AU698882B2 - Fabric softening composition - Google Patents

Description

i WO 95122594 PCTIEP95/00624 FABRIC SOFTENING COMPOSITION The present invention relates to fabric softening compositions, in particular the invention relates to aqueous dispersions of biodegradable fabric softening compositions comprising a water insoluble cationic fabric softening agent and perfume. The compositions are stable on storage and exhibit excellent perfume delivery when removed from a washing machine.

Rinse added fabric softener compositions are well known.

Typically such compositions contain a water insoluble quaternary ammonium fabric softening agent dispersed in water at a level of softening agent up to 7% by weight in which case the compositions are considered dilute, or at levels from 7% to 50% in which case the compositions are considered concentrates. In addition to softening, fabric softening compositions desirably have other benefits such as delivering perfume onto fabrics.

The fabric conditioning market is moving towards more concentrated compositions. One of the problems associated with such fabric softening compositions is that on storage they are physically unstable. This problem is accentuated by the presence of a perfume; the greater the level of perfume the worse the stability problem becomes.

r Physical instability manifests itself as a irreversible thickening on storage of the composition to a level where the composition is no longer pourable and can even lead to the formation of a gel. The thickening is very undesirable since the composition can no longer conveniently be used.

WO 95122594 PCT/EP95l00624 2 In the past physical stability of rinse added fabric softener compositions has been improved by the addition of viscosity control agents or anti-gelling agents. For example in EP 13 780 (Procter and Gamble) viscosity control agents are added to certain concentrated compositions. The agents may include C,,-Cie fatty alcohols. More recently in EP 280 550 (Unilever) it has been proposed to improve the physical stability of dilute compositions comprising biodegradable, ester-linked quaternary ammonium compounds and fatty acid by the addition of nonionic surfactants. EP 507 478 (Unilever) discloses a physically stable fabric softening composition comprising a water insoluble, biodegradable, ester-linked quaternary ammonium compounds and a nonionic stabilising agent.

With concentrated compositions comprising biodegradable ester-linked quaternary ammonium compounds the problem of physical instability is more acute than with traditional quaternary ammonium compounds.

CA 1 111 616 (Procter and Gamble) discloses a fabric softening composition comprising 0.1 to 10 wt% of a cationic fabric softener and 0.1 wt% to 20 wt of particles. The particles are comprised of a carrier substance and a perfume and have a melting point of from 38"C to 150'C, preferably from 65°C to 100'C.

We have now found that fabric softening compositions comprising quaternary ammonium compounds may exhibit excellent perfume substantivity and good storage stability.

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Thus, according to one aspect of the invention there is provided a fabric softening composition a fabric softening composition comprising: Lr 3 WO 95/22594 PCTIEP9:5100624 i) a quaternary am'moniurm. fabric softeni.ng agent, ii) from 0.1 wtW to 10 wt% of a perfuxnecarrier substance mix having a slip point below The slip point of the perfunie'carrier substance mix is measured as defined by British Standard BS 684 section 1.3 1991 ISO 6321:1991 (UK).

A further aspect of the invention i.s provided by a~ process for preparing a fabric softening composition as defined above, which comprises of the follcwinq steps: i) forming an aqueous dispersi.on of the quaternary ammoniumn fabric softeni.ng agent; ii) adding the perfume/carrier substance mix to the resulting dispersion.

one advantage of such a process is that it is simple. A further advantage afforded by the present invention is that the degree of fabric softening may be varied to suit different customer requirements in different markets, while maintaining high perfume delivery.

The invention also allows perfume to be incorporated without excessive perfume intensity from the undiluted product.

To give excellent perfume delivery when laundry is removed from the washing machine it is advantageous if the perfume carrier substance mix has a slip point below preferably from 0 to 37 0 C. I-ore preferably it has a slip point between and 370C.

Preferably the compositions of the invention are liquids, more preferably comprising an aqueous base.

WO 95/22594 PCT/EP95/00624 4 It is preferred if the carrier substance is an organic material. It is further preferred if the carrier substance is a fatty ester of a mono or polyhydric alcohol having from 1 to about 24 carbon atoms in the hydrocarbon chain with the proviso that the total number of carbon atoms in the carrier substance is equal to or greater than 16 and that at least one of the hydrocarbons radicals in the ester has 12 or more carbon atoms. Such fatty esters are preferably odourless.

It is preferred if the carrier substance in the perfume/carrier substance mix is a fatty acid glyceride or mixtures of fatty acid glycerides. Especially preferred carrier substances are triglycerides, most preferred are palm ii oil and tallow oil.

The perfume/carrier substance mix is preferably present at a level of from 1 to 10% of the composition, more preferably 3 wt% to 7 wt% of the total composition.

Fof good perfume delivery it is advantageous if the ratio of perfume to carrier substance is from 1:50 to 1:1, more preferably 1:20 to 1:2, most preferably 1:7 to 1:2.

To achieve good perfume delivery from the product it is favourable if the ratio of perfume/carrier substance mix to quaternary ammonium fabric softening agent is in the ratio of 5:1 to 1:10, more preferably 2:1 to 1:10.

It is preferable if the quaternary ammonium compound is biodegradable and has at least one ester link.

Advantageously the fabric softening composition comprises a water insoluble cationic compound having two C1.= 8 alkyl or alkenyl groups connected to the N atom via one or more ester links.

jy YIUa,~u. ,;iirc r.i.Mc i wo 95/22954 PCT/EP95/Q624 5 A preferred type of ester-linked quaternary ammonium fabric softening agent for use in the compositions according to the invention can be represented by the formula:

I

R, N+ -(CH 2

-T-R

2

(CH

2

,-T-R

2

S

wherein each Ri group is independently selected from C1- 4 alkyl, or hydroxyalkyl or C2- 4 alkenyl groups; and wherein each R 2 group is independently selected from Cs-2 8 alkyl or alkenyl groups; 0 0 II II T is or and n is an integer from A second preferred type of quaternary ammonium fabric softening agent can be represented by the formula: 5 io 0

II

OCR

2 3 N (CH)n CH II 2 0 wherein R 1 n and R 2 are as defined above.

H 1 T

I

L

WO 95/22594 PCT/EP95/00624 6 Preferred materials of this class and their method of preparation are, for example, described in US 4 337 180 (Lever Brothers). Preferably these materials comprise small amounts of the corresponding monoester as described in US 4 137 180, for example 1-tallowoxy, 2-hydroxytrimethyl ammonium propane chloride.

Preferably the level of ester linked quaternary ammonium compounds is at least 1% by weight of the composition, more preferably more than 7% by weight of the composition; especially interesting are concentrated compositions which comprise between 10 and 30 by weight of ester-linked quaternary ammonium compound.

Compositions of the invention may also contain nonionic stabilisers. Suitable nonionic stabilisers which can be used include the condensation products of C. C, primary linear alcohols with 10 to 25 moles of ethylene oxide. Use of less than 10 moles of ethylene oxide, especially when the alkyl chain is in the tallow range, leads to unacceptably high aquatic toxicity. In particular the following nonionic stabilisers are preferred: Genapol T-110, Genapol T-150, Genapol T-200, Genapol C-200 all ex Hoechst AG, Lutensol AT18 ex BASF, Genapol C-100 and Genapol C-150 ex Hoechst, or fatty alcohols for example Laurex CS, ex Albright and Wilson or Adol 340 ex Sherex (all Trade Marks). Preferably the nonionic stabiliser has an HLB value of from 10 to 20, more preferably 12 to 20. Preferably, the level of nonionic j stabiliser is within the range of from 0.1 to 10% by weight, S 30 more preferably from 0.5 to 5% by weight, most preferably from 1 to 4% by weight.

The composition can also contain fatty acids, for example J ,1.

1 1 1 f v

T

WO 95/22594 PCT/EP95/00624 -7-

C

8

C

24 alkyl or alkenyl monocarboxylic acids, or polymeric carboxylic acids. Preferably saturated fatty acids are used, in particular, hardened tallow fatty acids.

The level of fatty acid material is preferably more than 0.1% by weight, more preferably more than 0.2% by weight.

Especially preferred are concentrates comprising from 0.5 to by weight of fatty acid, more preferably 1% to 10% by weight. The weight ratio of quaternary ammonium material to fatty acid material is preferably from 10:1 to 1:10.

The compositions of the invention preferably have a pH of more than 1.5, more preferably less than The composition can also contain one or more optional ingredients, selected from non-aqueous solvents, pH buffering agents, perfumes, perfume carriers, fluorescers, colorants, hydrotropes, antifoaming agents, antiredeposition agents, enzymes, optical brightening agents, opacifiers, antishrinking agents, anti-wrinkle agents, anti-spotting agents, germicides, fungicides, anti-oxidants, anti-corrosion agents, drape imparting agents, antistatic agents and ironing aids.

The composition may also contain nonionic fabric softening agents.

The invention will now be illustrated by the following nonlimiting examples. In the examples all percentages are expressed by weight.

Comparative Examples are designated by letters, while Examples of the invention are designated by numbers.

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,-1 WO 95/22594 PCT/EP95/00624 8 ExamDles 1, 2, 3, 4, A, B, C and.D Compositions were prepared by the following method: antifoam, preservative and dyestuff were dissolved in warm (400C) water followed by addition of electrolyte (citric or CaCl) to form an aqueous solution. The biodegradable cationic fabric softening agent (HT TMAPC 1-trimethyl ammonium-2,3 dihardened tallowoyloxy propane chloride with some tallow fatty acid impurities (6:1 ratio) ex Hoechst) was melted (75-800C) and mixed with the nonionic (coco ethoxylate 20EO:coco 20). This premix was added to the aqueous solution over 5 min with stirring. The resulting mixture was recirculated through a Janke and Kunkel mill set at max shear (10,000 rpm). This recirculation/shearing continued for 30 mins after premix addition. Perfume was stirred directly into the mix or a premixed with palm/tallow oil at a temperature of 40-450C and then added by milling into the product over a 10 min period-at 8000 rpm.

(The palm/tallow raw materials are refined, bleached and deodorised).

iK I V 1 i 3! WO 95/22594 PCT/EP95/00624 9 TABLE 1 Formulations EXAMPLES A 1 B 2 Citric Acid 3.5 3.5 3.5 HT TMAPC 20 20 20 Nonionic (Coco 20) 1.0 1.0 3.0 Antifoam 0.06 0.06 0.06 0.06 Preservative 0.02 0.02 0.02 0.02 Perfume 1.0 1.0 1.0 Palm Oil 3.0 Tallow Oil Demin Water to 100 to 100 to 100 to 100 TABLE 2 Example C 3 D 4 CaC1, 0.20 0.20 0.20 0.20 HT TMAPC 20 20 20 Nonionic (Coco 20) 3.0 3.0 3.0 Antifoam 0.06 0.06 0.06 0.06 Preservative 0.02 0.02 0.02 0.02 Perfume 1.0 1.0 1.0 Palm Oil 3.0 Tallow Oil Demin Water to 100 to 100 to 100 to 100 i 4 1 *1 it. WO 95/22594 WO 9522594PCIVE P95100624 viscosity measurements were taken at 250 and at 106 sec",~ shear rate using a H-aake VT50OI rotoviscometer.

Examples A and B went solid within 3 days at 37WC storage.

Examples 1 and 2 showed viscosities as follows'- TABLE 3 Time 0 37 0 C 1 Viscosity 1 1 2 Initial. S, cP 118 oP days -122 cp 12 days 65 op 22 days -125 CP 28 days 93 cP 29 days -121 cP 38 days -118 cp 66 days -129 cP Examples C and D went solid within 3hrs at ambient temperature.

Examples 3 and 4 showed viscosities as follows: WO 95/22594 WO 9522594PCTIEP95/00624 TABLE 4 [Time 37 0 C IVisc t 3 1 4 -initial 64 cP 38 cP -7 days 34 cP days 68 cP 19 days 33 cP LO 21 days 82 cl? 43 days -36 dl? 56 days 87 cP 58 days -39 cl? 71 days 99 Examples 5,6,7,8EFCQ and H To demonstrate that this invention work~s with a variety of perfumes, 300g of an unperfumed base (at 35 cl?) of composition 4 was prepared with either perfume alone or perfume/palm oil mix by milling into the base using a Silverson mixer over a 5 min period. The samples were left at ambient temperature.

1~

V

WO 95/22594 PCT/EP95/00624 12 TABLE Examples Perfume Palm Oil Time to go Solid E Perfume A 10 mins Perfume A 3% Liquid after 10 days F Perfume B 2-3 days 6 Perfume B 3% Liquid after 10 days G Perfume C 10 mins 7 Perfume C 3% Liquid after 10 days H Perfume D 1-2 days 8 Perfume D 3% Liquid after 10 days Examoles 9,10 and I Examples were prepared by dispersing the cationic fabric softening agent in water, followed by the addition of the perfume or perfume/carrier substance mix.

The perfume substantivity was tested by adding ig of the resulting composition to 1 litre of water at ambient temperature and agitating for 2 minutes to disperse. Four 19 x 19 squares of terry towelling were than immersed in the dispersion and left for 5 minutes. The terry towelling was then removed from the dispersion, wrung dry and line dried overnight.

The terry towelling samples were evaluated by a panel of people using a random design to measure perfume strength.

rr'' ib WO 95/22594 PCT/EP95/00624 13 Each treatment was evaluated six times. The data was analysed by analysis of variance.

TABLE 6 Example 9 10 I HT TMAPC 14.5 14.5 14.5 Perfume 0.9 0.9 0.9 Softline 2000 Palm oil 5.0 2.7 Water to 100 The perfume release on the terry towelling was in the table below: as illustrated TABLE 7 A score of 0 indicates a no perfume impact.

A score of 5 indicates a very strong perfume impact.

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Claims (1)

1. 06. 07. 95 Name anid man address of tie ISA Authorized offcer E w'a P a 9 f e P B 5 1 Z P a rn z l a a i 2 Fax (+31-70) 340-3016Bls V Form PCTIMSA211 $but) (July~ 111) nacp 1 nf 2 A I I. INTERNATIONAL SEARCH REPORT lnternat Application No IPCT/EP 95/00624 [C.(Continuation) DOCUMENTS CONSIDERED TO BE2 RELEVANT Category [Chtaion of documnent, with indication, where appropriate, of the relevant passges [Relevant to claim No, A A EP,A,0 005 618 (UNILEVER PLC ;UNILEVER NV 28 November 1979 see page 21, line 17 page 22, line 4 WO,A,93 05137 (PROCTER GAMBLE) 18 March 1993 see the whole document 1-12 Fain PC=j1SA41S (ccAuatioa at aml that) tiuly lI2) page 2 of 2 INTERNATIONAL SEARCH REPORT Intemx 'Application No PCT/EP 95/00624 Patent document Publication Patent family Publication cited in search report date xmember(s) Tdate FR-A-2369340 26-05-78 GB-A- 1587122 01-04-81 AU-A- 3013877 03-05-79 CA-A- 1111616 03-11-81 DE-A- 2747726 03-05-78 JP-A- 53094042 17-08-78 US-A- 4152272 01-05-79 EP-A-0239910 07-10-87 GB-A- 2188653 07-10-87 AU-B- 599966 02-08-90 AU-A- 7096587 08-10-87 CA-A- 1279448 29-01-91 DE-A- 3782075 12-11-92 IE-B- 60303 29-06-94 JP-A- 63006168 12-01-88 US-A- 4767547 30-08-88 WO-A-9113143 05-09-91 US-A- 5066419 19-11-91 AU-B- 639078 15-07-93 AU-A- 7305891 18-09-91 CN-A- 1054264 04-09-91 CN-A- 1092806 28-09-94 EG-A- 19200 29-09-94 EP-A- 0543816 02-06-93 NZ-A- 237155 23-12-93 TR-A- 25559 01-07-93 US-A- 5154842 13-10-92 EP-A-0005618 28-11-79 AT-T- 1167 15-06-82 AU-B- 524331 09-09-8' AU-A- 4700479 22-11-79 CA-A- 1122520 27-04-82 DE-A- 2919513 29-11-79 FR-A,B 2425861 14-12-79 GB-A,B 2020977 28-11-79 JP-B- 3044782 09-07-91 JP-A- 54151129 28-11-79 NL-A- 7903763 20-11-79 US-A- 434715? 31-08-82 US-A- 446984L 04-09-84 US-A- 4579677 01-04-86 page 1 of 2 INTERNATIONAL SEARCH REPORT (Intenar' I Application No PCT/tP 95/00624 Patent document I Publication Patent family I Publication cited in search report date member(s) date W-A-9305137 18-03-93 US-A- 5234611 10-08-93 EP-A- 0601035 15-06-94 Foam PCAfSAJ2XS (Wat tw-4i (JUIM page 2 of 2