CA1130058A

CA1130058A - Liquid formulations

Info

Publication number: CA1130058A
Application number: CA340,005A
Authority: CA
Inventors: James B. Melville
Original assignee: Unilever PLC
Current assignee: Unilever PLC
Priority date: 1978-11-17
Filing date: 1979-11-16
Publication date: 1982-08-24
Also published as: WO1980001075A1; ES8100341A1; ZA796187B; EP0011499B1; DK307680A; JPS55500911A; DE2961275D1; PT70463A; AU531802B2; AU5292579A; ES486066A0; EP0011499A1; ATE357T1

Abstract

ABSTRACT OF THE DISCLOSURE
A liquid formulation for depositing perfumes on fabric surfaces comprises an aqueous base, 0.5 to 30% of a fabric conditioning agent such as a fabric softener and 0.5 - 50% of particles consisting of an intimate mixture of an amine and a perfume, the particles having a size of 0.1 -200 micron, preferably 0.1 to 5 micron. The amine may be a primary amine, a tertiary amine or a diamine. The particles are formed from a liquid melt of the amine and the perfume by dispersing in water. A benefit over particles consisting of non-ionic, cationic and perfume can be demonstrated.

Description

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FIELD OF THE INVENTION
This invention relates to liquid formulations cap-able of depositing perfumes on fabric surfaces. The formula-ticn may be used in diluted form and examples of the fabric surfaces are cotton, wool, polyacrylic, polyamide and poly-ester fibres. These formulations are intended for use in the rinse cycle of a fabric cleaning operation.
The liquid formulations of the invention will nor-mally be used to provide a fabric softening effect.
Perfumes are liquid compositions consisting of a number of organic compounds, capable of appreciation by smell.
The compounds are usually derived from natural sources but '~
synthetic materials are also used. Formulations intended for the laundering of fabric will normally contain a perfume to provide a pleasant after smell on the laundered fabrics.
Thus powder and liquid detergent formulations, and rinse cycle formulations contain perfumes.
It is desirable to have the perfume in a fabric treatment formulation used efficiently because it is a rela-tively high cost component of any formulation. In use the perfume will be present in the formulation at a relatively -low concentration and dilution will cause the fabric to be `
in contact with a liquid system containing a very low concen-tration of the perfume.
BACKGROU~D ART
The desirability of enhancing the effectiveness of perfumes has been acknowledged in the patent literature.

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li3aoss United States Patent Specification No. 4 152 272 (Young) des-cribes a fabric conditioning composition comprising particles of a wax-like carrier and a perfume. British Patent Specifi-cation No. 1 544 863 (Schilling et al) describes a fabric con- -ditioning composition for use in an automatic laundry dryer comprising particles of a mixed cationic/non-ionic carrier and a perfume. In German patent application No. 2 732 985 of Unilever Limited a deposition system is described which pro-vides increased deposition of materials providing a perceiv-able effect, for example perfumes. Amines are disclosed as matrix materials, but a cationic material is required as an essential component of the dispersed phase including the per-ceivable component.
DISCLOSURE OF THE INVENTION
We have now discovered that surprising good perfume deposition on fabrics can be achieved without the incorpora-tion of cationic materials in perfume-carrying amine particles~
Thus, according to the invention, there is provided a liquid formulation for depositing perfumes on fabric surfaces, wherein the formulation comprises an aqueous base having:
I i) a first dispersed phase constituting from about 0.5%
to about 50% by weight of the formulation and con-sisting of particles having an a~erage size of ~rom about 0.1 micron to about 200 microns, preferably 0.1 to 5.0 micron, the particles comprising an intimate mixture of (a) from about 0.5% to about 50% by weight, based on the weight of the particles,

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by weight, based on the weight of the particles of a matrix comprising at least one water dispersible amine of the formula R - N R R
where R is an alkyl or alkenyl group having from 8 to 22 carbon atoms, Rl is hydrogen or an alkyl or alkenyl group having 1 to 4 carbon atoms and R2 is hydrogen or an alkyl, alkenyl or amino-alkyl group having from 1 to 22 carbon atoms, the matrix con-taining no added cationic material; and ii) a second dispersed phase constituting from about 0.5%
to about 30% by weight of the formulati~n and com-prising a fabric conditioning agent.
The aqueous base will oontain water as a major con-stituent. While it is possible for this to be the sole com-ponent of the base, the latter will usually include other materials, for example, electrolytes, buffering agents, short chain alcohols, emulsifiers, colouring materials, bacteri- _ . . .
~ 20 ~cides, antioxidants, surface active agents and fluorescers.
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The alkyl groups, alkenyl groups and alkyl portion of the amino-alkyl groups may be linear or branched. Prefer-ably the amine is a primary or tertiary compound or a diamine, particularly a diamine of the formula R-NH-(CH2)3-NH2, where R is as defined above. Preferred compounds are methyl dihar-. .
dened tallow tertiary amine, hardened tallow primary amine, methyl, dicoco-tertiary amine, coco primary amine and N-alkyl _3_ ' ~ I

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~3(~()58 1:3 propylene diamines, where the alkyl group may be hardened tallow, coconut or C18/C20 mixture. The amines of utility in the invention can be solid, liquid or pasty and will have a solubility in water of not more than about 1% weight/volume.
The amines will be dispersible in the aqueous base liquid.
The fabric conditioning agent may be selected from the classes of: dialkyl quaternary ammonium salts e.g. dis-tearyl dimethyl ammonium chloride; amine salt derivatives;
amphoteric compounds e.g. alkyl sulphobetaines and imidazoline derivatives; or agents formed by complexing cationic and ani-onic species, e.g. as described in U.K. patent specification 2 007 735.
A list of suitable conditioning materials is given in German application 2 732 985.
The perfume may be selected from any perfumes and any mixtures thereof. Examples of fabric substantive perfumes suitable for use in the present invention are listed in S
Arctander, Perfume Flavors and Chemicals, Volumes I and II, published by the author, Montclair, New Jersey, U.S.A. and the Merck Index, 8th Edition, Merck & Co. Inc., Rahway, New Jersey, U.S.A. Deodorant perfumes such as disclosed in United States specification 4 134 838 may also ~e used.
A method of preparing the liquid formulation of the invention, includes the step of forming a liquid mixture of the amine and the perfume and dispersing the mixture in water.
The preferred method is to melt the amine and the perfume togethex and then disperse the mixture in heated ~ -4-- , :
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water. An aid to dispersion e.g. high speed stirrers, ultra-sonic agitators, vibrating reeds and continuous mixers may be used. In an alternative method the melt is solidified in bulk and then dispersed into water at ambient temperature.
BEST MODE OF CARRYING OUT INVENTION
Examples of formulations according to the invention will now be given. The benefit achieved by use of the inven-tion is demonstrated using the following test method:
Three pieces of 20 cm x 20 cm terry towelling (T) or bulked acrylic ~BA) were rinsed in a Terg-o-Tometer (a Registered Trade Mark) for 4 minutes at 75 cycles per minute agitation. The rinse li~uor was formed by adding 2 mls of formulation to 800 mls of water. The samples were spun dry for 30 seconds and dried overnight. The perfume effect was then gauged by an experienced panel and graded, from 0 to 5. The average grade was taken for each formulation.

0.9 g of methyl di-hardened tallow amine was melted and 0.2 g of a perfume added; the amine was maintained as near 20 to its melting point as possible consistent with good mixing. `
The melt was then added to 50 g water at 70C and a dispersion formed with the aid of an ultrasonic probe. The average par-ticle size was 0.4 microns. Dimethyl di-hardened tallow ammon-ium chloride (5 g) was dispersed in water (50 g) and the two dispersions mixed.
The perfume effect was gauged and compared to a con-trol formulation. This control was formed by dispersing 5 g :

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1:~L3(~058 of the above quaternary ammonium salt in water (100 g) and adding 0.2 g of the same perfume.
The results of this and the following Examples 2 -14 are given in the Table I which ~uotes the average grading for each ~formulation and defines the amine used by chain length of the alkyl group and type of amine.

Example 1 was repeated using methyl dicoco amine.

Example 1 was repeated using methyl di(C18~C20) alkyl amine. The long chain alkyl group was formed by a 50:50 molar mixture of C18 and C20 alkyl chains-Example 1 was repeated using hardened tallow primary amine.

Example 1 was re~eated using coconut primary amine.

Example 1 was repeated using C18/C20 primary amine-. .
Example 1 was repeated using di-hardened tallow secon-dary amine.

EXAMoeLE 8 Example 1 was repeated using di-coconut secondary amine.

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ll3aoss ~ ExAMæLE 9 Example l was repeated using dimethyl mono hardened tallow tertiary amine.

S Example 1 was repeated using dimethyl mono-coconut tertiary amine.
ExAMæ~E 11 Example 1 was repeated using dimethyl mono (C18/C20) alkyl tertiary amine.

Example 1 was repeated using N-hardened tallow 1:3 propylene diamine.
EXAMPLE 13 ~-Example 1 was repeated using N-coco 1:3 propylene diamine. -Example 1 was repeated using N-(C18/C20) 1:3 propyl-ene diamine.

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EXA~LES 15 TO 20 Example 1 was repeated using a number of perfume/
amine combinations and the results were compared with two controls. Control A was an aqueous dispersion of non-ionic/
cationic/perfume particles according to our German Patent Specification No. 2 732 985 containing the same quantity of perfume (0.2 g), where the non-ionic was tallow alcohol 3EO
[0.9 g) and the cationic was Arosurf* TA 100 (~imethyl dis-tearyl ammonium chloride)(0.05 g). Control B consisted of the same quantity of perfume dispersed in water.
The amines used were:
T 9701 - methyl dihardened tallow tertiary amine P 970 - hardened tallow primary amine `~
D 970 - hardened tallow 1:3 polypropylene diamine D 650 - coco 1:3 propylene diamine The results are given in the following table II:

TABLE II
MEAN PERFUME INTENSITIES
EXA~LE PERFUME AMINE TFRRY FABRIC ACRYLIC FABRIC
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LF 165 T9701 0.83 0.60 16 LF 165 P 970 1.31 0.61 17 LF 165 D 970 1.07 0.57 18 LF 165 D 650 1.30 0.68 Control-A LF 165 - 0.44 0.42 Control-B LF 165 - 0.35 0.26 19 LF 166 T9701 0.58 0-49 LF 166 P 970 0.54 0.49 Control-A LF 166 - 0.36 0.38 Control-B LF 166 - 0.26 0.28 *denotes trade mark _g_ ' I

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The perfume formulations used were:
LF 165 %
Benzyl Salicylate 5.0 Musk Xylene 5.0 Galaxolide 50~ 5.0 Hexyl Cinnamic Aldehyde 10.0 Lilial 5.0 Hydroxycitronellal 6.0 Methyl Dihydro Jasmonate 8.0 Citronellol Standard 5-0 Geraniol Standard 5.0 Phenyl Ethyl Alcohol 10.0 Oil of Bergamot Synthetic `- 5.0 Oil of Geranium Bourbon 5.0 Oil of Lavandin 5.0 Trichlor Methyl Phenyl Carbinyl Acetate 2.0 Oil of Patchouli 1.0 Linalol 10.0 Coumarin 2.0 : 20 Benzyl Acetate 2.0 Terpineol 4-0 100. o .

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Amyl Cinnamic Aldehyde 2.0 Anisic Aldehyde 1.5 Benzyl Acetate 6.0 5 ~Cinnamic Alcohol ~ 8.0 Hexyl Cinnamic Aldehyde 4.0 Hydroxycitronellal 8.0 Indole 10% 3.0 Iso Eugenol 1.0 10Lilial 7.0 .
Linalol 6.0 Lyral 7.0 Phenyl Ethyl Alcohol 18.0 Terpineol 16.0 15 Tonalid 12.0 Vanillin 0-5 100. 0 ..
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Claims

THE EMBODIMENTS OF THE INVENTION IN WHICH AN EXCLUSIVE
PROPERTY OR PRIVILEGE IS CLAIMED ARE DEFINED AS FOLLOWS:

1. A liquid formulation for depositing perfumes on fabric surfaces, wherein the formulation comprises an aqueous base having:
i) a first dispersed phase constituting from about 0.5%
to about 50% by weight of said formulation and con-sisting of particles having an average size of from about 0.1 micron to about 200 micron, the particles comprising an intimate mixture of (a) from about 0.5%
to about 50% by weight, based on the weight of soap particles, of a perfume; and (b) from about 50% to about 99.5% by weight, based on the weight of said particles of a matrix comprising at least one water dispersible amine of the formula where R is selected from the group consisting of alkyl and alkenyl groups having from 8 to 22 carbon atoms, R1 is selected from the groups consisting of hydrogen and alkyl and alkenyl groups having 1 to 4 carbon atoms and R2 is selected from the group con-sisting of hydrogen and an alkyl, alkenyl and amino-alkyl groups having from 1 to 22 carbon atoms, said matrix containing no added cationic material; and ii) a second dispersed phase constituting from about 0.5%
to about 30% by weight of said formulation and com-prising a fabric conditioning agent.

2. A liquid formulation according to Claim 1, wherein said amine is a primary amine.

3. A liquid formulation according to Claim 2, wherein said amine is selected from the group consisting of hardened tallow primary amine, coco primary amine and C18/C20 mixture primary amine.

4. A liquid formulation according to Claim 1, wherein said amine is a tertiary amine.

5. A liquid formulation according to Claim 4, wherein said amine is selected from the group consisting of methyl dihardened tallow tertiary amine, methyl dicoco tertiary amine and methyl di(C18/C20 mixture) tertiary amine.

6. A liquid formulation according to Claim 1, wherein said amine is a diamine.

7. A liquid formulation according to Claim 6, wherein said diamine has the formula where R is selected from the group consisting of alkyl and alkenyl groups having from 8 to 22 carbon atoms.

8. A liquid formulation according to Claim 7, wherein R is selected from the group consisting of hardened tallow, coconut and a C18/C20 mixture.

9. A liquid formulation according to Claim 1, wherein said amine has a solubility in water of not more than 1%
weight/volume.

10. A liquid formulation according to Claim 1, wherein said fabric conditioning agent is a fabric softening agent.

11. A liquid formulation according to Claim 10, wherein said fabric softening agent is a cationic material.

12. A liquid formulation according to Claim 10, wherein said fabric softening agent is selected from the group consist-ing of dialkyl quaternary ammonium salts, amine salts and am-photeric fabric softening agents.

13. A liquid formulation according to Claim 12, wherein said fabric softening agent is distearyl dimethyl ammonium chloride.

14. A liquid formulation according to Claim 12, wherein said amphoteric fabric softening agent is selected from the group consisting of alkyl sulphobetaines and imidazoline deriv-atives.

15. A liquid formulation according to Claim 1, containing from about 2% to about 10% by weight of said formulation of said fabric conditioning agent.

16. A liquid formulation according to Claim 1, containing from about 0.7% to about 0.2%, by weight of the formulation, of said particles.

17. A liquid formulation according to Claim 1, wherein said particles have a size in the range of from about 0.1 micron to about 5.0 micron.

18. A liquid formulation according to Claim 1, wherein said particles contain from about 10% to about 30%, by weight of said particles, of said perfume.

19. A method of preparing a liquid formulation according to Claim 1, including the steps of forming a liquid mixture of said amine and said perfume and dispersing said mixture in water.

20. A method according to Claim 19, wherein said liquid mixture is formed by melting said amine and said perfume to-gether.

21. A method according to Claim 19 or 20, wherein said liquid mixture is dispersed in heated water.

22. A method according to Claim 19 or 20, wherein said liquid mixture is solidified and then dispersed in water at ambient temperature.

23. A method of depositing perfumes on fabric surfaces, comprising treating said fabric surfaces with a liquid formu-lation according to Claim 1.