastic bottle with a neck located in the upper region of the bottle 20 with an outlet opening whose cross section is less than 40% of the average cross section of the bottle body and is 2 to 40 2 cm, and that the bottle has a hollow handle integral with this hollow handle, the interior of which communicates with the inner compartment of the bottle and whose cross-sectional areas are 1 to 10 cm2, with the bottleneck opening located close to one end thereof. (b) the particulate detergent is a free-flowing detergent mixture whose particle size has dimensions such that at least 90% of the particles pass through a screen having a mesh width of 2.35; mm and retained by a sieve with a mesh width of 0.075 mm, has a density of at least 0.5 g / cm3 and a flowability equal to at least 70% of dry 3g sand flow and that it is constructed on the basis of tacky or liquid non-ionic surfactants with, where appropriate, smaller proportions of anionic surfactants and at which the surfactants are placed on structural carrier particles. DK 152293 B Detergent container according to claim 1, characterized in that the detergent mixture contains approx. 60 to 98% detergent pellets have the structural fabric with a porous outer surface and with an inner skeleton and a tacky surfactant deposited on the inner region of the pellets, while the pellets outer surfaces are substantially free of surfactant. Detergent container according to claim 2, characterized in that the detergent contains 70 to 95% structural spheres and 5 to 30% surfactant. Detergent container according to claim 3, characterized in that the surfactant is an ethoxylated C8 to C22 aliphatic fatty alcohol containing 5 to 30 ethylene oxide units per liter. and that the structural spheres 1 contain 45 to 85 wt.% of a 15 phosphate salt, 15 to 15 wt.% of an alkali sieve 1 in cat, and approx. 5 to approx. 15% by weight of water and wherein the phosphate salt is built up as a mixture of hydrated and anhydrous salt in a weight ratio of 0.3 to approx. 0.7. Detergent container according to claim 4, characterized in that a) the cross-section of the bottleneck is within a range of from 3 to 20 cm 2 and that the cross-section of the handle is in a range from 2 to 5 cm 2 and that b) the detergent mixture has a particle size such that 95% of the particles pass through a 0.42 mm open mesh screen and are retained by a 0.075 mm open mesh screen and the density 30 ranges from 0.55 to 0; 8 g / cm3. Detergent container according to one of claims 1 to 5, characterized in that the upper area of the bottle wall is almost vertical at the bottle neck opening and the area closer to the handle extends at an angle of 30 ° to 60 °. Packaged detergent according to claims 1 to 6, characterized in that the bottle neck has an outer thread and that the closure 26 DK 152293 B has an inner thread and for its size is designed as a measuring cup which takes up 1/2 and 1/3 or 1/4 respectively of the amount required to wash the wash in a washing machine. 5 10 15 20 25 30 35