U.S. patent application number 12/971151 was filed with the patent office on 2011-04-14 for benefit agent containing delivery particle.
Invention is credited to Jiten Odhavji Dihora, Adam Keith Druckrey, Sandra Jacqueline Guinebretiere, An Pintens, Peggy Dorothy Sands, Johan Smets, Nianxi Yan.
Application Number | 20110086788 12/971151 |
Document ID | / |
Family ID | 39712058 |
Filed Date | 2011-04-14 |
United States Patent
Application |
20110086788 |
Kind Code |
A1 |
Smets; Johan ; et
al. |
April 14, 2011 |
BENEFIT AGENT CONTAINING DELIVERY PARTICLE
Abstract
The present invention relates to benefit agent containing
delivery particles, compositions comprising said particles, and
processes for making and using the aforementioned particles and
compositions. When employed in compositions, for example, cleaning
or fabric care compositions, such particles increase the efficiency
of benefit agent delivery, there by allowing reduced amounts of
benefit agents to be employed. In addition to allowing the amount
of benefit agent to be reduced, such particles allow a broad range
of benefit agents to be employed.
Inventors: |
Smets; Johan; (Lubbeek,
BE) ; Dihora; Jiten Odhavji; (Hamilton, OH) ;
Pintens; An; (Brasschaat, BE) ; Guinebretiere; Sandra
Jacqueline; (Appleton, WI) ; Druckrey; Adam
Keith; (Appleton, WI) ; Sands; Peggy Dorothy;
(Appleton, WI) ; Yan; Nianxi; (Appleton,
WI) |
Family ID: |
39712058 |
Appl. No.: |
12/971151 |
Filed: |
December 17, 2010 |
Related U.S. Patent Documents
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Application
Number |
Filing Date |
Patent Number |
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12156726 |
Jun 4, 2008 |
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12971151 |
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60934071 |
Jun 11, 2007 |
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Current U.S.
Class: |
510/105 ;
510/101; 510/106; 510/107; 510/349 |
Current CPC
Class: |
B01J 13/02 20130101;
D06M 23/12 20130101; C11D 17/0039 20130101; C11D 3/505 20130101;
A61K 8/11 20130101; D06M 13/005 20130101; A61K 2800/412 20130101;
A61P 29/00 20180101; Y10T 428/2987 20150115; A61Q 19/10
20130101 |
Class at
Publication: |
510/105 ;
510/101; 510/107; 510/106; 510/349 |
International
Class: |
C11D 17/00 20060101
C11D017/00; C11D 3/50 20060101 C11D003/50 |
Claims
1. A composition comprising: a.) benefit agent delivery particles
comprising a core material and a shell, said shell at least
partially surrounding said core material: i. at least 75% of said
benefit agent delivery particles having a fracture strength of from
about 0.2 MPa to about 10 MPa; and ii. said particles having a
benefit agent leakage of from 0% to about 30%; and b.) a consumer
product adjunct material.
2. The composition of claim 1, wherein at least 75% of said benefit
agent delivery particles have a particle size of from about 1
microns to about 80 microns.
3. The composition of claim 1 wherein at least 75% of said benefit
agent delivery particles have a particle wall thickness of from
about 30 nm to about 250 nm.
4. The composition of claim 1, wherein said benefit agent delivery
particles' core material comprises a material selected from the
group consisting of a perfume raw material and/or a material
selected from the group consisting of vegetable oil, esters of
vegetable oils, esters, straight or branched chain hydrocarbons,
partially hydrogenated terphenyls, dialkyl phthalates, alkyl
biphenyls, alkylated naphthalene, petroleum spirits, aromatic
solvents, silicone oils, and mixtures there of.
5. The composition of claim 1 wherein said benefit agent delivery
particles' wall material comprises a resin selected from the group
consisting of a reaction product of an aldehyde, with an amine.
6. The composition of claim 1 wherein said benefit agent delivery
particles comprise, based on total benefit agent delivery particle
weight, at least 1 weight %.
7. The composition of claim 1 wherein said benefit agent delivery
particles' core material comprises, based on total core material
weight, at least about 20 wt % benefit agent.
8. The composition of claim 1 wherein said benefit agent comprises
a perfume composition, said particles comprising, based on total
particle weight, from about 20 weight % to about 95 weight % of
said perfume composition.
9. The composition of claim 1 wherein said benefit agent delivery
particles' core material comprises: a.) a perfume composition
having a Clog P of less than 4.5; b.) a perfume composition
comprising, based on total perfume composition weight, 60% perfume
materials having a Clog P of less than 4.0; c.) a perfume
composition comprising, based on total perfume composition weight,
35% perfume materials having a Clog P of less than 3.5; d.) a
perfume composition comprising, based on total perfume composition
weight, 40% perfume materials having a Clog P of less than 4.0 and
at least 1% perfume materials having a Clog P of less than 2.0; e.)
a perfume composition comprising, based on total perfume
composition weight, 40% perfume materials having a Clog P of less
than 4.0 and at least 15% perfume materials having a Clog P of less
than 3.0; f.) a perfume composition comprising, based on total
perfume composition weight, at least 1% butanoate esters and at
least 1% of pentanoate esters; g.) a perfume composition
comprising, based on total perfume composition weight, at least 2%
of an ester comprising an allyl moiety and at least 10% of another
perfume comprising an ester moiety; h.) a perfume composition
comprising, based on total perfume composition weight, at least 1%
of an aldehyde comprising an alkyl chain moiety; i.) a perfume
composition comprising, based on total perfume composition weight,
at least 2% of a butanoate ester; j.) a perfume composition
comprising, based on total perfume composition weight, at least 1%
of a pentanoate ester; k.) a perfume composition comprising, based
on total perfume composition weight, at least 3% of an ester
comprising an allyl moiety and 1% of an aldehyde comprising an
alkyl chain moiety; l.) a perfume composition comprising, based on
total perfume composition weight, at least 25% of a perfume
comprising an ester moiety and 1% of an aldehyde comprising an
alkyl chain moiety; m.) a perfume compositions comprising, based on
total perfume composition weight, at least 2% of a material
selected from 4-(2,6,6-trimethyl-1-cyclohexenyl)-3-buten-2-one,
4-(2,6,6-trimethyl-2-cyclohexenyl)-3-buten-2-one and 3-buten-2-one,
3-methyl-4-(2,6,6-trimethyl-1-cyclohexen-2-yl)- and mixtures
thereof; n.) a perfume composition comprising, based on total
perfume composition weight, at least 0.1% of tridec-2-enonitrile,
and mandaril, and mixtures thereof; o.) a perfume composition
comprising, based on total perfume composition weight, at least 2%
of a material selected from 3,7-dimethyl-6-octene nitrile,
2-cyclohexylidene-2-phenylacetonitrile and mixtures thereof; p.) a
perfume composition comprising, based on total perfume composition
weight, at least 80% of one or more perfumes comprising a moiety
selected from the group consisting of esters, aldehydes, ionones,
nitriles, ketones and combinations thereof; q.) a perfume
composition comprising, based on total perfume composition weight,
at least 3% of an ester comprising an allyl moiety; a perfume
composition comprising, based on total perfume composition weight,
at least 20% of a material selected from the group consisting of:
1-methylethyl-2-methylbutanoate; ethyl-2-methyl pentanoate;
1,5-dimethyl-1-ethenylhexyl-4-enyl acetate; p-metnh-1-en-8-yl
acetate; 4-(2,6,6-trimethyl-2-cyclohexenyl)-3-buten-2-one;
4-acetoxy-3-methoxy-1-propenylbenzene; 2-propenyl
cyclohexanepropionate; bicyclo[2.2.1]hept-5-ene-2-carboxylic acid,
3-(1-methylethyl)-ethyl ester; bycyclo[2.2.1]heptan-2-ol,
1,7,7-trimethyl-, acetate; 1,5-dimethyl-1-ethenylhex-4-enylacetate;
hexyl 2-methyl propanoate; ethyl-2-methylbutanoate; 4-undecanone;
5-heptyldihydro-2(3h)-furanone; 1,6-nonadien-3-ol,3,7dimethyl-;
3,7-dimethylocta-1,6-dien-3-o;
3-cyclohexene-1-carboxaldehyde,dimethyl-; 3,7-dimethyl-6-octene
nitrile; 4-(2,6,6-trimethyl-1-cyclohexenyl)-3-buten-2-one;
tridec-2-enonitrile; patchouli oil; ethyl
tricycle[5.2.1.0]decan-2-carboxylate;
2,2-dimethyl-cyclohexanepropanol; hexyl ethanoate,
7-acetyl,1,2,3,4,5,6,7,8-octahydro-1,1,6,7-tetramethyl naphtalene;
allyl-cyclohexyloxy acetate; methyl nonyl acetic aldehyde;
1-spiro[4,5]dec-7-en-7-yl-4-pentenen-1-one;
7-octen-2-ol,2-methyl-6-methylene-,dihydro;
cyclohexanol,2-(1,1-dimethylethyl)-, acetate;
hexahydro-4,7-methanoinden-5(6)-yl
propionatehexahydro-4,7-methanoinden-5(6)-yl propionate;
2-methoxynaphtalene;
1-(2,6,6-trimethyl-3-cyclohexenyl)-2-buten-1-one;
1-(2,6,6-trimethyl-2-cyclohexenyl)-2-buten-1-one;
3,7-dimethyloctan-3-ol; 3-buten-2-one,
3-methyl-4-(2,6,6-trimethyl-1-cyclohexen-2-yl)-; hexanoic acid,
2-propenyl ester; (z)-non-6-en-1-al; 1-decyl aldehyde; 1-octanal;
4-t-butyl-.alpha.-methylhydrocinnamaldehyde;
alpha-hexylcinnamaldehyde; ethyl-2,4-hexadienoate; 2-propenyl
3-cyclohexanepropanoate; and mixtures thereof; r.) a perfume
composition comprising, based on total perfume composition weight,
at least 20% of a material selected from the group consisting of:
1-methylethyl-2-methylbutanoate; ethyl-2-methyl pentanoate;
1,5-dimethyl-1-ethenylhex-4-enyl acetate; p-menth-1-en-8-yl
acetate; 4-(2,6,6-trimethyl-2-cyclohexenyl)-3-buten-2-one;
4-acetoxy-3-methoxy-1-propenylbenzene; 2-propenyl
cyclohexanepropionate; bicyclo[2.2.1]hept-5-ene-2-carboxylic acid,
3-(1-methylethyl)-ethyl ester; bycyclo[2.2.1]heptan-2-ol,
1,7,7-trimethyl-, acetate; 1,5-dimethyl-1-ethenylhex-4-enyl
acetate; hexyl 2-methyl propanoate; ethyl-2-methylbutanoate,
4-undecanolide; 5-heptyldihydro-2(3h)-furanone; 5-hydroxydodecanoic
acid; decalactones; undecalactones, 1,6-nonadien-3-ol,3,7dimethyl-;
3,7-dimethylocta-1,6-dien-3-ol;
3-cyclohexene-1-carboxaldehyde,dimethyl-; 3,7-dimethyl-6-octene
nitrile; 4-(2,6,6-trimethyl-1-cyclohexenyl)-3-buten-2-one;
tridec-2-enonitrile; patchouli oil; ethyl
tricycle[5.2.1.0]decan-2-carboxylate;
2,2-dimethyl-cyclohexanepropanol; allyl-cyclohexyloxy acetate;
methyl nonyl acetic aldehyde;
1-spiro[4,5]dec-7-en-7-yl-4-pentenen-1-one;
7-octen-2-ol,2-methyl-6-methylene-,dihydro,
cyclohexanol,2-(1,1-dimethylethyl)-, acetate;
hexahydro-4,7-methanoinden-5(6)-yl
propionatehexahydro-4,7-methanoinden-5(6)-yl propionate;
2-methoxynaphtalene;
1-(2,6,6-trimethyl-3-cyclohexenyl)-2-buten-1-one;
1-(2,6,6-trimethyl-2-cyclohexenyl)-2-buten-1-one;
3,7-dimethyloctan-3-ol; 3-buten-2-one,
3-methyl-4-(2,6,6-trimethyl-1-cyclohexen-2-yl)-; hexanoic acid,
2-propenyl ester; (z)-non-6-en-1-al; 1-decyl aldehyde; 1-octanal;
4-t-butyl-.alpha.-methylhydrocinnamaldehyde;
ethyl-2,4-hexadienoate; 2-propenyl 3-cyclohexanepropanoate; and
mixtures thereof; s.) a perfume composition comprising, based on
total perfume composition weight, at least 5% of a material
selected from the group consisting of
3-cyclohexene-1-carboxaldehyde,dimethyl-; 3-buten-2-one,
3-methyl-4-(2,6,6-trimethyl-1-cyclohexen-2-yl)-; patchouli oil;
Hexanoic acid, 2-propenyl ester; 1-Octanal; 1-decyl aldehyde;
(z)-non-6-en-1-al; methyl nonyl acetic aldehyde;
ethyl-2-methylbutanoate; 1-methylethyl-2-methylbutanoate;
ethyl-2-methyl pentanoate; 4-hydroxy-3-ethoxybenzaldehyde;
4-hydroxy-3-methoxybenzaldehyde; 3-hydroxy-2-methyl-4-pyrone;
3-hydroxy-2-ethyl-4-pyrone and mixtures thereof; t.) a perfume
composition comprising, based on total perfume composition weight,
less than 10% perfumes having a Clog P greater than 5.0; u.) a
perfume composition comprising geranyl palmitate; or v.) a perfume
composition comprising a first and an optional second material,
said first material having: (i) a Clog P of at least 2; (ii) a
boiling point of less than about 280.degree. C.; and second
optional second material, when present, having (i) a Clog P of less
than 2.5; and (ii) a ODT of less than about 100 ppb.
10. The composition of claim 1, said composition comprising a
material selected from the group consisting of a formaldehyde
scavenger, a structurant, an anti-agglomoration agent and mixtures
thereof.
11. The composition of claim 1, said composition being a consumer
product comprising from about 0.001% to about 25%, based on total
consumer product mass weight of said benefit agent delivery
particles.
12. The composition of claim 1, said composition comprising a
formaldehyde scavenger.
13. The composition of claim 1, said composition comprising a
structurant, said structurant comprising a material selected from
the group consisting of polysaccharides, modified celluloses,
modified proteins, inorganic salts, quaternized polymeric
materials, imidazoles; nonionic polymers having a pKa less than
6.0, polyurethanes, and mixtures thereof.
14. A method of treating and/or cleaning a situs, said method
comprising a. optionally washing and/or rinsing said situs; b.
contacting said situs with a composition according to claim 1; and
c. optionally washing and/or rinsing said situs.
15. A situs treated with a composition according to claim 1.
16. A consumer product comprising a consumer adjunct material and
benefit agent delivery particle produced by the process of: a.)
preparing a first solution comprising, based on total solution
weight, from about 20% to about 90%, a first emulsifier and a first
resin, the ratio of said first emulsifier and said first resin
being from about 0.1:1 to about 10:1; b.) preparing a second
solution comprising based on total solution weight from about 20%
to about 95% water, a second emulsifier and a second resin, the
ratio of said second emulsifier and said second resin being from
about 0:1 to about 3:1; c.) combining a core material and said
first solution to form a first composition; d.) emulsifying said
first composition; e.) combining said first composition and said
second solution to form a second composition and optionally
combining any processing aids and said second composition; f.)
mixing said second composition for at least 15 minutes at a
temperature of from about 25.degree. C. to about 100.degree. C. and
optionally combining any processing aids to said second
composition; g.) optionally combining any scavenger material,
structurant, and/or anti-agglomeration agent with said second
composition during step f.) or thereafter h.) optionally spray
drying said second composition.
17. A consumer product according to claim 16, wherein said benefit
agent delivery particle's core material comprises a perfume raw
material.
18. A consumer product according to claim 16 wherein said core
material comprises: a.) a perfume composition having a Clog P of
less than 4.5; b.) a perfume composition comprising, based on total
perfume composition weight, 60% perfume materials having a Clog P
of less than 4.0; c.) a perfume composition comprising, based on
total perfume composition weight, 35% perfume materials having a
Clog P of less than 3.5; d.) a perfume composition comprising,
based on total perfume composition weight, 40% perfume materials
having a Clog P of less than 4.0 and at least 1% perfume materials
having a Clog P of less than 2.0; e.) a perfume composition
comprising, based on total perfume composition weight, 40% perfume
materials having a Clog P of less than 4.0 and at least 15% perfume
materials having a Clog P of less than 3.0; f.) a perfume
composition comprising, based on total perfume composition weight,
at least 1% of a butanoate ester and at least 1% of a pentanoate
ester; g.) a perfume composition comprising, based on total perfume
composition weight, at least 2% of an ester comprising an allyl
moiety and at least 10% of another perfume comprising an ester
moiety; h.) a perfume composition comprising, based on total
perfume composition weight, at least 1% of an aldehyde comprising
an alkyl chain moiety; i.) a perfume composition comprising, based
on total perfume composition weight, at least 2% of a butanoate
ester; j.) a perfume composition comprising, based on total perfume
composition weight, at least 1% of a pentanoate ester; k.) a
perfume composition comprising, based on total perfume composition
weight, at least 3% of an ester comprising an allyl moiety and 1%
of an aldehyde comprising an alkyl chain moiety;) l.) a perfume
composition comprising, based on total perfume composition weight,
at least 25% of a perfume comprising an ester moiety and 1% of an
aldehyde comprising an alkyl chain moiety; m.) a perfume
composition comprising, based on total perfume composition weight,
at least 2% of a material selected from ionones, preferably
4-(2,6,6-trimethyl-1-cyclohexenyl)-3-buten-2-one,
4-(2,6,6-trimethyl-2-cyclohexenyl)-3-buten-2-one and 3-buten-2-one,
3-methyl-4-(2,6,6-trimethyl-1-cyclohexen-2-yl)- and mixtures
thereof; n.) a perfume composition comprising, based on total
perfume composition weight, at least 0.1% of tridec-2-enonitrile,
and mandaril, and mixtures thereof; o.) a perfume composition
comprising, based on total perfume composition weight, at least 2%
of a material selected from 3,7-Dimethyl-6-octene nitrile,
2-cyclohexylidene-2-phenylacetonitrile and mixtures thereof; p.) a
perfume composition comprising, based on total perfume composition
weight, at least 80% of one or more perfumes comprising a moiety
selected from the group consisting of esters, aldehydes, ionones,
nitriles, ketones and combinations thereof; q.) a perfume
composition comprising, based on total perfume composition weight,
at least 3% of an ester comprising an allyl moiety; a perfume
composition comprising, based on total perfume composition weight,
at least 20% of a material selected from the group consisting of:
1-methylethyl-2-methylbutanoate; ethyl-2-methyl pentanoate;
1,5-dimethyl-1-ethenylhexyl-4-enyl acetate; p-metnh-1-en-8-yl
acetate; 4-(2,6,6-trimethyl-2-cyclohexenyl)-3-buten-2-one;
4-acetoxy-3-methoxy-1-propenylbenzene; 2-propenyl
cyclohexanepropionate; bicyclo[2.2.1]hept-5-ene-2-carboxylic acid,
3-(1-methylethyl)-ethyl ester; bycyclo[2.2.1]heptan-2-ol,
1,7,7-trimethyl-, acetate; 1,5-dimethyl-1-ethenylhex-4-enylacetate;
hexyl 2-methyl propanoate; ethyl-2-methylbutanoate; 4-undecanone;
5-heptyldihydro-2(3h)-furanone; 1,6-nonadien-3-ol,3,7dimethyl-;
3,7-dimethylocta-1,6-dien-3-ol;
3-cyclohexene-1-carboxaldehyde,dimethyl-; 3,7-dimethyl-6-octene
nitrile; 4-(2,6,6-trimethyl-1-cyclohexenyl)-3-buten-2-one;
tridec-2-enonitril; patchouli oil; ethyl
tricycle[5.2.1.0]decan-2-carboxylate;
2,2-dimethyl-cyclohexanepropanol; hexyl ethanoate;
7-acetyl,1,2,3,4,5,6,7,8-octahydro-1,1,6,7-tetramethyl naphtalene;
allyl-cyclohexyloxy acetate; methyl nonyl acetic aldehyde;
1-spiro[4,5]dec-7-en-7-yl-4-pentenen-1-one;
7-octen-2-ol,2-methyl-6-methylene-,dihydro;
cyclohexanol,2-(1,1-dimethylethyl)-, acetate;
hexahydro-4,7-methanoinden-5(6)-yl
propionatehexahydro-4,7-methanoinden-5(6)-yl propionate;
2-methoxynaphtalene;
1-(2,6,6-trimethyl-3-cyclohexenyl)-2-buten-1-one;
1-(2,6,6-trimethyl-2-cyclohexenyl)-2-buten-1-one;
3,7-dimethyloctan-3-ol; 3-buten-2-one,
3-methyl-4-(2,6,6-trimethyl-1-cyclohexen-2-yl)-; hexanoic acid,
2-propenyl ester; (z)-non-6-en-1-a; 1-decyl aldehyde; 1-octanal;
4-t-butyl-.alpha.-methylhydrocinnamaldehyde;
alpha-hexylcinnamaldehyde; ethyl-2,4-hexadienoate; 2-propenyl
3-cyclohexanepropanoate; and mixtures thereof; r.) a perfume
composition comprising, based on total perfume composition weight,
at least 20%, 30% or even 50% of a material selected from the group
consisting of: 1-methylethyl-2-methylbutanoate; ethyl-2-methyl
pentanoate; 1,5-dimethyl-1-ethenylhex-4-enyl acetate;
p-menth-1-en-8-yl acetate;
4-(2,6,6-trimethyl-2-cyclohexenyl)-3-buten-2-one;
4-acetoxy-3-methoxy-1-propenylbenzene; 2-propenyl
cyclohexanepropionate; bicyclo[2.2.1]hept-5-ene-2-carboxylic acid,
3-(1-methylethyl)-ethyl ester; bycyclo[2.2.1]heptan-2-ol;
1,7,7-trimethyl-, acetate; 1,5-dimethyl-1-ethenylhex-4-enyl
acetate; hexyl 2-methyl propanoate; ethyl-2-methylbutanoate,
4-undecanolide; 5-heptyldihydro-2(3h)-furanone; 5-hydroxydodecanoic
acid; decalactones; undecalactones;
1,6-nonadien-3-ol,,3,7dimethyl-; 3,7-dimethylocta-1,6-dien-3-ol;
3-cyclohexene-1-carboxaldehyde,dimethyl-; 3,7-dimethyl-6-octene
nitrile; 4-(2,6,6-trimethyl-1-cyclohexenyl)-3-buten-2-one;
tridec-2-enonitrile; patchouli oil; ethyl
tricycle[5.2.1.0]decan-2-carboxylate;
2,2-dimethyl-cyclohexanepropanol; allyl-cyclohexyloxy acetate;
methyl nonyl acetic aldehyde;
1-spiro[4,5]dec-7-en-7-yl-4-pentenen-1-one;
7-octen-2-ol,2-methyl-6-methylene-,dihydro,
cyclohexanol,2-(1,1-dimethylethyl)-, acetate;
hexahydro-4,7-methanoinden-5(6)-yl
propionatehexahydro-4,7-methanoinden-5(6)-yl propionate;
2-methoxynaphtalene;
1-(2,6,6-trimethyl-3-cyclohexenyl)-2-buten-1-one;
1-(2,6,6-trimethyl-2-cyclohexenyl)-2-buten-1-one;
3,7-dimethyloctan-3-ol; 3-buten-2-one,
3-methyl-4-(2,6,6-trimethyl-1-cyclohexen-2-yl)-; hexanoic acid,
2-propenyl ester; (z)-non-6-en-1-al; 1-decyl aldehyde; 1-octanal;
4-t-butyl-.alpha.-methylhydrocinnamaldehyde;
ethyl-2,4-hexadienoate; 2-propenyl 3-cyclohexanepropanoate; and
mixtures thereof; s.) a perfume composition comprising, based on
total perfume composition weight, at least 5% of a material
selected from the group consisting of
3-cyclohexene-1-carboxaldehyde,dimethyl-; 3-buten-2-one,
3-methyl-4-(2,6,6-trimethyl-1-cyclohexen-2-yl)-; patchouli oil;
Hexanoic acid, 2-propenyl ester; 1-Octanal; 1-decyl aldehyde;
(z)-non-6-en-1-al; methyl nonyl acetic aldehyde;
ethyl-2-methylbutanoate; 1-methylethyl-2-methylbutanoate;
ethyl-2-methyl pentanoate; 4-hydroxy-3-ethoxybenzaldehyde;
4-hydroxy-3-methoxybenzaldehyde; 3-hydroxy-2-methyl-4-pyrone;
3-hydroxy-2-ethyl-4-pyrone and mixtures thereof; t.) a perfume
composition comprising, based on total perfume composition weight,
less than 10% a perfume having a Clog P greater than 5.0; u.) a
perfume composition comprising geranyl palmitate; or v.) a perfume
composition comprising a first and an optional second material,
said first material having: (i) a Clog P of at least 2; (ii) a
boiling point of less than about 280.degree. C.; and second
optional second material, when present, having (i) a Clog P of less
than 2.5; and (ii) a ODT of less than about 100 ppb.
19. A consumer product according to claim 16 wherein said resin
material comprises a reaction product of an aldehyde, with an
amine, amine is selected from the group consisting of melamine,
urea, benzoguanamine, glycoluril, and mixtures thereof.
20. A consumer product according to claim 16 wherein said
emulsifier comprises a moiety selected from the group consisting of
carboxy, hydroxyl, thiol, amine, amide and combinations thereof,
said emulsifier having a pKa of less than 5.
21. A consumer product according to claim 16 wherein said core
material comprises a material selected from the group consisting of
vegetable oil, esters of vegetable oils, esters, straight or
branched chain hydrocarbons, partially hydrogenated terphenyls,
dialkyl phthalates, alkyl biphenyls, alkylated naphthalene,
petroleum spirits, aromatic solvents, silicone oils, and mixtures
there of.
22. A consumer product according to claim 16 wherein in any of the
process steps, the pH of the first and second solutions is
controlled such that the pH of said first and second solution is
from about 3.0 to 7.0.
23. A consumer product according to claim 16 wherein in step f.),
from about 0% to about 10%, based on total second composition
weight, of a salt comprising an anion and cation, said anion being
selected from the group consisting of chloride, sulfate, phosphate,
nitrate, polyphosphate, citrate, maleate, fumarate and mixtures
thereof; and said cation being selected from the group consisting
of a Periodic Group IA element, Periodic Group IIA element,
ammonium cation and mixtures thereof.
24. A method of treating and/or cleaning a situs, said method
comprising a. optionally washing and/or rinsing said situs; b.
contacting said situs with a composition according to claim 16; and
c. optionally washing and/or rinsing said situs.
25. A situs treated with the consumer product of claim 16.
Description
CROSS-REFERENCES TO RELATED APPLICATIONS
[0001] This application is a continuation of and claims priority
under 35 U.S.C. .sctn.120 to U.S. application Ser. No. 12/156,726,
filed Jun. 4, 2008, which in turn claims priority under 35 U.S.C.
.sctn.119(e) to U.S. Provisional Application Ser. No. 60/934,071
filed Jun. 11, 2007.
FIELD OF INVENTION
[0002] The present application relates to benefit agent containing
delivery particles, compositions comprising such particles, and
processes for making and using such particles and compositions.
BACKGROUND OF THE INVENTION
[0003] Benefit agents, such as perfumes, silicones, waxes, flavors,
vitamins and fabric softening agents, are expensive and/or
generally less effective when employed at high levels in consumer
products, for example, personal care compositions, cleaning
compositions, and fabric care compositions. As a result, there is a
desire to maximize the effectiveness of such benefit agents. One
method of achieving such objective is to improve the delivery
efficiencies of such benefit agents. Unfortunately, it is difficult
to improve the delivery efficiencies of benefit agents as such
agents may be lost do to the agents' physical or chemical
characteristics, or such agents may be incompatible with other
compositional components or the situs that is treated.
[0004] Accordingly, there is a need for a benefit agent containing
delivery particle that provides improved benefit agent delivery
efficiency.
SUMMARY OF THE INVENTION
[0005] The present invention relates to benefit agent containing
delivery particles comprising a core material and a wall material
that at least partially surrounds the core material. The present
invention also relates to compositions comprising said particles,
and processes for making and using such particles and
compositions.
DETAILED DESCRIPTION OF THE INVENTION
Definitions
[0006] As used herein "consumer product" means baby care, beauty
care, fabric & home care, family care, feminine care, health
care, snack and/or beverage products or devices intended to be used
or consumed in the form in which it is sold, and not intended for
subsequent commercial manufacture or modification. Such products
include but are not limited to diapers, bibs, wipes; products for
and/or methods relating to treating hair (human, dog, and/or cat),
including, bleaching, coloring, dyeing, conditioning, shampooing,
styling; deodorants and antiperspirants; personal cleansing;
cosmetics; skin care including application of creams, lotions, and
other topically applied products for consumer use; and shaving
products, products for and/or methods relating to treating fabrics,
hard surfaces and any other surfaces in the area of fabric and home
care, including: air care, car care, dishwashing, fabric
conditioning (including softening), laundry detergency, laundry and
rinse additive and/or care, hard surface cleaning and/or treatment,
and other cleaning for consumer or institutional use; products
and/or methods relating to bath tissue, facial tissue, paper
handkerchiefs, and/or paper towels; tampons, feminine napkins;
products and/or methods relating to oral care including
toothpastes, tooth gels, tooth rinses, denture adhesives, tooth
whitening; over-the-counter health care including cough and cold
remedies, pain relievers, RX pharmaceuticals, pet health and
nutrition, and water purification; processed food products intended
primarily for consumption between customary meals or as a meal
accompaniment (non-limiting examples include potato chips, tortilla
chips, popcorn, pretzels, corn chips, cereal bars, vegetable chips
or crisps, snack mixes, party mixes, multigrain chips, snack
crackers, cheese snacks, pork rinds, corn snacks, pellet snacks,
extruded snacks and bagel chips); and coffee.
[0007] As used herein, the term "cleaning composition" includes,
unless otherwise indicated, granular or powder-form all-purpose or
"heavy-duty" washing agents, especially cleaning detergents;
liquid, gel or paste-form all-purpose washing agents, especially
the so-called heavy-duty liquid types; liquid fine-fabric
detergents; hand dishwashing agents or light duty dishwashing
agents, especially those of the high-foaming type; machine
dishwashing agents, including the various tablet, granular, liquid
and rinse-aid types for household and institutional use; liquid
cleaning and disinfecting agents, including antibacterial hand-wash
types, cleaning bars, mouthwashes, denture cleaners, dentifrice,
car or carpet shampoos, bathroom cleaners; hair shampoos and
hair-rinses; shower gels and foam baths and metal cleaners; as well
as cleaning auxiliaries such as bleach additives and "stain-stick"
or pre-treat types, substrate-laden products such as dryer added
sheets, dry and wetted wipes and pads, nonwoven substrates, and
sponges; as well as sprays and mists.
[0008] As used herein, the term "fabric care composition" includes,
unless otherwise indicated, fabric softening compositions, fabric
enhancing compositions, fabric freshening compositions and
combinations there of.
[0009] As used herein, the phrase "benefit agent containing
delivery particle" encompasses microcapsules including perfume
microcapsules.
[0010] As used herein, the terms "particle", "benefit agent
containing delivery particle", "capsule" and "microcapsule" are
synonymous.
[0011] As used herein, the articles including "a" and "an" when
used in a claim, are understood to mean one or more of what is
claimed or described.
[0012] As used herein, the terms "include", "includes" and
"including" are meant to be non-limiting.
[0013] The test methods disclosed in the Test Methods Section of
the present application should be used to determine the respective
values of the parameters of Applicants' inventions.
[0014] Unless otherwise noted, all component or composition levels
are in reference to the active portion of that component or
composition, and are exclusive of impurities, for example, residual
solvents or by-products, which may be present in commercially
available sources of such components or compositions.
[0015] All percentages and ratios are calculated by weight unless
otherwise indicated. All percentages and ratios are calculated
based on the total composition unless otherwise indicated.
[0016] It should be understood that every maximum numerical
limitation given throughout this specification includes every lower
numerical limitation, as if such lower numerical limitations were
expressly written herein. Every minimum numerical limitation given
throughout this specification will include every higher numerical
limitation, as if such higher numerical limitations were expressly
written herein. Every numerical range given throughout this
specification will include every narrower numerical range that
falls within such broader numerical range, as if such narrower
numerical ranges were all expressly written herein.
Benefit Agent Delivery Particle
[0017] Applicants discovered that the problem of achieving
effective and efficient benefit agent delivery can be solved in an
economical manner when a benefit agent containing delivery
particle, comprising a core material and a wall material that at
least partially surrounds said core material and having a certain
combination of physical and chemical characteristics is employed.
Such physical and chemical characteristics are Fracture Strength,
Particle Size, Particle Wall Thickness and Benefit Agent
Leakage.
[0018] In a first aspect, a benefit agent delivery particles
comprising a core material and a shell, said shell at least
partially surrounding said core material, is disclosed. As tested
in accordance with Applicants test methods, at least 75%, 85% or
even 90% of said benefit agent delivery particles have a fracture
strength of from about 0.2 MPa to about 10 MPa, from about 0.4 MPa
to about 5 MPa, from about 0.6 MPa to about 3.5 MPa, or even from
about 0.7 MPa to about 3 MPa; and a benefit agent leakage of from
0% to about 30%, from 0% to about 20%, or even from 0% to about
5%.
[0019] In one aspect, at least 75%, 85% or even 90% of said benefit
agent delivery particles may have a particle size of from about 1
microns to about 80 microns, about 5 microns to 60 microns, from
about 10 microns to about 50 microns, or even from about 15 microns
to about 40 microns.
[0020] In one aspect, at least 75%, 85% or even 90% of said benefit
agent delivery particles may have a particle wall thickness of from
about 30 nm to about 250 nm, from about 80 nm to about 180 nm, or
even from about 100 nm to about 160 nm.
[0021] In one aspect, said benefit agent delivery particles' core
material may comprise a material selected from the group consisting
of a perfume raw material and/or optionally a material selected
from the group consisting of vegetable oil, including neat and/or
blended vegetable oils including caster oil, coconut oil,
cottonseed oil, grape oil, rapeseed, soybean oil, corn oil, palm
oil, linseed oil, safflower oil, olive oil, peanut oil, coconut
oil, palm kernel oil, castor oil, lemon oil and mixtures thereof;
esters of vegetable oils, esters, including dibutyl adipate,
dibutyl phthalate, butyl benzyl adipate, benzyl octyl adipate,
tricresyl phosphate, trioctyl phosphate and mixtures thereof;
straight or branched chain hydrocarbons, including those straight
or branched chain hydrocarbons having a boiling point of greater
than about 80.degree. C.; partially hydrogenated terphenyls,
dialkyl phthalates, alkyl biphenyls, including
monoisopropylbiphenyl, alkylated naphthalene, including
dipropylnaphthalene, petroleum spirits, including kerosene, mineral
oil and mixtures thereof; aromatic solvents, including benzene,
toluene and mixtures thereof; silicone oils; and mixtures there
of.
[0022] In one aspect, said benefit agent delivery particles' wall
material may comprise a suitable resin including the reaction
product of an aldehyde and an amine, suitable aldehydes include,
formaldehyde. Suitable amines include melamine, urea,
benzoguanamine, glycoluril, and mixtures thereof. Suitable
melamines include, methylol melamine, methylated methylol melamine,
imino melamine and mixtures thereof. Suitable ureas include,
dimethylol urea, methylated dimethylol urea, urea-resorcinol, and
mixtures thereof. Suitable materials for making may be obtained
from one or more of the following companies Solutia Inc. (St Louis,
Mo. U.S.A.), Cytec Industries (West Paterson, N.J. U.S.A.),
sigma-Aldrich (St. Louis, Mo. U.S.A.).
[0023] In one aspect, said benefit agent delivery particles' core
material may comprise a material selected from the group consisting
of: [0024] a.) a perfume composition having a Clog P of less than
4.5, less than, 4.25, less than 4.0 or even less than 3.75; [0025]
b.) a perfume composition comprising, based on total perfume
composition weight, 60% or even 70% perfume materials having a Clog
P of less than 4.0; [0026] c.) a perfume composition comprising,
based on total perfume composition weight, 35% or 50% or even 60%
perfume materials having a Clog P of less than 3.5; [0027] d.) a
perfume composition comprising, based on total perfume composition
weight, 40% perfume materials having a Clog P of less than 4.0 or
even less than 3.5 and at least 1% perfume materials having a Clog
P of less than 2.0; [0028] e.) a perfume composition comprising,
based on total perfume composition weight, 40% perfume materials
having a Clog P of less than 4.0 or even less than 3.5 and at least
15% perfume materials having a Clog P of less than 3.0; [0029] f.)
a perfume composition comprising, based on total perfume
composition weight, at least 1% or even 2% of a butanoate ester and
at least 1% of a pentanoate ester; [0030] g.) a perfume composition
comprising, based on total perfume composition weight, at least 2%
or even 3% an ester comprising an allyl moiety and at least 10%,
25% or even 30% of another perfume comprising an ester moiety;
[0031] h.) a perfume composition comprising, based on total perfume
composition weight, at least 1% or even 5% of an aldehyde
comprising an alkyl chain moiety; [0032] i.) a perfume composition
comprising, based on total perfume composition weight, at least 2%
of a butanoate ester; [0033] j.) a perfume composition comprising,
based on total perfume composition weight, at least 1% of a
pentanoate ester; [0034] k.) a perfume composition comprising,
based on total perfume composition weight, at least 3% of an ester
comprising an allyl moiety and 1% of an aldehyde comprising an
alkyl chain moiety; [0035] l.) a perfume composition comprising,
based on total perfume composition weight, at least 25% of a
perfume comprising an ester moiety and 1% of an aldehyde comprising
an alkyl chain moiety; [0036] m.) a perfume compositions
comprising, based on total perfume composition weight, at least 2%
or even 10% of a material selected from ionones, like
4-(2,6,6-trimethyl-1-cyclohexenyl)-3-buten-2-one,
4-(2,6,6-trimethyl-2-cyclohexenyl)-3-buten-2-one and 3-buten-2-one,
3-methyl-4-(2,6,6-trimethyl-1-cyclohexen-2-yl)- and mixtures
thereof; [0037] n.) a perfume composition comprising, based on
total perfume composition weight, at least 0.1% or even 1% of
tridec-2-enonitrile, and mandaril, and mixtures thereof; [0038] o.)
a perfume composition comprising, based on total perfume
composition weight, at least 2% or even 5% of a material selected
from 3,7-Dimethyl-6-octene nitrile,
2-cyclohexylidene-2-phenylacetonitrile and mixtures thereof; [0039]
p.) a perfume composition comprising, based on total perfume
composition weight, at least 80% of one or more perfumes comprising
a moiety selected from the group consisting of esters, aldehydes,
ionones, nitriles, ketones and combinations thereof; [0040] q.) a
perfume composition comprising, based on total perfume composition
weight, at least 3% of an ester comprising an allyl moiety; a
perfume composition comprising, based on total perfume composition
weight, at least 20%, 30% or even 50% of a material selected from
the group consisting of: 1-methylethyl-2-methylbutanoate;
ethyl-2-methyl pentanoate; 1,5-dimethyl-1-ethenylhexyl-4-enyl
acetate; p-metnh-1-en-8-yl acetate;
4-(2,6,6-trimethyl-2-cyclohexenyl)-3-buten-2-one;
4-acetoxy-3-methoxy-1-propenylbenzene; 2-propenyl
cyclohexanepropionate; bicyclo[2.2.1]hept-5-ene-2-carboxylic acid,
3-(1-methylethyl)-ethyl ester; bycyclo[2.2.1]heptan-2-ol,
1,7,7-trimethyl-, acetate; 1,5-dimethyl-1-ethenylhex-4-enylacetate;
hexyl 2-methyl propanoate; ethyl-2-methylbutanoate; 4-undecanone;
5-heptyldihydro-2(3h)-furanone; 1,6-nonadien-3-ol,3,7dimethyl-;
3,7-dimethylocta-1,6-dien-3-ol;
3-cyclohexene-1-carboxaldehyde,dimethyl-; 3,7-dimethyl-6-octene
nitrile; 4-(2,6,6-trimethyl-1-cyclohexenyl)-3-buten-2-one;
tridec-2-enonitrile; patchouli oil; ethyl
tricycle[5.2.1.0]decan-2-carboxylate;
2,2-dimethyl-cyclohexanepropanol; hexyl ethanoate;
7-acetyl,1,2,3,4,5,6,7,8-octahydro-1,1,6,7-tetramethyl naphtalene;
allyl-cyclohexyloxy acetate; methyl nonyl acetic aldehyde;
1-spiro[4,5]dec-7-en-7-yl-4-pentenen-1-one;
7-octen-2-ol,2-methyl-6-methylene-,dihydro;
cyclohexanol,2-(1,1-dimethylethyl)-, acetate;
hexahydro-4,7-methanoinden-5(6)-yl
propionatehexahydro-4,7-methanoinden-5(6)-yl propionate;
2-methoxynaphtalene;
1-(2,6,6-trimethyl-3-cyclohexenyl)-2-buten-1-one;
1-(2,6,6-trimethyl-2-cyclohexenyl)-2-buten-1-one;
3,7-dimethyloctan-3-ol; 3-buten-2-one,
3-methyl-4-(2,6,6-trimethyl-1-cyclohexen-2-yl)-; hexanoic acid,
2-propenyl ester; (z)-non-6-en-1-al; 1-decyl aldehyde; 1-octanal;
4-t-butyl-.alpha.-methylhydrocinnamaldehyde;
alpha-hexylcinnamaldehyde; ethyl-2,4-hexadienoate; 2-propenyl
3-cyclohexanepropanoate; and mixtures thereof; [0041] r.) a perfume
composition comprising, based on total perfume composition weight,
at least 20%, 30% or even 50% of a material selected from the group
consisting of: 1-methylethyl-2-methylbutanoate; ethyl-2-methyl
pentanoate; 1,5-dimethyl-1-ethenylhex-4-enyl acetate;
p-menth-1-en-8-yl acetate;
4-(2,6,6-trimethyl-2-cyclohexenyl)-3-buten-2-one;
4-acetoxy-3-methoxy-1-propenylbenzene; 2-propenyl
cyclohexanepropionate; bicyclo[2.2.1]hept-5-ene-2-carboxylic acid,
3-(1-methylethyl)-ethyl ester; bycyclo[2.2.1]heptan-2-ol,
1,7,7-trimethyl-, acetate; 1,5-dimethyl-1-ethenylhex-4-enyl
acetate; hexyl 2-methyl propanoate; ethyl-2-methylbutanoate,
4-undecanolide; 5-heptyldihydro-2(3h)-furanone; 5-hydroxydodecanoic
acid; decalactones; undecalactones; 1,6-nonadien-3-ol,3,7dimethyl-;
3,7-dimethylocta-1,6-dien-3-ol;
3-cyclohexene-1-carboxaldehyde,dimethyl-; 3,7-dimethyl-6-octene
nitrile; 4-(2,6,6-trimethyl-1-cyclohexenyl)-3-buten-2-one;
tridec-2-enonitrile; patchouli oil; ethyl
tricycle[5.2.1.0]decan-2-carboxylate;
2,2-dimethyl-cyclohexanepropanol; allyl-cyclohexyloxy acetate;
methyl nonyl acetic aldehyde;
1-spiro[4,5]dec-7-en-7-yl-4-pentenen-1-one;
7-octen-2-ol,2-methyl-6-methylene-,dihydro,
cyclohexanol,2-(1,1-dimethylethyl)-, acetate;
hexahydro-4,7-methanoinden-5(6)-yl
propionatehexahydro-4,7-methanoinden-5(6)-yl propionate;
2-methoxynaphtalene;
1(2,6,6-trimethyl-3-cyclohexenyl)-2-buten-1-one;
1-(2,6,6-trimethyl-2-cyclohexenyl)-2-buten-1-one;
3,7-dimethyloctan-3-ol; 3-buten-2-one,
3-methyl-4-(2,6,6-trimethyl-1-cyclohexen-2-yl)-; hexanoic acid,
2-propenyl ester; (z)-non-6-en-1-al; 1-decyl aldehyde; 1-octanal;
4-t-butyl-.alpha.-methylhydrocinnamaldehyde;
ethyl-2,4-hexadienoate; 2-propenyl 3-cyclohexanepropanoate; and
mixtures thereof; [0042] s.) a perfume composition comprising,
based on total perfume composition weight, at least 5% of a
material selected from the group consisting of
3-cyclohexene-1-carboxaldehyde,dimethyl-; 3-buten-2-one,
3-methyl-4-(2,6,6-trimethyl-1-cyclohexen-2-yl)-; patchouli oil;
Hexanoic acid, 2-propenyl ester; 1-Octanal; 1-decyl aldehyde;
(z)-non-6-en-1-al; methyl nonyl acetic aldehyde;
ethyl-2-methylbutanoate; 1-methylethyl-2-methylbutanoate;
ethyl-2-methyl pentanoate; 4-hydroxy-3-ethoxybenzaldehyde;
4-hydroxy-3-methoxybenzaldehyde; 3-hydroxy-2-methyl-4-pyrone;
3-hydroxy-2-ethyl-4-pyrone and mixtures thereof; [0043] t.) a
perfume composition comprising, based on total perfume composition
weight, less than 10% or even 5% perfumes having a Clog P greater
than 5.0; [0044] u.) a perfume composition comprising geranyl
palmitate; or [0045] v.) a perfume composition comprising a first
and an optional second material, said first material having: [0046]
(i) a Clog P of at least 2, from about 2 to about 12, from about
2.5 to about 8, or even from about 2.5 to about 6; [0047] (ii) a
boiling point of less than about 280.degree. C., from about
50.degree. C. to about less than about 280.degree. C., from about
50.degree. C. to about less than about 265.degree. C., or even from
about 80.degree. C. to about less than about 250.degree. C.; and
[0048] second optional second material, when present, having [0049]
(i) a Clog P of less than 2.5, or even less than 2 to about 0.1;
and [0050] (ii) a ODT of less than about 100 ppb, from about
0.00001 ppb to about less than about 100 ppb, from about 0.00001
ppb to about less than about 50 ppb or even from about 0.00001 ppb
to about less than about 20 ppb.
[0051] In one aspect, said benefit agent delivery particles may
comprise, based on total benefit agent delivery particle weight, at
least 1 weight %, from about 20 to about 95 weight %, from about 50
to about 90 weight %, or even from about 80 to about 85 weight % of
a benefit agent.
[0052] In one aspect, said benefit agent delivery particles' core
material may comprise, based on total core material weight, at
least about 20, from about 50 to about 70, or even from about 60 to
about 100 wt % benefit agent.
[0053] In one aspect, said benefit agent delivery particles may
comprise, based on total particle weight, from about 20 weight % to
about 95 weight %, from about 50 weight % to about 90 weight %,
from about 70 weight % to about 85 weight %, or even from about 80
weight % to about 85 weight % of a perfume composition.
[0054] In one aspect, said benefit agent delivery particles may be
spray dried said benefit agent delivery particles.
[0055] In one aspect, said benefit agent delivery particles may
have any combination of the aforementioned parameters as listed in
the aforementioned aspects.
[0056] Suitable materials for making may be supplied from one or
more of the following companies Firmenich (Geneva, Switzerland),
Givaudan (Argenteuil, France), IFF (Hazlet, N.J., U.S.A), Quest
(Mount Olive, N.J., U.S.A.), Bedoukian (Danbury, Conn., U.S.A.),
Sigma Aldrich (St. Louis, Mo., U.S.A.), Millennium Specialty
Chemicals (Olympia Fields, Ill., U.S.A.), Polarone International
(Jersey City, N.J., U.S.A.), Fragrance Resources (Keyport, N.J.,
U.S.A.), and Aroma & Flavor Specialties (Danbury, Conn.,
U.S.A.) or made by following the teachings of Example I of U.S.
Pat. No. 5,625,205 and replacing the succinic acid with palmitic
acid or Example II of U.S. Pat. No. 5,652,205 and replacing lauroyl
chloride with palmitoyl chloride.
Process of Making Benefit Agent Containing Delivery Particles
[0057] In one aspect, a process comprising: [0058] a.) preparing a
first solution comprising, based on total solution weight from
about 20% to about 90%, from about 40% to about 80%, or even from
about 60% to about 80% water, a first emulsifier and a first resin,
the ratio of said first emulsifier and said first resin being from
about 0.1:0 to about 10:0, from about 0.1:1 to about 10:1, from
about 0.5:1 to about 3:1, or even from about 0.8:1 to about 1.1:1;
[0059] b.) preparing a second solution comprising based on total
solution weight from about 20% to about 95% water, a second
emulsifier and a second resin, the ratio of said second emulsifier
and said second resin being from about 0:1 to about 3:1, from about
0.04:1 to about 0.2:1, or even from about 0.05:1 to about 0.15:1;
[0060] c.) combining a core material and said first solution to
form a first composition; [0061] d.) emulsifying said first
composition; [0062] e.) combining said first composition and said
second solution to form a second composition and optionally
combining any processing aids and said second composition--said
first composition and said second solution may be combined in any
order but in one aspect said second solution is added to said first
composition or said second solution and said first composition are
combined simultaneously; [0063] f.) mixing said second composition
for at least 15 minutes, at least 1 hour or even from about 4 hours
to about 100 hours at a temperature of from about 25.degree. C. to
about 100.degree. C., from about 45.degree. C. to about 90.degree.
C., or even from about 50.degree. C. to about 80.degree. C. heat
and optionally combining any processing aids to said second
composition; [0064] g.) optionally combining any scavenger
material, structurant, and/or anti-agglomeration agent with said
second composition during step f.) or thereafter--such materials
may be combined in any order but in one aspect the scavenger
material is combined first, any structurant second, and then
anti-agglomeration agent is combined; and [0065] h.) optionally
spray drying said second composition is disclosed.
[0066] In one aspect of the aforementioned process, said core
material comprises a perfume raw material.
[0067] In one aspect, said benefit agent delivery particles' core
material may comprise a material selected from the group consisting
of: [0068] a.) a perfume composition having a Clog P of less than
4.5, less than, 4.25, less than 4.0 or even less than 3.75; [0069]
b.) a perfume composition comprising, based on total perfume
composition weight, 60% or even 70% perfume materials having a Clog
P of less than 4.0; [0070] c.) a perfume composition comprising,
based on total perfume composition weight, 35% or 50% or even 60%
perfume materials having a Clog P of less than 3.5; [0071] d. a
perfume composition comprising, based on total perfume composition
weight, 40% perfume materials having a Clog P of less than 4.0 or
even less than 3.5 and at least 1% perfume materials having a Clog
P of less than 2.0; [0072] e.) a perfume composition comprising,
based on total perfume composition weight, 40% perfume materials
having a Clog P of less than 4.0 or even less than 3.5 and at least
15% perfume materials having a Clog P of less than 3.0; [0073] f.)
a perfume composition comprising, based on total perfume
composition weight, at least 1% or even 2% of a butanoate ester and
at least 1% of a pentanoate ester; [0074] g.) a perfume composition
comprising, based on total perfume composition weight, at least 2%
or even 3% of an ester comprising an allyl moiety and at least 10%,
25% or even 30% of another perfume comprising an ester moiety;
[0075] h.) a perfume composition comprising, based on total perfume
composition weight, at least 1% or even 5% of an aldehyde
comprising an alkyl chain moiety; [0076] i.) a perfume composition
comprising, based on total perfume composition weight, at least 2%
of a butanoate ester; [0077] j.) a perfume composition comprising,
based on total perfume composition weight, at least 1% of a
pentanoate ester; [0078] k.) a perfume composition comprising,
based on total perfume composition weight, at least 3% of an ester
comprising an allyl moiety and 1% of an aldehyde comprising an
alkyl chain moiety; [0079] l.) a perfume composition comprising,
based on total perfume composition weight, at least 25% of a
perfume comprising an ester moiety and 1% of an aldehyde comprising
an alkyl chain moiety; [0080] m.) a perfume compositions
comprising, based on total perfume composition weight, at least 2%
or even 10% of a material selected from ionones, like
4-(2,6,6-trimethyl-1-cyclohexenyl)-3-buten-2-one,
4-(2,6,6-trimethyl-2-cyclohexenyl)-3-buten-2-one and 3-buten-2-one,
3-methyl-4-(2,6,6-trimethyl-1-cyclohexen-2-yl)- and mixtures
thereof; [0081] n.) a perfume composition comprising, based on
total perfume composition weight, at least 0.1% or even 1% of
tridec-2-enonitrile, and mandaril, and mixtures thereof; [0082] o.)
a perfume composition comprising, based on total perfume
composition weight, at least 2% or even 5% of a material selected
from 3,7-Dimethyl-6-octene nitrile,
2-cyclohexylidene-2-phenylacetonitrile and mixtures thereof; [0083]
p.) a perfume composition comprising, based on total perfume
composition weight, at least 80% of one or more perfumes comprising
a moiety selected from the group consisting of esters, aldehydes,
ionones, nitriles, ketones and combinations thereof; [0084] q.) a
perfume composition comprising, based on total perfume composition
weight, at least 3% of an ester comprising an allyl moiety; a
perfume composition comprising, based on total perfume composition
weight, at least 20%, 30% or even 50% of a material selected from
the group consisting of: 1-methylethyl-2-methylbutanoate;
ethyl-2-methyl pentanoate; 1,5-dimethyl-1-ethenylhexyl-4-enyl
acetate; p-metnh-1-en-8-yl acetate;
4-(2,6,6-trimethyl-2-cyclohexenyl)-3-buten-2-one;
4-acetoxy-3-methoxy-1-propenylbenzene; 2-propenyl
cyclohexanepropionate; bicyclo[2.2.1]hept-5-ene-2-carboxylic acid,
3-(1-methylethyl)-ethyl ester; bycyclo[2.2.1]heptan-2-ol,
1,7,7-trimethyl-, acetate; 1,5-dimethyl-1-ethenylhex-4-enylacetate;
hexyl 2-methyl propanoate; ethyl-2-methylbutanoate; 4-undecanone;
5-heptyldihydro-2(3h)-furanone; 1,6-nonadien-3-ol,3,7dimethyl-;
3,7-dimethylocta-1,6-dien-3-ol;
3-cyclohexene-1-carboxaldehyde,dimethyl-; 3,7-dimethyl-6-octene
nitrile; 4-(2,6,6-trimethyl-1-cyclohexenyl)-3-buten-2-one;
tridec-2-enonitrile; patchouli oil; ethyl
tricycle[5.2.1.0]decan-2-carboxylate;
2,2-dimethyl-cyclohexanepropanol; hexyl ethanoate;
7-acetyl,1,2,3,4,5,6,7,8-octahydro-1,1,6,7-tetramethyl naphtalene;
allyl-cyclohexyloxy acetate; methyl nonyl acetic aldehyde;
1-spiro[4,5]dec-7-en-7-yl-4-pentenen-1-one;
7-octen-2-ol,2-methyl-6-methylene-,dihydro;
cyclohexanol,2-(1,1-dimethylethyl)-, acetate;
hexahydro-4,7-methanoinden-5(6)-ylpropionatehexahydro-4,7-methanoinden-5(-
6)-yl propionate; 2-methoxynaphtalene;
1-(2,6,6-trimethyl-3-cyclohexenyl)-2-buten-1-one;
1-(2,6,6-trimethyl-2-cyclohexenyl)-2-buten-1-one;
3,7-dimethyloctan-3-ol; 3-buten-2-one,
3-methyl-4-(2,6,6-trimethyl-1-cyclohexen-2-yl)-; hexanoic acid,
2-propenyl ester; (z)-non-6-en-1-al; 1-decyl aldehyde; 1-octanal;
4-t-butyl-.alpha.-methylhydrocinnamaldehyde;
alpha-hexylcinnamaldehyde; ethyl-2,4-hexadienoate; 2-propenyl
3-cyclohexanepropanoate; and mixtures thereof; [0085] r.) a perfume
composition comprising, based on total perfume composition weight,
at least 20%, 30% or even 50% of a material selected from the group
consisting of: 1-methylethyl-2-methylbutanoate; ethyl-2-methyl
pentanoate; 1,5-dimethyl-1-ethenylhex-4-enyl acetate;
p-menth-1-en-8-yl acetate;
4-(2,6,6-trimethyl-2-cyclohexenyl)-3-buten-2-one;
4-acetoxy-3-methoxy-1-propenylbenzene; 2-propenyl
cyclohexanepropionate; bicyclo[2.2.1]hept-5-ene-2-carboxylic acid,
3-(1-methylethyl)-ethyl ester; bycyclo[2.2.1]heptan-2-ol,
1,7,7-trimethyl-, acetate; 1,5-dimethyl-1-ethenylhex-4-enyl
acetate; hexyl 2-methyl propanoate; ethyl-2-methylbutanoate,
4-undecanolide; 5-heptyldihydro-2(3h)-furanone; 5-hydroxydodecanoic
acid; decalactones; undecalactones;
1,6-nonadien-3-ol,3,7-dimethyl-; 3,7-dimethylocta-1,6-dien-3-ol;
3-cyclohexene-1-carboxaldehyde,dimethyl-; 3,7-dimethyl-6-octene
nitrile; 4-(2,6,6-trimethyl-1-cyclohexenyl)-3-buten-2-one;
tridec-2-enonitrile; patchouli oil; ethyl
tricycle[5.2.1.0]decan-2-carboxylate;
2,2-dimethyl-cyclohexanepropanol; allyl-cyclohexyloxy acetate;
methyl nonyl acetic aldehyde;
1-spiro[4,5]dec-7-en-7-yl-4-pentenen-1-one;
7-octen-2-ol,2-methyl-6-methylene-,dihydro,
cyclohexanol,2-(1,1-dimethylethyl)-, acetate;
hexahydro-4,7-methanoinden-5(6)-ylpropionatehexahydro-4,7-methanoinden-5(-
6)-yl propionate; 2-methoxynaphtalene;
1-(2,6,6-trimethyl-3-cyclohexenyl)-2-buten-1-one;
1-(2,6,6-trimethyl-2-cyclohexenyl)-2-buten-1-one;
3,7-dimethyloctan-3-ol; 3-buten-2-one,
3-methyl-4-(2,6,6-trimethyl-1-cyclohexen-2-yl)-; hexanoic acid,
2-propenyl ester; (z)-non-6-en-1-al; 1-decyl aldehyde; 1-octanal;
4-t-butyl-.alpha.-methylhydrocinnamaldehyde;
ethyl-2,4-hexadienoate; 2-propenyl 3-cyclohexanepropanoate; and
mixtures thereof; [0086] s.) a perfume composition comprising,
based on total perfume composition weight, at least 5% of a
material selected from the group consisting of
3-cyclohexene-1-carboxaldehyde,dimethyl-; 3-buten-2-one,
3-methyl-4-(2,6,6-trimethyl-1-cyclohexen-2-yl)-; patchouli oil;
Hexanoic acid, 2-propenyl ester; 1-Octanal; 1-decyl aldehyde;
(z)-non-6-en-1-al; methyl nonyl acetic aldehyde;
ethyl-2-methylbutanoate; 1-methylethyl-2-methylbutanoate;
ethyl-2-methyl pentanoate; 4-hydroxy-3-ethoxybenzaldehyde;
4-hydroxy-3-methoxybenzaldehyde; 3-hydroxy-2-methyl-4-pyrone;
3-hydroxy-2-ethyl-4-pyrone and mixtures thereof; [0087] t.) a
perfume composition comprising, based on total perfume composition
weight, less than 10% or even 5% perfumes having a Clog P greater
than 5.0; [0088] u.) a perfume composition comprising geranyl
palmitate; or [0089] v.) a perfume composition comprising a first
and an optional second material, said first material having: [0090]
(i) a Clog P of at least 2, from about 2 to about 12, from about
2.5 to about 8, or even from about 2.5 to about 6; [0091] (ii) a
boiling point of less than about 280.degree. C., from about
50.degree. C. to about less than about 280.degree. C., from about
50.degree. C. to about less than about 265.degree. C., or even from
about 80.degree. C. to about less than about 250.degree. C.; and
[0092] second optional second material, when present, having [0093]
(i) a Clog P of less than 2.5, or even less than 2 to about 0.1;
and [0094] (ii) a ODT of less than about 100 ppb, from about
0.00001 ppb to about less than about 100 ppb, from about 0.00001
ppb to about less than about 50 ppb or even from about 0.00001 ppb
to about less than about 20 ppb.
[0095] In one or more aspects of the process, said first and second
resins may comprise the reaction product of an aldehyde and an
amine, suitable aldehydes include, formaldehyde. Suitable amines
include melamine, urea, benzoguanamine, glycoluril, and mixtures
thereof. Suitable melamines include, methylol melamine, methylated
methylol melamine, imino melamine and mixtures thereof. Suitable
ureas include, dimethylol urea, methylated dimethylol urea,
urea-resorcinol, and mixtures thereof.
[0096] In one or more aspects of the process, said first and second
emulsifiers may comprise a moiety selected from the group
consisting of carboxy, hydroxyl, thiol, amine, amide and
combinations thereof. In one aspect, said emulsifier may have a pKa
of less than 5, preferably greater than 0 but less than 5.
Emulsifiers include acrylic acid-alkyl acrylate copolymer,
poly(acrylic acid), polyoxyalkylene sorbitan fatty esters,
polyalkylene co-carboxy anhydrides, polyalkylene co-maleic
anhydrides, poly(methyl vinyl ether-co-maleic anhydride),
poly(propylene-co-maleic anhydride), poly(butadiene co-maleic
anhydride), and poly(vinyl acetate-co-maleic anhydride), polyvinyl
alcohols, polyalkylene glycols, polyoxyalkylene glycols, and
mixtures thereof.
[0097] In one or more aspects of the process, said core material
may comprise perfume raw material and/or optionally a material
selected from the group consisting of a material selected from the
group consisting of vegetable oil, including neat and/or blended
vegetable oils including caster oil, coconut oil, cottonseed oil,
grape oil, rapeseed, soybean oil, corn oil, palm oil, linseed oil,
safflower oil, olive oil, peanut oil, coconut oil, palm kernel oil,
castor oil, lemon oil and mixtures thereof; esters of vegetable
oils, esters, including dibutyl adipate, dibutyl phthalate, butyl
benzyl adipate, benzyl octyl adipate, tricresyl phosphate, trioctyl
phosphate and mixtures thereof; straight or branched chain
hydrocarbons, including those straight or branched chain
hydrocarbons having a boiling point of greater than about
80.degree. C.; partially hydrogenated terphenyls, dialkyl
phthalates, alkyl biphenyls, including monoisopropylbiphenyl,
alkylated naphthalene, including dipropylnaphthalene, petroleum
spirits, including kerosene, mineral oil and mixtures thereof;
aromatic solvents, including benzene, toluene and mixtures thereof;
silicone oils; and mixtures there of.
[0098] In one or more aspects of the process, the pH of the first
and second solutions may be controlled such that the pH of said
first and second solution is from about 3.0 to 7.0.
[0099] In one or more aspects of the process, during step f.), from
about 0% to about 10%, from about 1% to about 5% or even from about
2% to about 4%, based on total second composition weight, of a salt
comprising an anion and cation, said anion being selected from the
group consisting of chloride, sulfate, phosphate, nitrate,
polyphosphate, citrate, maleate, fumarate and mixtures thereof; and
said cation being selected from the group consisting of a Periodic
Group IA element, Periodic Group IIA element, ammonium cation and
mixtures thereof, preferably sodium sulfate, may be combined with
said second composition.
[0100] In one or more aspects of the process, any of the
aforementioned processing parameters may be combined.
[0101] Useful structurant materials that may be added to adequately
suspend the benefit agent containing delivery particles include
polysaccharides, for example, gellan gum, waxy maize or dent corn
starch, octenyl succinated starches, derivatized starches such as
hydroxyethylated or hydroxypropylated starches, carrageenan, guar
gum, pectin, xanthan gum, and mixtures thereof; modified celluloses
such as hydrolyzed cellulose acetate, hydroxy propyl cellulose,
methyl cellulose, and mixtures thereof; modified proteins such as
gelatin; hydrogenated and non-hydrogenated polyalkenes, and
mixtures thereof; inorganic salts, for example, magnesium chloride,
calcium chloride, calcium formate, magnesium formate, aluminum
chloride, potassium permanganate, laponite clay, bentonite clay and
mixtures thereof; polysaccharides in combination with inorganic
salts; quaternized polymeric materials, for example, polyether
amines, alkyl trimethyl ammonium chlorides, diester ditallow
ammonium chloride; imidazoles; nonionic polymers with a pKa less
than 6.0, for example polyethyleneimine, polyethyleneimine
ethoxylate; polyurethanes. Such materials can be obtained from CP
Kelco Corp. of San Diego, Calif., USA; Degussa AG or Dusseldorf,
Germany; BASF AG of Ludwigshafen, Germany; Rhodia Corp. of
Cranbury, N.J., USA; Baker Hughes Corp. of Houston, Tex., USA;
Hercules Corp. of Wilmington, Del., USA; Agrium Inc. of Calgary,
Alberta, Canada, ISP of New Jersey, U.S.A.
[0102] Useful anti-agglomeration agent materials include, divalent
salts such as magnesium salts, for example, magnesium chloride,
magnesium acetate, magnesium phosphate, magnesium formate,
magnesium boride, magnesium titanate, magnesium sulfate
heptahydrate; calcium salts, for example, calcium chloride, calcium
formate, calcium acetate, calcium bromide; trivalent salts, such as
aluminum salts, for example, aluminum sulfate, aluminum phosphate,
aluminum chloride hydrate and polymers that have the ability to
suspend anionic particles such as suspension polymers, for example,
polyethylene imines, alkoxylated polyethylene imines,
polyquaternium-6 and polyquaternium-7.
[0103] In one aspect of the invention, benefit agent containing
delivery particles are manufactured and are subsequently coated
with a material to reduce the rate of leakage of the benefit agent
from the particles when the particles are subjected to a bulk
environment containing, for example, surfactants, polymers, and
solvents. Non-limiting examples of coating materials that can serve
as barrier materials include materials selected from the group
consisting of pyrrolidone polymers, such as polyvinyl pyrrolidone
homopolymer, and its various copolymers with styrene, vinyl
acetate, imidazoles, primary and secondary amine containing
monomers, polyethyleneimines, including ethoxylated
polyethyeleimines, methyl acrylate, polyvinyl acetal; maleic
anhydride; polyvinyl alcohol homopolymer, and its various
copolymers with vinyl acetate, 2-acrylamide-2-methylpropane
sulfonate, primary and secondary amine containing monomers, methyl
acrylate; polyacrylamides; polyacrylic acids; polyethyleneimines,
ethoxylated polyethyleneimines; microcrystalline waxes; paraffin
waxes; modified polysaccharides such as waxy maize or dent corn
starch, octenyl succinated starches, derivatized starches such as
hydroxyethylated or hydroxypropylated starches, carrageenan, guar
gum, pectin, xanthan gum; modified celluloses such as hydrolyzed
cellulose acetate, hydroxy propyl cellulose, methyl cellulose, and
the like; modified proteins such as gelatin; hydrogenated and
non-hydrogenated polyalkenes; fatty acids; hardened shells such as
urea crosslinked with formaldehyde, gelatin-polyphosphate,
melamine-formaldehyde, polyvinyl alcohol cross-linked with sodium
tetraborate or gluteraldehyde; latexes of styrene-butadiene, ethyl
cellulose, inorganic materials such as clays including magnesium
silicates, aluminosilicates; sodium silicates, and the like; and
mixtures thereof. Such materials can be obtained from CP Kelco
Corp. of San Diego, Calif., USA; Degussa AG or Dusseldorf, Germany;
BASF AG of Ludwigshafen, Germany; Rhodia Corp. of Cranbury, N.J.,
USA; Baker Hughes Corp. of Houston, Tex., USA; Hercules Corp. of
Wilmington, Del., USA; Agrium Inc. of Calgary, Alberta, Canada, ISP
of New Jersey U.S.A. In one aspect, for example, wherein the
particle is employed in a fabric conditioning composition, the
coating material comprises sodium silicate. While not being bound
by theory, it is believed that sodium silicate's solubility at high
pH, but poor solubility at low pH makes it an ideal material for
use on particles that may be used in compositions that are
formulated at pH below 7 but used in an environment wherein the pH
is greater or equal to 7. However, the coating aspect of the
present invention is not limited to the benefit agent containing
delivery particles of the present invention as any benefit agent
containing delivery particle may benefit from the coatings and
coating processes disclosed herein.
[0104] In one aspect, benefit agent containing delivery particles
may be combined with a formaldehyde scavenger. In one aspect, such
benefit agent containing delivery particles may comprise the
benefit agent containing delivery particles of the present
invention. Suitable formaldehyde scavengers include materials
selected from the group consisting of sodium bisulfite, melamine,
urea, ethylene urea, cysteine, cysteamine, lysine, glycine, serine,
carnosine, histidine, glutathione, 3,4-diaminobenzoic acid,
allantoin, glycouril, anthranilic acid, methyl anthranilate, methyl
4-aminobenzoate, ethyl acetoacetate, acetoacetamide, malonamide,
ascorbic acid, 1,3-dihydroxyacetone dimer, biuret, oxamide,
benzoguanamine, pyroglutamic acid, pyrogallol, methyl gallate,
ethyl gallate, propyl gallate, triethanol amine, succinamide,
thiabendazole, benzotriazol, triazole, indoline, sulfanilic acid,
oxamide, sorbitol, glucose, cellulose, poly(vinyl alcohol),
partially hydrolyzed poly(vinylformamide), poly(vinyl amine),
poly(ethylene imine), poly(oxyalkyleneamine), poly(vinyl
alcohol)-co-poly(vinyl amine), poly(4-aminostyrene),
poly(1-lysine), chitosan, hexane diol,
ethylenediamine-N,N'-bisacetoacetamide,
N-(2-ethylhexyl)acetoacetamide, 2-benzoylacetoacetamide,
N-(3-phenylpropyl)acetoacetamide, lilial, helional, melonal,
triplal, 5,5-dimethyl-1,3-cyclohexanedione,
2,4-dimethyl-3-cyclohexenecarboxaldehyde,
2,2-dimethyl-1,3-dioxan-4,6-dione, 2-pentanone, dibutyl amine,
triethylenetetramine, ammonium hydroxide, benzylamine,
hydroxycitronellol, cyclohexanone, 2-butanone, pentane dione,
dehydroacetic acid, or a mixture thereof. These formaldehyde
scavengers may be obtained from Sigma/Aldrich/Fluka of St. Louis,
Mo. U.S.A. or PolySciences, Inc. of Warrington, Pa., U.S.A.
[0105] Such formaldehyde scavengers are typically combined with a
slurry containing said benefit agent containing delivery particle,
at a level, based on total slurry weight, of from about 2 wt. % to
about 18 wt. %, from about 3.5 wt. % to about 14 wt. % or even from
about 5 wt. % to about 13 wt. %.
[0106] In one aspect, such formaldehyde scavengers may be combined
with a product containing a benefit agent containing delivery
particle, said scavengers being combined with said product at a
level, based on total product weight, of from about 0.005% to about
0.8%, alternatively from about 0.03% to about 0.5%, alternatively
from about 0.065% to about 0.25% of the product formulation.
[0107] In another aspect, such formaldehyde scavengers may be
combined with a slurry containing said benefit agent containing
delivery particle, at a level, based on total slurry weight, of
from about 2 wt. % to about 14 wt. %, from about 3.5 wt. % to about
14 wt. % or even from about 5 wt. % to about 14 wt. % and said
slurry may be added to a product matrix to which addition an
identical or different scavenger may be added at a level, based on
total product weight, of from about 0.005% to about 0.5%,
alternatively from about 0.01% to about 0.25%, alternatively from
about 0.05% to about 0.15% of the product formulation,
[0108] In one aspect, one or more of the aforementioned
formaldehyde scavengers may be combined with a liquid fabric
enhancing product containing a benefit agent containing delivery
particle at a level, based on total liquid fabric enhancing product
weight, of from 0.005% to about 0.8%, alternatively from about
0.03% to about 0.4%, alternatively from about 0.06% to about 0.25%
of the product formulation
[0109] In one aspect, such formaldehyde scavengers may be combined
with a consumer product, for example, a liquid laundry detergent
product containing a benefit agent containing delivery particle,
said scavengers being selected from the group consisting of sodium
bisulfite, melamine, urea, ethylene urea, cysteine, cysteamine,
lysine, glycine, serine, carnosine, histidine, glutathione,
3,4-diaminobenzoic acid, allantoin, glycouril, anthranilic acid,
methyl anthranilate, methyl 4-aminobenzoate, ethyl acetoacetate,
acetoacetamide, malonamide, ascorbic acid, 1,3-dihydroxyacetone
dimer, biuret, oxamide, benzoguanamine, pyroglutamic acid,
pyrogallol, methyl gallate, ethyl gallate, propyl gallate,
triethanol amine, succinamide, thiabendazole, benzotriazol,
triazole, indoline, sulfanilic acid, oxamide, sorbitol, glucose,
cellulose, poly(vinyl alcohol), partially hydrolyzed
poly(vinylformamide), poly(vinyl amine), poly(ethylene imine),
poly(oxyalkyleneamine), poly(vinyl alcohol)-co-poly(vinyl amine),
poly(4-aminostyrene), poly(1-lysine), chitosan, hexane diol,
ethylenediamine-N,N'-bisacetoacetamide,
N-(2-ethylhexyl)acetoacetamide, 2-benzoylacetoacetamide,
N-(3-phenylpropyl)acetoacetamide, lilial, helional, melonal,
triplal, 5,5-dimethyl-1,3-cyclohexanedione,
2,4-dimethyl-3-cyclohexenecarboxaldehyde,
2,2-dimethyl-1,3-dioxan-4,6-dione, 2-pentanone, dibutyl amine,
triethylenetetramine, ammonium hydroxide, benzylamine,
hydroxycitronellol, cyclohexanone, 2-butanone, pentane dione,
dehydroacetic acid and mixtures thereof, and combined with said
liquid laundry detergent product at a level, based on total liquid
laundry detergent product weight, of from about 0.003 wt. % to
about 0.20 wt. %, from about 0.03 wt. % to about 0.20 wt. % or even
from about 0.06 wt. % to about 0.14 wt. %.
[0110] In one aspect, such formaldehyde scavengers may be combined
with a hair conditioning product containing a benefit agent
containing delivery particle, at a level, based on total hair
conditioning product weight, of from about 0.003 wt. % to about
0.30 wt. %, from about 0.03 wt. % to about 0.20 wt. % or even from
about 0.06 wt. % to about 0.14 wt. %., said selection of scavengers
being identical to the list of scavengers in the previous paragraph
relating to a liquid laundry detergent product.
[0111] Suitable equipment for use in the processes disclosed herein
may include continuous stirred tank reactors, homogenizers, turbine
agitators, recirculating pumps, paddle mixers, plough shear mixers,
ribbon blenders, vertical axis granulators and drum mixers, both in
batch and, where available, in continuous process configurations,
spray dryers, and extruders. Such equipment can be obtained from
Lodige GmbH (Paderborn, Germany), Littleford Day, Inc. (Florence,
Ky., U.S.A.), Forberg AS (Larvik, Norway), Glatt Ingenieurtechnik
GmbH (Weimar, Germany), Niro (Soeborg, Denmark), Hosokawa Bepex
Corp. (Minneapolis, Minn., U.S.A.), Arde Barinco (New Jersey,
U.S.A.).
Compositions Comprising Benefit Agent Containing Delivery
Particles
[0112] Applicants' compositions comprise any embodiment of the
particle disclosed in the present application--including any
embodiment produced by the benefit agent delivery making process
detailed in the present specification. In one aspect, said
composition is a consumer product. While the precise level of
particle that is employed depends on the type and end use of the
composition, a composition may comprise from about 0.01 to about
10, from about 0.1 to about 10, or even from about 0.2 to about 5
weight % of said particle based on total composition weight. In one
aspect, a consumer product comprising from about 0.001% to about
25%, from about 0.001% to about 10%, or from about 0.01% to about
3%, based on total consumer product mass weight, of the
aforementioned benefit agent delivery particles is disclosed.
[0113] In one aspect, a cleaning composition comprising from about
0.005% to about 10%, from about 0.01% to about 3%, or from about
0.1% to about 1% based on total cleaning composition mass weight of
the aforementioned benefit agent delivery particles is
disclosed.
[0114] In one aspect, a fabric care composition comprising from
about 0.005% to about 10%, from about 0.01% to about 3%, or from
about 0.1% to about 1% based on total fabric care mass weight of
the aforementioned benefit agent delivery particle composition is
disclosed.
[0115] In one aspect, when the aforementioned particle composition
is employed in a consumer product, for example a liquid consumer
product, the particle composition may have a deposition of at least
10%, 20%, 30%, 40%, 50%, 60%, 70%, 80%, 90%, or even 100%.
[0116] In one aspect, when the aforementioned particle composition
is employed in a consumer product, for example a liquid consumer
product, the particle composition may have less than 50%, 40%, 30%,
20%, 10% or even 0% leakage of the encapsulated benefit agent from
the microcapsules of said particle composition into said consumer
product.
[0117] In one aspect, a cleaning composition may comprise, from
about 0.1 to about 1 weight % of such particle based on total
cleaning composition weight of such particle. In one aspect, a
fabric treatment composition may comprise, based on total fabric
treatment composition weight, form about 0.01 to about 10% of such
particle.
[0118] Aspects of the invention include the use of the particles of
the present invention in laundry detergent compositions (e.g.,
TIDE.TM.), hard surface cleaners (e.g., MR CLEAN.TM.) automatic
dishwashing liquids (e.g., CASCADE.TM.), dishwashing liquids (e.g.,
DAWN.TM.), and floor cleaners (e.g., SWIFFER.TM.). Non-limiting
examples of cleaning compositions may include those described in
U.S. Pat. Nos. 4,515,705; 4,537,706; 4,537,707; 4,550,862;
4,561,998; 4,597,898; 4,968,451; 5,565,145; 5,929,022; 6,294,514;
and 6,376,445. The cleaning compositions disclosed herein are
typically formulated such that, during use in aqueous cleaning
operations, the wash water will have a pH of between about 6.5 and
about 12, or between about 7.5 and 10.5. Liquid dishwashing product
formulations typically have a pH between about 6.8 and about 9.0.
Cleaning products are typically formulated to have a pH of from
about 7 to about 12. Techniques for controlling pH at recommended
usage levels include the use of buffers, alkalis, acids, etc., and
are well known to those skilled in the art.
[0119] Fabric treatment compositions disclosed herein typically
comprise a consumer adjunct material such as a fabric softening
active ("FSA"). Suitable fabric softening actives, include, but are
not limited to, materials selected from the group consisting of
quats, amines, fatty esters, sucrose esters, silicones, dispersible
polyolefins, clays, polysaccharides, fatty oils, polymer latexes
and mixtures thereof.
Consumer Product Adjunct Materials
[0120] While not essential for the purposes of the present
invention, the non-limiting list of adjuncts illustrated
hereinafter are suitable for use in the instant compositions and
may be desirably incorporated in certain embodiments of the
invention, for example to assist or enhance performance, for
treatment of the substrate to be cleaned, or to modify the
aesthetics of the composition as is the case with perfumes,
colorants, dyes or the like. It is understood that such adjuncts
are in addition to the components that are supplied via Applicants'
delivery particles and FSAs. The precise nature of these additional
components, and levels of incorporation thereof, will depend on the
physical form of the composition and the nature of the operation
for which it is to be used. Suitable adjunct materials include, but
are not limited to, polymers, for example cationic polymers,
surfactants, builders, chelating agents, dye transfer inhibiting
agents, dispersants, enzymes, and enzyme stabilizers, catalytic
materials, bleach activators, polymeric dispersing agents, clay
soil removal/anti-redeposition agents, brighteners, suds
suppressors, dyes, additional perfume and perfume delivery systems,
structure elasticizing agents, fabric softeners, carriers,
hydrotropes, processing aids and/or pigments. In addition to the
disclosure below, suitable examples of such other adjuncts and
levels of use are found in U.S. Pat. Nos. 5,576,282, 6,306,812 B1
and 6,326,348 B1 that are incorporated by reference.
[0121] As stated, the adjunct ingredients are not essential to
Applicants' cleaning and fabric care compositions. Thus, certain
embodiments of Applicants' compositions do not contain one or more
of the following adjuncts materials: bleach activators,
surfactants, builders, chelating agents, dye transfer inhibiting
agents, dispersants, enzymes, and enzyme stabilizers, catalytic
metal complexes, polymeric dispersing agents, clay and soil
removal/anti-redeposition agents, brighteners, suds suppressors,
dyes, additional perfumes and perfume delivery systems, structure
elasticizing agents, fabric softeners, carriers, hydrotropes,
processing aids and/or pigments. However, when one or more adjuncts
are present, such one or more adjuncts may be present as detailed
below:
[0122] Surfactants--The compositions according to the present
invention can comprise a surfactant or surfactant system wherein
the surfactant can be selected from nonionic and/or anionic and/or
cationic surfactants and/or ampholytic and/or zwitterionic and/or
semi-polar nonionic surfactants. The surfactant is typically
present at a level of from about 0.1%, from about 1%, or even from
about 5% by weight of the cleaning compositions to about 99.9%, to
about 80%, to about 35%, or even to about 30% by weight of the
cleaning compositions.
[0123] Builders--The compositions of the present invention can
comprise one or more detergent builders or builder systems. When
present, the compositions will typically comprise at least about 1%
builder, or from about 5% or 10% to about 80%, 50%, or even 30% by
weight, of said builder. Builders include, but are not limited to,
the alkali metal, ammonium and alkanolammonium salts of
polyphosphates, alkali metal silicates, alkaline earth and alkali
metal carbonates, aluminosilicate builders polycarboxylate
compounds. ether hydroxypolycarboxylates, copolymers of maleic
anhydride with ethylene or vinyl methyl ether,
1,3,5-trihydroxybenzene-2,4,6-trisulphonic acid, and
carboxymethyl-oxysuccinic acid, the various alkali metal, ammonium
and substituted ammonium salts of polyacetic acids such as
ethylenediamine tetraacetic acid and nitrilotriacetic acid, as well
as polycarboxylates such as mellitic acid, succinic acid,
oxydisuccinic acid, polymaleic acid, benzene 1,3,5-tricarboxylic
acid, carboxymethyloxysuccinic acid, and soluble salts thereof.
[0124] Chelating Agents--The compositions herein may also
optionally contain one or more copper, iron and/or manganese
chelating agents. If utilized, chelating agents will generally
comprise from about 0.1% by weight of the compositions herein to
about 15%, or even from about 3.0% to about 15% by weight of the
compositions herein.
[0125] Dye Transfer Inhibiting Agents--The compositions of the
present invention may also include one or more dye transfer
inhibiting agents. Suitable polymeric dye transfer inhibiting
agents include, but are not limited to, polyvinylpyrrolidone
polymers, polyamine N-oxide polymers, copolymers of
N-vinylpyrrolidone and N-vinylimidazole, polyvinyloxazolidones and
polyvinylimidazoles or mixtures thereof. When present in the
compositions herein, the dye transfer inhibiting agents are present
at levels from about 0.0001%, from about 0.01%, from about 0.05% by
weight of the cleaning compositions to about 10%, about 2%, or even
about 1% by weight of the cleaning compositions.
[0126] Dispersants--The compositions of the present invention can
also contain dispersants. Suitable water-soluble organic materials
are the homo- or co-polymeric acids or their salts, in which the
polycarboxylic acid may comprise at least two carboxyl radicals
separated from each other by not more than two carbon atoms.
[0127] Enzymes--The compositions can comprise one or more detergent
enzymes which provide cleaning performance and/or fabric care
benefits. Examples of suitable enzymes include, but are not limited
to, hemicellulases, peroxidases, proteases, cellulases, xylanases,
lipases, phospholipases, esterases, cutinases, pectinases,
keratanases, reductases, oxidases, phenoloxidases, lipoxygenases,
ligninases, pullulanases, tannases, pentosanases, malanases,
.beta.-glucanases, arabinosidases, hyaluronidase, chondroitinase,
laccase, and amylases, or mixtures thereof. A typical combination
is a cocktail of conventional applicable enzymes like protease,
lipase, cutinase and/or cellulase in conjunction with amylase.
[0128] Enzyme Stabilizers--Enzymes for use in compositions, for
example, detergents can be stabilized by various techniques. The
enzymes employed herein can be stabilized by the presence of
water-soluble sources of calcium and/or magnesium ions in the
finished compositions that provide such ions to the enzymes.
[0129] Catalytic Metal Complexes--Applicants' compositions may
include catalytic metal complexes. One type of metal-containing
bleach catalyst is a catalyst system comprising a transition metal
cation of defined bleach catalytic activity, such as copper, iron,
titanium, ruthenium, tungsten, molybdenum, or manganese cations, an
auxiliary metal cation having little or no bleach catalytic
activity, such as zinc or aluminum cations, and a sequestrate
having defined stability constants for the catalytic and auxiliary
metal cations, particularly ethylenediaminetetraacetic acid,
ethylenediaminetetra (methyl-enephosphonic acid) and water-soluble
salts thereof. Such catalysts are disclosed in U.S. Pat. No.
4,430,243.
[0130] If desired, the compositions herein can be catalyzed by
means of a manganese compound. Such compounds and levels of use are
well known in the art and include, for example, the manganese-based
catalysts disclosed in U.S. Pat. No. 5,576,282.
[0131] Cobalt bleach catalysts useful herein are known, and are
described, for example, in U.S. Pat. Nos. 5,597,936 and 5,595,967.
Such cobalt catalysts are readily prepared by known procedures,
such as taught for example in U.S. Pat. Nos. 5,597,936, and
5,595,967.
[0132] Compositions herein may also suitably include a transition
metal complex of a macropolycyclic rigid ligand--abbreviated as
"MRL". As a practical matter, and not by way of limitation, the
compositions and cleaning processes herein can be adjusted to
provide on the order of at least one part per hundred million of
the benefit agent MRL species in the aqueous washing medium, and
may provide from about 0.005 ppm to about 25 ppm, from about 0.05
ppm to about 10 ppm, or even from about 0.1 ppm to about 5 ppm, of
the MRL in the wash liquor.
[0133] Preferred transition-metals in the instant transition-metal
bleach catalyst include manganese, iron and chromium. Preferred
MRL's herein are a special type of ultra-rigid ligand that is
cross-bridged such as
5,12-diethyl-1,5,8,12-tetraazabicyclo[6.6.2]hexa-decane.
[0134] Suitable transition metal MRLs are readily prepared by known
procedures, such as taught for example in WO 00/32601, and U.S.
Pat. No. 6,225,464.
Processes of Making Compositions
[0135] The compositions of the present invention can be formulated
into any suitable form and prepared by any process chosen by the
formulator, non-limiting examples of which are described in U.S.
Pat. No. 5,879,584; U.S. Pat. No. 5,691,297; U.S. Pat. No.
5,574,005; U.S. Pat. No. 5,569,645; U.S. Pat. No. 5,565,422; U.S.
Pat. No. 5,516,448; U.S. Pat. No. 5,489,392; U.S. Pat. No.
5,486,303 all of which are incorporated herein by reference.
Method of Use
[0136] Compositions containing the benefit agent delivery particle
disclosed herein can be used to clean or treat a situs inter alia a
surface or fabric. Typically at least a portion of the situs is
contacted with an embodiment of Applicants' composition, in neat
form or diluted in a liquor, for example, a wash liquor and then
the situs may be optionally washed and/or rinsed. In one aspect, a
situs is optionally washed and/or rinsed, contacted with a particle
according to the present invention or composition comprising said
particle and then optionally washed and/or rinsed. For purposes of
the present invention, washing includes but is not limited to,
scrubbing, and mechanical agitation. The fabric may comprise most
any fabric capable of being laundered or treated in normal consumer
use conditions. Liquors that may comprise the disclosed
compositions may have a pH of from about 3 to about 11.5. Such
compositions are typically employed at concentrations of from about
500 ppm to about 15,000 ppm in solution. When the wash solvent is
water, the water temperature typically ranges from about 5.degree.
C. to about 90.degree. C. and, when the situs comprises a fabric,
the water to fabric ratio is typically from about 1:1 to about
30:1.
Test Methods
[0137] It is understood that the test methods that are disclosed in
the Test Methods Section of the present application should be used
to determine the respective values of the parameters of Applicants'
invention as such invention is described and claimed herein.
[0138] (1) Fracture Strength [0139] a.) Place 1 gram of particles
in 1 liter of distilled deionized (DI) water. [0140] b.) Permit the
particles to remain in the DI water for 10 minutes and then recover
the particles by filtration, using a 60 mL syringe filter, 1.2
micron nitrocellulose filter (Millipore, 25 mm diameter). [0141]
c.) Determine the rupture force of 50 individual particles. The
rupture force of a particle is determined using the procedure given
in Zhang, Z.; Sun, G; "Mechanical Properties of
Melamine-Formaldehyde microcapsules," J. Microencapsulation, vol
18, no. 5, pages 593-602, 2001. Then calculate the fracture
strength of each particle by dividing the rupture force (in
Newtons) by the cross-sectional area of the respective spherical
particle (.pi.r.sup.2, where r is the radius of the particle before
compression), said cross-sectional area being determined as
follows: measuring the particle size of each individual particle
using the experimental apparatus and method of Zhang, Z.; Sun, G;
"Mechanical Properties of Melamine-Formaldehyde microcapsules," J.
Microencapsulation, vol 18, no. 5, pages 593-602, 2001. [0142] d.)
Use the 50 independent measurements from c.) above, and calculate
the percentage of particles having a fracture strength within the
claimed range fracture strength range.
[0143] (2) ClogP [0144] The "calculated logP" (ClogP) is determined
by the fragment approach of Hansch and Leo (cf., A. Leo, in
Comprehensive Medicinal Chemistry, Vol. 4, C. Hansch, P. G.
Sammens, J. B. Taylor, and C. A. Ramsden, Eds. P. 295, Pergamon
Press, 1990, incorporated herein by reference). ClogP values may be
calculated by using the "CLOGP" program available from Daylight
Chemical Information Systems Inc. of Irvine, Calif. U.S.A.
[0145] (3) Boiling Point [0146] Boiling point is measured by ASTM
method D2887-04a, "Standard Test Method for Boiling Range
Distribution of Petroleum Fractions by Gas Chromatography," ASTM
International.
[0147] (4) Odor Detection Threshold (ODT) [0148] Odour detection
threshold is determined using the protocol found in U.S. Pat. No.
6,869,923 B1, from Column 3, line 39 through Column 4, line 15.
[0149] (5) Particle Size [0150] a.) Place 1 gram of particles in 1
liter of distilled deionized (DI) water. [0151] b.) Permit the
particles to remain in the DI water for 10 minutes and then recover
the particles by filtration, using a 60 mL syringe filter, 1.2
micron nitrocellulose filter (Millipore, 25 mm diameter). [0152]
c.) Determine the particle size of 50 individual particles using
the experimental apparatus and method of Zhang, Z.; Sun, G;
"Mechanical Properties of Melamine-Formaldehyde microcapsules," J.
Microencapsulation, vol 18, no. 5, pages 593-602, 2001. [0153] d.)
Use the 50 independent measurements from c.) above, and calculate
the percentage of particles having a particle size within the
claimed range.
[0154] (6) Particle Wall Thickness [0155] All references to Leica
Microsystems refer to the Company with Corporate Headquarters
located at: [0156] Leica Microsystems GmbH [0157]
Ernst-Leitz-Strasse 17-37 [0158] 35578 Wetzlar [0159] All
references to Drummond refer to the Company located at: [0160]
Drummond Scientific Company [0161] 500 Parkway, Box 700 [0162]
Broomall, Pa. 19008 [0163] All references to Hitachi refer to the
Company with Corporate Headquarters located at: [0164] Hitachi High
Technologies [0165] 24-14, Nishi-Shimbashi 1-chome, Minato-ku,
[0166] Tokyo 105-8717, Japan [0167] All references to Gatan refer
to the Company with Corporate Headquarters located at: [0168]
Gatan, Inc. [0169] 5933 Coronado Lane [0170] Pleasanton, Calif.
94588 [0171] All references to Quartz refer to the Company with
offices located at: [0172] Quartz Imaging Corporation [0173]
Technology Enterprise Facility III [0174] 6190 Agronomy Rd, Suite
406 [0175] Vancouver, B.C. Canada V6T 1Z3 [0176] Materials: [0177]
Methylcyclohexane--Alfa Aesar Catalogue Number A16057 or equivalent
[0178] Capillary Pipettes--Drummond Catalogue Number 5-000-1005 or
equivalent [0179] Flat Specimen Carrier--Leica Microsystems P/N
706897 or equivalent [0180] Copper Washers--Leica Microsystems P/N
706867 or equivalent [0181] Flat Specimen Pod--Leica Microsystems
P/N 706839 or equivalent [0182] Loading Device for Flat Specimen
Holder--Leica Microsystems P/N 706832 or equivalent [0183] Torque
Wrench--Leica Microsystems P/N 870071 or equivalent [0184] Allen
Bit, 2 mm--Leica Microsystems P/N 870072 or equivalent [0185]
Forceps--Leica Microsystems P/N 840105 or equivalent [0186] Gatan
Planchette Collet--Gatan P/N PEP5099 [0187] Gatan Planchette
Specimen Holder--Gatan P/N PEP1395 [0188] Instruments: [0189]
Scanning Electron Microscope--Hitachi Model S-5200 SEM/STEM or
equivalent [0190] High Pressure Freezer--Leica Microsystems Model
706802 EM Pact or equivalent [0191] Cryotransfer Device--Gatan
Model CT3500 or equivalent [0192] Cryotransfer System--Gatan Model
CT2500 or equivalent [0193] Gatan ITC Temperature Controller--Gatan
Model ITC502 or equivalent [0194] Image Analysis Software--Quartz
PCI Version 5 or equivalent [0195] Sample: Obtain the sample of
microcapsules as per the procedure of 1 above entitled "Fracture
Strength". 50 samples are required.
[0196] Test Procedure [0197] 1) Turn on the Leica Microsystems High
Pressure Freezer (Leica Microsystems Model Number 706802). [0198]
2) Fill up the methylcyclohexane container on the High Pressure
Freezer with methylcyclohexane (Alfa Aesar Cat. # A16057 or
equivalent). [0199] 3) Fill up the liquid nitrogen dewar on the
High Pressure Freezer. [0200] 4) Fill the liquid nitrogen bath on
the High Pressure Freezer [0201] 5) The display on the High
Pressure Freezer will show Load Sample on the front panel when the
instrument is ready to use. [0202] 6) Start the Hitachi Model
S-5200 SEM/STEM and set the Accelerating Voltage to 3.0 KV and the
Emission Current to 20 .mu.A. [0203] 7) Fill the Anti-contaminator
Dewar located on the lower right side of the Hitachi Model S-5200
SEM/STEM microscope column with liquid nitrogen. [0204] 8) Fill the
liquid nitrogen dewar on the Gatan Alto 2500 Cryotransfer System
(Gatan Model CT2500). Replenish the liquid nitrogen until the dewar
remains full. The device is ready to use when the prepchamber
temperature reads below -190.degree. C. [0205] 9) Place a copper
washer (Leica Microsystems P/N 706867) on top of the flat specimen
carrier such that the hole in the washer aligns with the well in
the flat specimen carrier. [0206] 10) Take a glass capillary
pipette (Drummond P/N 5-000-1005 or similar) and insert the
provided wire plunger into one end of the pipette [0207] 11) Insert
the pipette into the microcapsule dispersion and withdraw the
plunger part way to pull a few microliters of the dispersion into
the pipette. [0208] 12) Place the tip of the pipette in the well in
the flat specimen carrier and push the plunger into the pipette to
dispense a small amount of liquid until the well is just slightly
overfilled. [0209] 13) Insert a 2 mm Allen key bit (Leica
Microsystems P/N 870072) into the torque wrench (Leica Microsystems
P/N 870071). [0210] 14) Using the torque wrench with the bit,
loosen the Diamond Locking Screw in the Flat Specimen Pod (Leica
Microsystems P/N 706839). [0211] 15) Place the Flat Specimen Holder
and Copper Washer into the Flat Specimen Pod. [0212] 16) Use the
torque wrench with the 2 mm Allen key bit to tighten the Diamond
Locking Screw in the Flat Specimen Pod onto the specimen until the
torque wrench clicks twice. [0213] 17) Attach the Loading Device
for the Flat Specimen Holder (Leica Microsystems P/N 706832) to the
Flat Specimen Pod by screwing it onto the exposed threads of the
Diamond Locking Screw. [0214] 18) Place the Loading Device for the
Flat Specimen Holder with the Flat Specimen Pod onto the EM Pact
High Pressure Freezer (Leica Microsystems P/N 706802) and insert it
into the High Pressure Freezer. [0215] 19) Freeze the specimen
using the High Pressure Freezer. [0216] 20) Transfer the Flat
Specimen Pod to the Unloading Station and unscrew the Loading
Device for the Flat Specimen Carrier being careful to keep it
immersed in the liquid nitrogen bath. [0217] 21) Using the torque
wrench, loosen the Diamond Locking Screw. [0218] 22) Using tweezers
with the tips cooled in liquid nitrogen until the liquid nitrogen
stops boiling, remove the Flat Specimen Carrier from the Flat
Specimen Pod and place it into a small container in the liquid
nitrogen bath. [0219] 23) Place the Gatan CT3500 Cryotransfer
Device (Gatan Model Number CT3500) into the Gatan Specimen
Workstation. [0220] 24) Fill the liquid nitrogen dewar on the Gatan
CT3500 Cryotransfer device and fill the dewar on the Gatan Specimen
Workstation replenishing the liquid nitrogen as necessary until
rapid boiling of the liquid nitrogen stops. [0221] 25) Transfer the
Flat Specimen Holder to the Gatan Specimen Workstation while
keeping it in a container of liquid nitrogen. [0222] 26) Using
tweezers cooled in liquid nitrogen until the liquid nitrogen stops
boiling, place the flat specimen holder into the Gatan Planchette
Collet (Gatan P/N PEP5099) and press down firmly. [0223] 27) Place
the assembly from step 26 into the Gatan Planchette Specimen Holder
(Gatan P/N PEP1395) and press down firmly. [0224] 28) Push the
Gatan Cryotransfer device back into the Gatan Specimen Workstation.
[0225] 29) Using the Gatan supplied 5 mm Friction Tool, screw the
Gatan Planchette Specimen Holder into the Gatan Cryotransfer
device. [0226] 30) Remove the Gatan Cryotransfer device from the
Gatan Specimen Workstation and insert it into the Gatan Alto 2500
Cryotransfer System. [0227] 31) Attach the Gatan ITC Temperature
Controller (Gatan Model Number ITC502) to the Gatan Cryotransfer
device by attaching the Temperature Measurement Lead from the Gatan
ITC controller to the connector on top of the Gatan Cryotransfer
device. [0228] 32) Using the Gatan ITC Controller, raise the
temperature of the specimen to -120.degree. C. [0229] 33) Using the
fracturing knife, break off the copper washer to fracture the
specimen. [0230] 34) Reduce the temperature of the specimen below
-160.degree. C. [0231] 35) With the voltage set to 6 KV and the gas
flow set to provide 10 mA sputter current, press the sputter button
and once the current displays 10 mA, let the coater run for 60-90
seconds coating the specimen with gold/palladium. [0232] 36) Close
the frost shield on the Gatan CT3500 Cryotransfer Device and
transfer the specimen to the Hitachi S-5200 SEM/STEM. [0233] 37)
Wait for the temperature of the Gatan CT3500 Cryotransfer device to
stabilize, typically between -170.degree. C. and -172.degree. C.
[0234] 38) Open the frost shield on the Gatan CT3500 Cryotransfer
device by turning the frost shield control knob counter-clockwise.
[0235] 39) Move the sample around using the stage control
trackball, locate a broken microcapsule and adjust the
magnification to 50,000 to 150,000.times.. [0236] 40) Adjust the
focus and stigmation controls to obtain the best image. [0237] 41)
Acquire an image of the cross-section of the capsule wall.
[0238] Calculations [0239] 1) Select the ruler tool in the Quartz
PCI software. [0240] 2) Move the cursor to one edge of the
microcapsule wall. [0241] 3) Click and hold the left mouse button
while dragging the mouse cursor to the opposite side of the capsule
wall keeping the drawn line perpendicular to the face of the
capsule wall to measure the wall thickness. [0242] 4) Use 50
independent measurements (1 measurement for each capsule) to
calculate the percentage of particles having a wall thickness in
the claimed range.
[0243] (7) Benefit Agent Leakage [0244] a.) Obtain 2, one gram
samples of benefit agent particle composition. [0245] b.) Add 1
gram (Sample 1) of particle composition to 99 grams of product
matrix that the particle will be employed in and with the second
sample immediately proceed to Step d below. [0246] c.) Age the
particle containing product matrix (Sample 1) of a.) above for 2
weeks at 35.degree. C. in a sealed, glass jar. [0247] d.) Recover
the particle composition's particles from the product matrix of c.)
(Sample 1 in product matrix) and from particle composition (Sample
2) above by filtration. [0248] e.) Treat each particle sample from
d.) above with a solvent that will extract all the benefit agent
from each samples' particles. [0249] f.) Inject the benefit agent
containing solvent from each sample from e.) above into a Gas
Chromatograph and integrate the peak areas to determine the total
quantity of benefit agent extracted from each sample. [0250] g.)
The benefit agent leakage is defined as:
[0250] Value from f.) above for Sample 2-Value from f.) above for
Sample 1.
EXAMPLES
[0251] While particular embodiments of the present invention have
been illustrated and described, it would be obvious to those
skilled in the art that various other changes and modifications can
be made without departing from the spirit and scope of the
invention. It is therefore intended to cover in the appended claims
all such changes and modifications that are within the scope of
this invention.
Example 1
84 wt % Core/16 wt % Wall Melamine Formaldehyde (MF) Capsule
[0252] 25 grams of butyl acrylate-acrylic acid copolymer emulsifier
(Colloid C351, 25% solids, pka 4.5-4.7, (Kemira Chemicals, Inc.
Kennesaw, Ga. U.S.A.) is dissolved and mixed in 200 grams deionized
water. The pH of the solution is adjusted to pH of 4.0 with sodium
hydroxide solution. 8 grams of partially methylated methylol
melamine resin (Cymel 385, 80% solids, (Cytec Industries West
Paterson, N.J., U.S.A.)) is added to the emulsifier solution. 200
grams of perfume oil is added to the previous mixture under
mechanical agitation and the temperature is raised to 50.degree. C.
After mixing at higher speed until a stable emulsion is obtained,
the second solution and 4 grams of sodium sulfate salt are added to
the emulsion. This second solution contains 10 grams of butyl
acrylate-acrylic acid copolymer emulsifier (Colloid C351, 25%
solids, pka 4.5-4.7, Kemira), 120 grams of distilled water, sodium
hydroxide solution to adjust pH to 4.8, 25 grams of partially
methylated methylol melamine resin (Cymel 385, 80% solids, Cytec).
This mixture is heated to 70.degree. C. and maintained overnight
with continuous stifling to complete the encapsulation process. 23
grams of acetoacetamide (Sigma-Aldrich, Saint Louis, Mo., U.S.A.)
is added to the suspension. An average capsule size of 30 um is
obtained as analyzed by a Model 780 Accusizer.
Example 2
80 wt % Core/20 wt % Wall Melamine Formaldehyde Capsule
[0253] 18 grams of a blend of 50% butyl acrylate-acrylic acid
copolymer emulsifier (Colloid C351, 25% solids, pka 4.5-4.7,
Kemira) and 50% polyacrylic acid (35% solids, pKa 1.5-2.5, Aldrich)
is dissolved and mixed in 200 grams deionized water. The pH of the
solution is adjusted to pH of 3.5 with sodium hydroxide solution.
6.5 grams of partially methylated methylol melamine resin (Cymel
385, 80% solids Cytec) is added to the emulsifier solution. 200
grams of perfume oil is added to the previous mixture under
mechanical agitation and the temperature is raised to 60.degree. C.
After mixing at higher speed until a stable emulsion is obtained,
the second solution and 3.5 grams of sodium sulfate salt are poured
into the emulsion. This second solution contains 10 grams of butyl
acrylate-acrylic acid copolymer emulsifier (Colloid C351, 25%
solids, pka 4.5-4.7, Kemira), 120 grams of distilled water, sodium
hydroxide solution to adjust pH to 4.6, 30 grams of partially
methylated methylol melamine resin (Cymel 385, 80% Cytec). This
mixture is heated to 75.degree. C. and maintained 6 hours with
continuous stirring to complete the encapsulation process. 23 grams
of acetoacetamide (Sigma-Aldrich, Saint Louis, Mo., U.S.A.) is
added to the suspension.
Example 3
80 wt % Core/20 wt % Melamine Formaldehyde Wall Capsule
[0254] 36 grams of butyl acrylate-acrylic acid copolymer emulsifier
(Colloid C351, 25% solids, pKa 4.5-4.7, Kemira) is dissolved and
mixed in 200 grams deionized water. The pH of the solution is
adjusted to pH of 5.0 with sodium hydroxide solution. 12 grams of
partially methylated methylol melamine resin (Cymel 385, 80%
solids, Cytec) is added to the emulsifier solution. 200 grams of
perfume oil is added to the previous mixture under mechanical
agitation and the temperature is raised to 65.degree. C. After
mixing at higher speed until a stable emulsion is obtained, the
second solution and 5 grams of sodium sulfate salt are added to the
emulsion. This second solution contains 12 grams of butyl
acrylate-acrylic acid copolymer emulsifier (Colloid C351, 25%
solids, pKa 4.5-4.7, Kemira), 120 grams of distilled water, sodium
hydroxide solution to adjust pH to 5, 33 grams of partially
methylated methylol melamine resin (Cymel 385, 80% solids, Cytec).
This mixture is heated to 65.degree. C. and maintained overnight
with continuous stirring to complete the encapsulation process. 23
grams of acetoacetamide (Sigma-Aldrich, Saint Louis, Mo., U.S.A.)
is added to the suspension.
Example 4
80 wt % Core/20 wt % Wall Melamine Formaldehyde Capsule
[0255] 20 grams of butyl acrylate-acrylic acid copolymer emulsifier
(Colloid C351, 25% solids, pKa 4.5-4.7, Kemira) is dissolved and
mixed in 200 grams deionized water. The pH of the solution is
adjusted to pH of 5.5 with sodium hydroxide solution. 6 grams of
partially methylated methylol melamine resin (Cymel 385, 80%
solids, Cytec) is added to the emulsifier solution. 200 grams of
perfume oil is added to the previous mixture under mechanical
agitation and the temperature is raised to 55.degree. C. After
mixing at higher speed until a stable emulsion is obtained, the
second solution and 9 grams of sodium sulfate salt is added to the
emulsion. This second solution contains 8 grams of polyacrylic acid
(35% solids, pka 1.5-2.5, Aldrich), 120 grams of distilled water,
sodium hydroxide solution to adjust pH to 4.4, 35 grams of
partially methylated methylol melamine resin (Cymel 385, 80%
solids, Cytec). This mixture is heated to 80.degree. C. and
maintained 4 hours with continuous stifling to complete the
encapsulation process. 23 grams of acetoacetamide (Sigma-Aldrich,
Saint Louis, Mo., U.S.A.) is added to the suspension.
Example 5
Melamine Formaldehyde Capsule
[0256] The composition of and the procedures for preparing the
capsules are the same composition as in Example 4 except for the
following: the melamine formaldehyde resin is a mix of 80%
partially methylated methylol melamine resin and 20% of fully
methylated melamine resin.
Example 6
Melamine Formaldehyde Capsule
[0257] The procedure for preparing the capsules is the same as in
Example 4, except for the following compositional changes to the
perfume emulsification liquor (the first solution):
TABLE-US-00001 Material A B C D E F G Copolymer of 42 31 0 20 26 18
0 Polyacrylic Acid- Butyl Acrylate Polyacrylic Acid 0 21 29 14 0 22
27 20% NaOH 2 3 6 9 2 7 7 Melamine Resin 19 21 21 8 4 7 17 Perfume
Oil 265 290 246 224 220 200 204 Water 95 104 103 225 159 189
237
[0258] The procedure for preparing the capsules is the same as in
Example 4, except for the following compositional changes to the
second solution:
TABLE-US-00002 Material A B C D E F G Copolymer of 11 0 15 0 0 3 3
Polyacrylic Acid- Butyl Acrylate Polyacrylic Acid 11 12 0 4 9 8 10
20% NaOH 0.4 0.4 0.1 0.3 0.4 0.4 0.4 Melamine Resin 8 4 16 13 26 23
29 Water 115 126 43 147 52 47 78
[0259] Followed by the addition of acetoacetamide at a level of 5
wt % of the weight of the batch.
Example 7
Melamine Formaldehyde Capsule
[0260] The composition of and the procedures for preparing the
capsules are the same composition as in Example 4 except for the
following: 0.7% of ammonium hydroxide is added to the suspension
instead of acetoacetamide.
Example 8
Production of Spray Dried Microcapsule
[0261] 1200 g of perfume microcapsule slurry, containing one or
more of the variants of microcapsules disclosed in the present
specification, is mixed together with 700 g of water for 10 minutes
using an IKA Eurostar mixer with R1382 attachment at a speed of 180
rpm. The mixture is then transferred over to a feeding vessel to be
spray dried in a 1.2 m diameter Niro Production Minor. The slurry
is fed into the tower using a Watson-Marlow 504U peristaltic pump
and atomised using a 100 mm diameter rotary atomiser run at 18000
rpm, with co-current air flow for drying. The slurry is dried using
an inlet temperature of 200.degree. C. and outlet temperature of
95.degree. C. to form a fine powder. The equipment used the spray
drying process may be obtained from the following suppliers: IKA
Werke GmbH & Co. KG, Janke and Kunkel--Str. 10, D79219 Staufen,
Germany; Niro A/S Gladsaxevej 305, P.O. Box 45, 2860 Soeborg,
Denmark and Watson-Marlow Bredel Pumps Limited, Falmouth, Cornwall,
TR11 4RU, England.
Example 9
[0262] Non-limiting examples of product formulations containing
microcapsules summarized in the following table.
TABLE-US-00003 EXAMPLES (% wt) A B C D E F G H I J FSA.sup.a 14
16.47 14 12 12 16.47 -- -- 5 5 FSA.sup.b -- 3.00 -- -- -- FSA.sup.c
-- -- 6.5 -- -- Ethanol 2.18 2.57 2.18 1.95 1.95 2.57 -- -- 0.81
0.81 Isopropyl -- -- -- -- -- -- 0.33 1.22 -- -- Alcohol
Starch.sup.d 1.25 1.47 2.00 1.25 -- 2.30 0.5 0.70 0.71 0.42
Microcapsule 0.6 0.75 0.6 0.75 0.37 0.60 0.37 0.6 0.37 0.37 (%
active)* Formaldehyde 0.40 0.13 0.065 0.25 0.03 0.030 0.030 0.065
0.03 0.03 Scavenger.sup.e Phase 0.21 0.25 0.21 0.21 0.14 -- -- 0.14
-- -- Stabilizing Polymer.sup.f Suds -- -- -- -- -- -- -- 0.1 -- --
Suppressor.sup.g Calcium 0.15 0.176 0.15 0.15 0.30 0.176 --
0.1-0.15 -- -- Chloride DTPA.sup.h 0.017 0.017 0.017 0.017 0.007
0.007 0.20 -- 0.002 0.002 Preservative 5 5 5 5 5 5 -- 250.sup.j 5 5
(ppm).sup.i,j Antifoam.sup.k 0.015 0.018 0.015 0.015 0.015 0.015 --
-- 0.015 0.015 Dye 40 40 40 40 40 40 11 30-300 30 30 (ppm) Ammonium
0.100 0.118 0.100 0.100 0.115 0.115 -- -- -- -- Chloride HCl 0.012
0.014 0.012 0.012 0.028 0.028 0.016 0.025 0.011 0.011
Structurant.sup.l 0.01 0.01 0.01 0.01 0.01 0.01 0.01 0.01 0.01 0.01
Neat 0.8 0.7 0.9 0.5 1.2 0.5 1.1 0.6 1.0 0.9 Unencapsulated Perfume
Deionized .dagger. .dagger. .dagger. .dagger. .dagger. .dagger.
.dagger. .dagger. .dagger. .dagger. Water
.sup.aN,N-di(tallowoyloxyethyl)-N,N-dimethylammonium chloride.
.sup.bMethyl bis(tallow amidoethyl)2-hydroxyethyl ammonium methyl
sulfate. .sup.cReaction product of Fatty acid with
Methyldiethanolamine in a molar ratio 1.5:1, quaternized with
Methylchloride, resulting in a 1:1 molar mixture of
N,N-bis(stearoyl-oxy-ethyl) N,N-dimethyl ammonium chloride and
N-(stearoyl-oxy-ethyl) N,-hydroxyethyl N,N dimethyl ammonium
chloride. .sup.dCationic high amylose maize starch available from
National Starch under the trade name CATO .RTM.. .sup.eThe
formaldehyde scavenger is acetoacetamide available from Aldrich.
.sup.fCopolymer of ethylene oxide and terephthalate having the
formula described in U.S. Pat. No. 5,574,179 at col.15, lines 1-5,
wherein each X is methyl, each n is 40, u is 4, each R1 is
essentially 1,4-phenylene moieties, each R2 is essentially
ethylene, 1,2-propylene moieties, or mixtures thereof. .sup.gSE39
from Wacker .sup.hDiethylenetriaminepentaacetic acid. .sup.iKATHON
.RTM. CG available from Rohm and Haas Co. "PPM" is "parts per
million." .sup.jGluteraldehyde .sup.kSilicone antifoam agent
available from Dow Corning Corp. under the trade name DC2310.
.sup.lHydrophobically-modified ethoxylated urethane available from
Rohm and Haas under the tradename Aculan 44. *Suitable combinations
of the microcapsules provided in Examples 1 through 8. (Percent
active relates to the core content of the microcapsule.) .dagger.
balance
Example 10
Microcapsules in Dry Laundry Formulations
TABLE-US-00004 [0263] % w/w granular laundry detergent composition
Component A B C D E F G Brightener 0.1 0.1 0.1 0.2 0.1 0.2 0.1 Soap
0.6 0.6 0.6 0.6 0.6 0.6 0.6 Ethylenediamine disuccinic acid 0.1 0.1
0.1 0.1 0.1 0.1 0.1 Acrylate/maleate copolymer 1.5 1.5 1.5 1.5 1.5
1.5 1.5 Hydroxyethane di(methylene 0.4 0.4 0.4 0.4 0.4 0.4 0.4
phosphonic acid) Mono-C.sub.12-14 alkyl, di-methyl, 0.5 0.5 0.5 0.5
0.5 0.5 0.5 mono-hydroyethyl quaternary ammonium chloride Linear
alkyl benzene 0.1 0.1 0.2 0.1 0.1 0.2 0.1 Linear alkyl benzene
sulphonate 10.3 10.1 19.9 14.7 10.3 17 10.5 Magnesium sulphate 0.4
0.4 0.4 0.4 0.4 0.4 0.4 Sodium carbonate 19.5 19.2 10.1 18.5 29.9
10.1 16.8 Sodium sulphate 29.6 29.8 38.8 15.1 24.4 19.7 19.1 Sodium
Chloride 0.1 0.1 0.1 0.1 0.1 0.1 0.1 Zeolite 9.6 9.4 8.1 18 10 13.2
17.3 Photobleach particle 0.1 0.1 0.2 0.1 0.2 0.1 0.2 Blue and red
carbonate speckles 1.8 1.8 1.8 1.8 1.8 1.8 1.8 Ethoxylated Alcohol
AE7 1 1 1 1 1 1 1 Tetraacetyl ethylene diamine 0.9 0.9 0.9 0.9 0.9
0.9 0.9 agglomerate (92 wt % active) Citric acid 1.4 1.4 1.4 1.4
1.4 1.4 1.4 PDMS/clay agglomerates (9.5% 10.5 10.3 5 15 5.1 7.3
10.2 wt % active PDMS) Polyethylene oxide 0.2 0.2 0.2 0.2 0.2 0.2
0.2 Enzymes e.g. Protease (84 mg/g 0.2 0.3 0.2 0.1 0.2 0.1 0.2
active), Amylase (22 mg/g active) Suds suppressor agglomerate 0.2
0.2 0.2 0.2 0.2 0.2 0.2 (12.4 wt % active) Sodium percarbonate
(having 7.2 7.1 4.9 5.4 6.9 19.3 13.1 from 12% to 15% active AvOx)
Perfume oil 0.5 0.5 0.5 0.5 0.5 0.5 0.5 Solid perfume particles 0.4
0 0.4 0.4 0.4 0.4 0.6 Perfume microcapsules* 1.3 2.4 1 1.3 1.3 1.3
0.7 Water 1.4 1.4 1.4 1.4 1.4 1.4 1.4 Misc 0.1 0.1 0.1 0.1 0.1 0.1
0.1 Total Parts 100 100 100 100 100 100 100 *Microcapsule added as
35% active slurry. Core/wall ratio can range from 80/20 up to 90/10
and average particle diameter can range from 5 .mu.m to 50
.mu.m
Example 11
Liquid Laundry Formulations (HDLs)
TABLE-US-00005 [0264] Ingredient HDL 1 HDL 2 HDL3 HDL4 HDL 5 HDL 6
Alkyl Ether Sulphate 0.00 0.50 12.0 12.0 6.0 7.0 Dodecyl Benzene
8.0 8.0 1.0 1.0 2.0 3.0 Sulphonic Acid Ethoxylated Alcohol 8.0 6.0
5.0 7.0 5.0 3.0 Citric Acid 5.0 3.0 3.0 5.0 2.0 3.0 Fatty Acid 3.0
5.0 5.0 3.0 6.0 5.0 Ethoxysulfated 1.9 1.2 1.5 2.0 1.0 1.0
hexamethylene diamine quaternized Diethylene triamine penta 0.3 0.2
0.2 0.3 0.1 0.2 methylene phosphonic acid Enzymes 1.20 0.80 0 1.2 0
0.8 Brightener (disulphonated 0.14 0.09 0 0.14 0.01 0.09 diamino
stilbene based FWA) Cationic hydroxyethyl 0 0 0.10 0 0.200 0.30
cellulose Poly(acrylamide-co- 0 0 0 0.50 0.10 0
diallyldimethylammonium chloride) Hydrogenated Castor Oil 0.50 0.44
0.2 0.2 0.3 0.3 Structurant Boric acid 2.4 1.5 1.0 2.4 1.0 1.5
Ethanol 0.50 1.0 2.0 2.0 1.0 1.0 1,2 propanediol 2.0 3.0 1.0 1.0
0.01 0.01 Glutaraldehyde 0 0 19 ppm 0 13 ppm 0 Diethyleneglycol
(DEG) 1.6 0 0 0 0 0 2,3-Methyl-1,3- 1.0 1.0 0 0 0 0 propanediol (M
pdiol) Mono Ethanol Amine 1.0 0.5 0 0 0 0 NaOH Sufficient To pH 8
pH 8 pH 8 pH 8 pH 8 pH 8 Provide Formulation pH of: Sodium Cumene
2.00 0 0 0 0 0 Sulphonate (NaCS) Silicone (PDMS) emulsion 0.003
0.003 0.003 0.003 0.003 0.003 Perfume 0.7 0.5 0.8 0.8 0.6 0.6
Polyethyleneimine 0.01 0.10 0.00 0.10 0.20 0.05 Perfume
Microcapsules* 1.00 5.00 1.00 2.00 0.10 0.80 Water Balance Balance
Balance Balance Balance Balance to 100% to 100% to 100% to 100% to
100% to 100% *Perfume Microcapsules Slurry in accordance with the
teaching of the present specification.
Example 12
Urea Formaldehyde Capsule
[0265] Into a mixture of 89.5 grams of water, 5 grams of urea, 0.5
gram of resorcinol and 5 grams of an alkyl acrylate-acrylic acid
copolymer, adjusted to pH 4.0, were emulsified 90 grams of perfume
oil. These mixtures were emulsified and the resulting mixture is
placed in a container which is mounted in a room temperature water
bath, continuous stirring is provided, 13.5 grams of 37%
formaldehyde solution were added and the bath is heated to
55.degree. C. and maintained at that temperature overnight to
initiate and complete encapsulation.
Example 13
[0266] The perfume microcapsules of Examples 1-7 are tested in
accordance with the test methods of the present invention are found
to have a fracture strengths of from about 0.2 MPa to about 10 MPa,
from about 0.4 MPa to about 5 MPa, from about 0.6 MPa to about 3.5
MPa, and even from about 0.7 MPa to about 3 MPa; a benefit agent
leakage of from 0% to about 30%, from 0% to about 20%, and even
from 0% to about 5%; a particle size of from about 1 microns to
about 80 microns, about 5 microns to 60 microns, from about 10
microns to about 50 microns, and even from about 15 microns to
about 40 microns; and a particle wall thickness of from about 60 nm
to about 250 nm, from about 80 nm to about 180 nm, or even from
about 100 nm to about 160 nm.
Example 12
TABLE-US-00006 [0267] Examples of liquid detergents A B C D C14-C15
alkyl poly ethoxylate (8) 6.25 4.00 6.25 6.25 C12-C14 alkyl poly
ethoxylate (7) 0.40 0.30 0.40 0.40 C12-C14 alkyl poly ethoxylate
(3) 10.60 6.78 10.60 10.60 sulfate Na salt Linear Alkylbenzene
sulfonate acid 0.19 1.16 0.79 0.79 Citric Acid 3.75 2.40 3.75 3.75
C12-C18 Fatty Acid 4.00 2.56 7.02 7.02 Enzymes 0.60 0.4 0.60 0.60
Boric Acid 2.4 1.5 1.25 1.25 Trans-sulphated ethoxylated 1.11 0.71
1.11 1.11 hexamethylene diamine quat Diethylene triamine penta 0.17
0.11 0.17 0.17 methylene phosphonic acid Fluorescent brightener
0.09 0.06 0.14 0.14 Hydrogenated Castor Oil 0.05 0.300 0.20 0.20
Ethanol 2.50 1.00 2.50 2.50 1,2 propanediol 1.14 0.7 1.14 1.14
Sodium hydroxide 3.8 2.6 4.60 4.60 Mono Ethanol Amine 0.8 0.5 Na
Cumene Sulphonate Silicone emulsion 0.0030 0.0030 0.0030 0.0030 Dye
0.002 0.002 0.002 0.002 Opacifier (Styrene Acrylate based)
Bentonite Softening Clay Acrylamide/MAPTAC (ex Nalco 0.40 0.40
Chemicals of Naperville, IL) Mirapol 550 (ex Rhodia Chemie, France)
Polyquaternium 10 - Cationic hydroxyl ethyl cellulose PP-5495
(silicone ex Dow Corning Corporation, Midland, MI) DC 1664
(silicone ex Dow Corning Corporation, Midland, MI) Pearlescent
agent * 0.2 Perfume micro capsules 0.8 0.5 1.0 0.7 (expressed as
perfume oil) Perfume 0.7 0.55 1.00 1.00 Poly Ethylene Imine MW
25000 Water Up Up Up Up to 100 to 100 to 100 to 100 * Mica-TiO2
(Prestige Silk Silver Star ex Eckart) or BiOCl (Biron Silver CO -
Merck) or pre-crystallized EGDS (Tegopearl N 100 ex Degussa,
expressed as pure EGDS)
TABLE-US-00007 Examples of liquid detergents E F G H C14-C15 alkyl
poly ethoxylate (8) 6.25 4.00 6.25 6.25 C12-C14 alkyl poly
ethoxylate (7) 0.40 0.30 0.40 C12-C14 alkyl poly ethoxylate (3)
10.60 6.78 10.60 10.60 sulfate Na salt Linear Alkylbenzene
sulfonate acid 0.79 1.19 0.79 0.79 Citric Acid 3.75 2.40 3.75 3.75
C12-C18 Fatty Acid 7.02 4.48 7.02 7.02 Enzymes 0.60 1.0 0.60 Boric
Acid 1.25 1.25 1.25 1.25 Trans-sulphated ethoxylated 1.11 0.71 1.11
1.11 hexamethylene diamine quat Diethylene triamine penta 0.17 0.11
0.17 0.17 methylene phosphonic acid Fluorescent brightener 0.14
0.06 0.14 Hydrogenated Castor Oil 0.20 0.300 0.20 0.20 Ethanol 2.50
1.00 2.50 2.50 1,2 propanediol 1.14 0.09 1.14 1.14 Sodium hydroxide
4.60 3.01 4.60 4.60 Mono Ethanol Amine Na Cumene Sulphonate
Silicone emulsion 0.0030 0.0030 0.0030 0.0030 Dye 0.002 0.00084
0.00084 0.00084 Opacifier (Styrene Acrylate based) 0.1 Bentonite
Softening Clay Acrylamide/MAPTAC (ex Nalco 0.40 Chemicals of
Naperville, IL) Mirapol 550 0.40 0.25 (ex Rhodia Chemie, France)
Polyquaternium 10 - Cationic 0.30 hydroxyl ethyl cellulose PP-5495
(silicone ex Dow Corning 3.0 Corporation, Midland, MI) DC 1664
(silicone ex Dow Corning 3.0 3.0 Corporation, Midland, MI)
Pearlescent agent * 0.2 Perfume micro capsules 0.9 0.3 0.5 1.2
(expressed as perfume oil) Perfume 1.00 .65 1.00 1.00 Poly Ethylene
Imine MW 25000 Water Up Up Up Up to 100 to 100 to 100 to 100
TABLE-US-00008 Examples of liquid detergents I J K C14-C15 alkyl
poly ethoxylate (8) 4.00 6.1 C12-C14 alkyl poly ethoxylate (7) 2.00
C12-C14 alkyl poly ethoxylate (3) 6.78 sulfate Na salt Linear
Alkylbenzene sulfonate acid 1.19 7.8 15.0 Citric Acid 2.40 2.6 2.50
C12-C18 Fatty Acid 4.48 2.6 11.4 Enzymes .55 .07 Boric Acid 1.25
1.50 1.3 Trans-sulphated ethoxylated 0.71 1.20 hexamethylene
diamine quat Diethylene triamine penta 0.11 0.20 0.7 methylene
phosphonic acid Fluorescent brightener 0.09 0.14 Hydrogenated
Castor Oil 0.300 0.45 0.09 Ethanol 1.00 1.40 0.7 1,2 propanediol
0.09 3.30 6.7 Sodium hydroxide 3.01 3.00 5.5 Mono Ethanol Amine
0.50 Na Cumene Sulphonate 1.6 Silicone emulsion 0.0030 0.0030 0.30
Dye 0.00084 0.02 0.004 Opacifier (Styrene Acrylate based) Bentonite
Softening Clay 3.40 Acrylamide/MAPTAC (ex Nalco Chemicals of
Naperville, IL) Mirapol 550 (ex Rhodia Chemie, France)
Polyquaternium 10 - Cationic 0.18 hydroxyl ethyl cellulose PP-5495
(silicone ex Dow Corning Corporation, Midland, MI) DC 1664
(silicone ex Dow Corning 3.0 Corporation, Midland, MI) Pearlescent
agent * 0.2 Perfume micro capsules 0.2 0.45 0.75 (expressed as
perfume oil) Perfume 0.65 0.5 1.0 Poly Ethylene Imine MW 25000 0.08
Water Up Up Up to 100 to 100 to 100
TABLE-US-00009 Examples of liquid detergents L M ** N C14-C15 alkyl
poly ethoxylate (8) 3.7 20.7 C12-C14 alkyl poly ethoxylate (7) 16.7
C12-C14 alkyl poly ethoxylate (3) 17.8 5.5 sulfate Na salt Linear
Alkylbenzene sulfonate acid 12.5 22.9 13.5 Citric Acid 3.9 1.7
C12-C18 Fatty Acid 11.1 18 5.1 Enzymes 3 1.2 3 Boric Acid 0.5 0.5
Trans-sulphated ethoxylated 3.25 1.2 hexamethylene diamine quat PEI
600 EO20 1.25 1.2 Diethylene triamine penta 1.6 0.85 methylene
phosphonic acid or HEDP Fluorescent brightener 0.2 0.3 0.14
Hydrogenated Castor Oil 0.2 1,2 propanediol 4.3 20.3 11.7 Sodium
hydroxide 1.0 3.9 Mono Ethanol Amine 9.8 6.8 3.1 Dye Present
Present Present PDMS 2.15 Potassium sulphite 0.2 Perfume micro
capsules 1.6 1.5 1.4 (expressed as perfume oil) Perfume 1.2 1.6 1.0
Form. Phenyl Boronic Acid Present Water Up Up Up to 100 to 100 to
100 ** Low water liquid detergent in Polyvinyl alcohol
unidose/sachet
[0268] The dimensions and values disclosed herein are not to be
understood as being strictly limited to the exact numerical values
recited. Instead, unless otherwise specified, each such dimension
is intended to mean both the recited value and a functionally
equivalent range surrounding that value. For example, a dimension
disclosed as "40 mm" is intended to mean "about 40 mm".
[0269] All documents cited in the Detailed Description of the
Invention are, in relevant part, incorporated herein by reference;
the citation of any document is not to be construed as an admission
that it is prior art with respect to the present invention. To the
extent that any meaning or definition of a term in this document
conflicts with any meaning or definition of the same term in a
document incorporated by reference, the meaning or definition
assigned to that term in this document shall govern.
[0270] While particular embodiments of the present invention have
been illustrated and described, it would be obvious to those
skilled in the art that various other changes and modifications can
be made without departing from the spirit and scope of the
invention. It is therefore intended to cover in the appended claims
all such changes and modifications that are within the scope of
this invention.
* * * * *