U.S. patent application number 10/548775 was filed with the patent office on 2006-07-27 for controlled release compositions.
Invention is credited to Sylvie Bouzeloc, Serge Creutz, Tine Marie Leaym.
Application Number | 20060167117 10/548775 |
Document ID | / |
Family ID | 33099985 |
Filed Date | 2006-07-27 |
United States Patent
Application |
20060167117 |
Kind Code |
A1 |
Leaym; Tine Marie ; et
al. |
July 27, 2006 |
Controlled release compositions
Abstract
A composition for controlled release of an active material such
as a fragrance, sunscreen, vitamin or biocide in a product such as
a hair shampoo, shower gel, another personal product such as an
antiperspirant or deodorant, a household cleaning product such as a
laundry detergent, hard surface cleaner or polishes, or a fabric
softener, air freshener or tumble drier sheet, comprises a blend of
the active material and a waxy cyclopolysiloxane. The
cyclopolysiloxane is preferably substituted by hydrocarbon
substituents having 12 or more carbon atoms and may also contain an
aryl or aralkyl substituent.
Inventors: |
Leaym; Tine Marie; (Saginaw,
MI) ; Bouzeloc; Sylvie; (Montigny-Le-Tilleul, BE)
; Creutz; Serge; (Rocourt, BE) |
Correspondence
Address: |
DOW CORNING CORPORATION CO1232
2200 W. SALZBURG ROAD
P.O. BOX 994
MIDLAND
MI
48686-0994
US
|
Family ID: |
33099985 |
Appl. No.: |
10/548775 |
Filed: |
March 26, 2004 |
PCT Filed: |
March 26, 2004 |
PCT NO: |
PCT/EP04/04011 |
371 Date: |
September 8, 2005 |
Current U.S.
Class: |
514/310 ;
424/432; 514/876 |
Current CPC
Class: |
A61Q 17/04 20130101;
A61Q 5/02 20130101; A61Q 19/00 20130101; A61Q 15/00 20130101; A61K
8/891 20130101; A61Q 13/00 20130101; C11D 3/3734 20130101; C11D
3/373 20130101; D06M 15/643 20130101; A61Q 19/10 20130101 |
Class at
Publication: |
514/876 ;
424/432 |
International
Class: |
A61F 6/14 20060101
A61F006/14 |
Foreign Application Data
Date |
Code |
Application Number |
Mar 27, 2003 |
GB |
0306995.2 |
Sep 20, 2003 |
GB |
0322044.9 |
Claims
1. A process for controlling the release of an active material,
selected from fragrances, sunscreens, vitamins, drugs, biocides,
pest repellents, catalysts and cooling agents, from a cleaning
composition, personal care product, household care product or
textile treatment composition by blending the active material and a
waxy silicone material before adding the active material to the
cleaning composition, personal care product, household care product
or textile treatment composition, characterized in that the waxy
silicone material has a melting point 10-200.degree. C., that the
waxy silicone material comprises a cyclopolysiloxane in which at
least 20 percent of the silicon atoms in the cyclopolysiloxane have
an alkyl substituent having 16 to 100 carbon atoms, and that 10 to
80 percent of the silicon atoms of the cyclopolysiloxane have a
silicon-bonded substituent of the formula X-Ph, wherein X denotes a
divalent aliphatic organic group bonded to silicon through a carbon
atom and Ph denotes an aromatic group.
2. A process according to claim 17 in which 50-80 percent of the
silicon atoms in the cyclopolysiloxane have an alkyl substituent
having 16 to 100 carbon atoms, and 20 to 50 percent of the silicon
atoms of the cyclopolysiloxane have a silicon-bonded substituent of
the formula X-Ph.
3. A composition for controlling the release of an active material,
selected from fragrances, sunscreens, vitamins, drugs, biocides,
pest repellents, catalysts and cooling agents, from a cleaning
composition, personal care product, household care product or
textile treatment composition, comprising a blend of the active
material and a waxy silicone material, characterized in that the
blend of active material and waxy silicone material is in
particulate or emulsion form, that the waxy silicone material has a
melting point 10-200.degree. C., that the waxy silicone material
comprises a cyclopolysiloxane in which at least 20 percent of the
silicon atoms in the cyclopolysiloxane have an alkyl substituent
having 16 to 100 carbon atoms, and that 10 to 80 percent of the
silicon atoms of the cyclopolysiloxane have a silicon-bonded
substituent of the formula X-Ph, wherein X denotes a divalent
aliphatic organic group bonded to silicon through a carbon atom and
Ph denotes an aromatic group.
4. A composition according to claim 19 in which 50-80 percent of
the silicon atoms in the cyclopolysiloxane have an alkyl
substituent having 16 to 100 carbon atoms and 20 to 50 percent of
the silicon atoms of the cyclopolysiloxane have a silicon-bonded
substituent of the formula X-Ph.
5. A composition according to claim 19, characterized in that the
blend of active material and waxy cyclopolysiloxane is present as
the disperse phase of an oil-in-water emulsion.
6. A composition according to claim 19, characterized in that the
emulsifying surfactant of the said oil-in-water emulsion comprises
a cationic surfactant a cationic surfactant comprising a quaternary
ammonium material containing at least one ester linking group in
the quaternary ammonium molecule.
7. A composition for controlling the release of an active material,
selected from fragrances, sunscreens, vitamins, drugs, biocides,
pest repellents, catalysts and cooling agents, from a cleaning
composition, personal care product, household care product or
textile treatment composition, comprising a blend of the active
material and a waxy silicone material, characterized in that the
blend of active material and waxy silicone material is in emulsion
form, that the waxy silicone material has a melting point
10-200.degree. C., that the waxy silicone material comprises a
cyclopolysiloxane in which at least 20 percent of the silicon atoms
in the cyclopolysiloxane have an alkyl substituent having 16 to 100
carbon atoms, that 10 to 80 percent of the silicon atoms of the
cyclopolysiloxane have a silicon-bonded substituent of the formula
X-Ph, wherein X denotes a divalent aliphatic organic group bonded
to silicon through a carbon atom and Ph denotes an aromatic group,
and that the emulsifying surfactant of the emulsion is a quaternary
ammonium material containing at least one ester linking group in
the quaternary ammonium molecule.
8. A composition according to claim 23 in which 50-80 percent of
the silicon atoms in the cyclopolysiloxane have an alkyl
substituent having 16 to 100 carbon atoms and 20 to 50 percent of
the silicon atoms of the cyclopolysiloxane have a silicon-bonded
substituent of the formula X-Ph.
9. A cyclopolysiloxane comprising a wax having a melting point of
10-200.degree. C. wherein at least 20 percent of the silicon atoms
in the cyclopolysiloxane wax have an alkyl substituent containing
16 to 100 carbon atoms, and 10 to 80 percent of the silicon atoms
of the cyclopolysiloxane wax have a silicon-bonded substituent of
the formula X-Ph, wherein X denotes a divalent aliphatic organic
group bonded to silicon through a carbon atom and Ph denotes an
aromatic group.
10. A cyclopolysiloxane according to claim 25 in which 50-80
percent of the silicon atoms in the cyclopolysiloxane wax have an
alkyl substituent containing 16 to 100 carbon atoms, and 20 to 50
percent of the silicon atoms of the cyclopolysiloxane wax have a
silicon-bonded substituent of the formula X-Ph.
Description
[0001] This invention relates to compositions and processes for the
controlled release of active materials suitable for incorporation
in personal care products such as hair shampoos and soaps and
shower gels for personal washing, in other personal care products
such as antiperspirants or deodorants, in cleaning compositions
such as laundry detergents, hard surface cleaners or wiping cloths,
in other household care products such as polishes or air
fresheners, or in textile treatment compositions such as fabric
softeners or tumble drier sheets.
[0002] One type of active material for which controlled release is
desired is a fragrance composition. Fragrances are frequently
incorporated in detergents and other cleaning products to give a
pleasant odour during use of the cleaning product and to mask the
inherent smell of the soap or other surfactant present in the
cleaning product. The fragrances are generally complex mixtures of
fragrant compounds of varying volatility. Upon storage in a
cleaning composition, perfumes and fragrances can be altered
through interactions and/or reactions with the other components of
the composition. Due to their volatile nature, the fragrant
compounds tend to be dissipated with time, particularly the most
volatile compounds which are often associated with perceived
freshness. Moreover, when used, such as during washing of fabrics
with a laundry detergent, most of the perfume is also lost in the
aqueous phase during the washing cycle. It has been recognised as
desirable that the fragrance should survive storage in the cleaning
composition and also survive the cleaning process and should be
deposited on the fabric, so that fabrics laundered with a detergent
containing the fragrance should have the pleasant odour of the
fragrance.
[0003] Furthermore, once adsorbed onto the targeted surface, for
example fabrics or hair or skin, the fragrance tends to be
dissipated very quickly. There is thus a need to improve the
storage stability of perfumes and fragrances, their delivery in the
application and their long-lasting effect through sustained delayed
release once applied on fabrics.
[0004] Various methods of protecting the fragrance composition have
been proposed. The perfume may be mixed with a porous carrier such
as zeolite and then coated with a protective barrier, for example a
sugar derivative before incorporation in a laundry detergent as
described in WO98/41607. U.S. Pat. No. 4,973,422 describes
encapsulating perfume particles with a pH sensitive coating
comprising an acrylic resin and cellulose esters. WO-A-98/28936
describes mixing the perfume with an aqueous slurry of polymer
beads made of hydrophobic polyacrylate; polyvinyl alcohol can be
adsorbed at the surface of the beads to improve deposition.
WO-A-00/02981 describes reacting a perfume component with an amine
to obtain a release of the active component over a longer period of
time.
[0005] U.S. Pat. No. 6,050,129 relates to a process for testing
diffusivity, odour character and odour intensity of a fragrance
material used in an air freshener and describes mixing perfume with
a hydrophobic wax such as candelilla wax or carnauba wax and
emulsifying the blend in water, preferably with cationic
surfactants, to form a long lasting fragrance composition for use
in a hair care composition such as a shampoo/conditioner.
[0006] WO-A-01/25389 describes a domestic care product comprising a
fragrance particle. The particle comprises a fragrance composition
and a silicone polymer having a melting point of at least
10.degree. C. At least 20% of the silicone atoms in the silicone
polymer have a substituent of 16 carbon atoms or more.
[0007] U.S. Pat. No. 5,160,494 describes a perfume composition
comprising a perfume oil and a volatile alkylmethylsiloxane, which
may be a short chain linear alkylmethylsiloxane or a cyclic
alkylmethylsiloxane.
[0008] JP-A-1-294612 describes a makeup cosmetic such as lipstick,
foundation, eye shadow or sunstick containing a cyclic poly(methyl
16-30 C alkyl siloxane) wax to impart waxy properties to the
cosmetic. JP-A-7-41413 describes a makeup cosmetic containing the
same cyclic polysiloxane wax and an alkyl-modified silicone oil to
impart superior cosmetic holding. There is no suggestion in these
patents of controlled release of any ingredient.
[0009] EP-A-908174 describes a fragrance composition comprising
ellipsoidal hydrophobic particles consisting of a single phase
solid solution of a hydrophobic polymer or wax of melting point
35-120.degree. C. having dissolved therein a hydrophobic fragrance
material, and a hydrophilic surfactant proximate to the outer
surface of the particles.
[0010] According to the present invention a process for controlling
the release of an active material, selected from fragrances,
sunscreens, vitamins, drugs, biocides, pest repellents, catalysts
and cooling agents, from a cleaning composition, personal care
product, household care product or textile treatment composition by
blending the active material and a waxy silicone material before
adding the active material to the cleaning composition, personal
care product, household care product or textile treatment
composition, is characterised in that the waxy silicone material is
a cyclopolysiloxane substituted by hydrocarbon substituents having
12 or more carbon atoms.
[0011] One example of an active material is a fragrance
composition. The fragrance composition may be solid or liquid and
may be a single fragrant compound, or a natural scented oil, or may
be a mixture of fragrant compounds and/or natural oils. Examples of
such natural oils and fragrant compounds are described in
WO-A-01/25389; these natural oils and fragrant compounds are in
particular those suitable for use in cleaning compositions for
household or personal use, or for air fresheners. The fragrance
composition may be a perfume for incorporation in a personal care
product such as a skin cream, shampoo or face cream, or may be a
flavour or aroma compound to be applied for example to food or food
packaging. Flavour compounds, for example fruit flavours such as
strawberry essence, can also be applied to toys or other objects.
The fragrance composition can alternatively comprise a chemically
protected fragrance compound such as a reaction product of the
fragrance compound.
[0012] An alternative type of active material which can be
incorporated in the controlled release composition is a sunscreen
composition. Examples of sunscreens include those which absorb
ultraviolet light between about 290-320 nanometers (the UV-B
region) such as para-aminobenzoic acid derivatives and cinnamates
such as octyl methoxycinnamate or 2-ethoxyethyl p-methoxycinnamate;
and those which absorb ultraviolet light in the range of 320-400
nanometers (the UV-A region) such is benzophenones and butyl
methoxy dibenzoylmethane. Additional examples of sunscreen
chemicals which may be used as active material in the present
invention include menthyl anthranilate; homomenthyl salicylate;
glyceryl p-aminobenzoate; isobutyl p-aminobenzoate; isoamyl
p-dimethylaminobenzoate; 2,2'-dihydroxy-4-methoxybenzophenone;
2-hydroxy-4-methoxybenzophenone; 4-mono and
4-bis(3-hydroxy-propyl)amino isomers of ethyl benzoate; and
2-ethylhexyl p-dimethylaminobenzoate. The invention is particularly
applicable to lipophilic screening agents, including the family of
screening agents derived from dibenzoylmethane and more especially
4-tert-butyl-4'-methoxydibenzoylmethane, which effectively have a
high intrinsic power of absorption. These dibenzoylmethane
derivatives are well known as UV-A active screening agents and are
described in particular in European patent application
EP-A-0,114,607. 4-(tert-butyl)-4'-methoxydibenzoylmethane is sold
under the trade mark "Parsol 1789" by Givaudan. Another
dibenzoylmethane derivative which is preferred according to the
present invention is 4-isopropyldibenzoylmethane, sold under the
name "Eusolex 8020" by Merck. Octocrylene, a liquid lipophilic
screening agent known for its activity in the UV-B range and sold
under the trade mark "Uvinul N 539" by BASF. Another lipophilic (or
liposoluble) screening agent which can be used in the invention is
p-methylbenzylidenecamphor, which is known as a UV-B absorber and
is sold under the trade name "Eusolex 6300" by Merck. The sunscreen
can alternatively be a hydrophilic screening agent, for example one
or more of those described in Application EP-A-678,292,
particularly a 3-benzylidine-2-camphorsulphonic derivative such as
benzene-1,4-[di(3-methylidenecamphor-10-sulphonic acid)], known
under the trade name Mexoryl SX, or a sulphonic derivative of
benzophenone or 2-phenylbenzimidazole-5-sulphonic acid, for example
that sold under the trade mark "Eusolex 232" by Merck,
benzene-1,4-di(benzimidazol-2-yl-5-sulphonic acid) or
benzene-1,4-di(benzoxazol-2-yl-5-sulphonic acid).
[0013] An alternative type of active material which can be
incorporated in the controlled release composition is a vitamin
composition. Vitamins are a class of organic compounds that must be
ingested part of the diet for humans (and other organisms) in order
to maintain health and well being. Some vitamins also have
beneficial effects when applied topically and for this reason are
popular ingredients in various personal care formulations, where it
is desired that the vitamin should be released gradually after the
formulation has been applied to the skin or hair.
[0014] Vitamins comprise a variety of different organic compounds
such as alcohols, acids, sterols, and quinones. They can be
classified into two solubility groups: lipid-soluble vitamins and
water-soluble vitamins. Lipid-soluble vitamins that have utility in
personal care formulations include retinol (vitamin A),
ergocalciferol (vitamin D.sub.2), cholecalciferol (vitamin
D.sub.3), phytonadione (vitamin K.sub.1), and tocopherol (vitamin
E). Water-soluble vitamins that have utility in personal care
formulations include ascorbic acid (vitamin C), thiamin (vitamin
B.sub.1) niacin (nicotinic acid), niacinamide (vitamin B.sub.3),
riboflavin (vitamin B.sub.2), pantothenic acid (vitamin B.sub.5),
biotin, folic acid, pyridoxine (vitamin B.sub.6), and
cyanocobalamin (vitamin B.sub.12). The present invention is
particularly useful in giving controlled release of lipid-soluble
vitamins but can also give controlled release of some water-soluble
vitamins. Examples of vitamins which have been blended with a waxy
cyclopolysiloxane to give controlled release are vitamins A and
E.
[0015] Many of the vitamins that are used in personal care
compositions are inherently unstable and therefore present
difficulties in the preparation of shelf-stable personal care
compositions. The instability of the vitamins is usually related to
their susceptibility to oxidation. For this reason, vitamins are
often converted into various derivatives that are more stable in
personal care formulations. These vitamin derivatives offer other
advantages in addition to improved stability. Vitamin derivatives
can be more amenable to certain kinds of personal care
formulations. For example a lipid-soluble vitamin can be
derivatized to produce a water-soluble material that is easier to
incorporate into a water-based formulation. Retinol and tocopherol
are two lipid-soluble vitamins that are particularly useful in skin
care compositions and consequently there are many different
derivatives of these two vitamins that are used in personal care
compositions. Derivatives of retinol include retinyl palmitate
(vitamin A palmitate), retinyl acetate (vitamin A acetate), retinyl
linoleate (vitamin A linoelate), and retinyl propionate (vitamin A
propioniate). Derivatives of tocopherol include tocopheryl acetate
(vitamin E acetate), tocopheryl linoleate (vitamin E linoleate),
tocopheryl succinate (vitamin E succinate), tocophereth-5,
tocophereth-10, tocophereth-12, tocophereth-18, tocophereth-50
(ethoxlyated vitamin E derivatives), PPG-2 tocophereth-5, PPG-5
tocophereth-2, PPG-10 tocophereth-30, PPG-20 tocophereth-50, PPG-30
tocophereth-70, PPG-70 tocophereth-100 (propoxylated and
ethoxylated vitamin E derivatives), and sodium tocopheryl
phosphate. The invention can be used to give controlled release of
these vitamin derivatives. Derivatives of ascorbic acid (Vitamin C)
such as ascorbyl palmitate, ascorbyl dipalmitate, ascorbyl
glucoside, ascorbyl tetraisopalmitate, and tetrahexadecyl ascorbate
can also be used as the active material, as can vitamin derivatives
incorporating two different vitamins in the same compound, for
example ascorbyl tocopheryl maleate, potassium ascorbyl tocopheryl
phosphate or tocopheryl nicotinate.
[0016] A further alternative type of active material which can be
incorporated in the controlled release composition is a biocide,
for example to give prolonged protection of a composition against
bacterial degradation or to give a prolonged biocidal effect to a
substrate to which the composition has been applied. The active
material can also be a pest repellent, for example an insect
repellent, or a repellent for rodents, or a repellent for any
animal including cats or dogs. Insect repellent personal care
products can for example be in the form of creams, sticks or
sprays, and controlled release of the insect repellent from the
personal care product is required after the product has been
applied to the skin.
[0017] A further alternative type of active material which can be
incorporated in the controlled release composition is a catalyst,
for example a curing catalyst in coatings or adhesives where
controlled release is advantageous to give thorough cure without
curing too rapidly. One example of such a catalyst is a fatty amine
to be used as curing agent for an epoxy resin composition.
[0018] The invention can also be used to give controlled release of
a cooling agent (a material which gives a cooling sensation to the
skin) such as menthol or other cooling agents described in
WO96/19119. The blend of cooling agent and waxy cyclopolysiloxane
material can be incorporated in a skin care composition to give
prolonged release of the cooling agent when the composition is
rubbed into the skin. The invention can also be used to give
controlled release of a drug (a pharmaceutically active material)
from a composition which is applied to the skin to dose the drug by
transdermal delivery.
[0019] The invention is particularly applicable to hydrophobic
lipophilic active materials, since these are more readily miscible
with the waxy cyclopolysiloxanes and are less readily released from
blends with waxy cyclopolysiloxanes, but the invention is also
effective in giving controlled release of hydrophilic active
materials provided these are not so hydrophilic that they have a
high solubility in water.
[0020] We have found that the waxy cyclopolysiloxanes tend to be
more miscible with the active materials, and in particular with
perfume compounds, than linear polysiloxane waxes are. We have also
found that the waxy cyclopolysiloxanes tend to provide a longer
lasting effect, that is a more sustained release of the fragrance
or sunscreen or vitamin.
[0021] The waxy cyclopolysiloxane generally contains hydrocarbon
substituents having 12 or more carbon atoms. The waxy
cyclopolysiloxane preferably comprises methyl alkyl siloxane units
((CH3)(R')SiO2/2), where R' is a long chain alkyl group having 12
or more, preferably 16 to 100 carbon atoms. The long chain alkyl
group R' can optionally be substituted by polar substituents such
as amino, amido, alcohol, alkoxy, or ester groups. All the siloxane
units of the waxy cyclopolysiloxane may be such methyl alkyl
siloxane units, or the waxy cyclopolysiloxane may additionally
contain dimethyl siloxane units or units of the formula
((CH.sub.3)(R'')SiO.sub.2/2) where R'' is an alkyl group having
1-11 carbon atoms, for example ethyl, a cycloalkyl group such as
2-cyclohexylethyl, a haloalkyl group or an aromatic group. The
methyl group of the above siloxane units could be replaced by ethyl
or another lower alkyl group if desired. Preferably at least 20% of
the silicon atoms in the polysiloxane, and most preferably at least
50%, have an alkyl substituent having 16 to 100 carbon atoms, most
preferably 20 to 45 carbon atoms. The cyclopolysiloxane is
preferably a cyclotetrasiloxane or cyclopentasiloxane or a mixture
thereof. One preferred type of waxy cyclopolysiloxane contains
aromatic groups, for example aryl groups attached directly to Si
such as phenyl, or aralkyl groups comprising phenyl or substituted
phenyl groups attached to silicone through an alkylene linkage, in
addition to long chain alkyl groups. Waxy cyclopolysiloxanes
containing aralkyl groups, that is, silicon-bonded substituents of
the formula X-Ph, wherein X denotes a divalent aliphatic organic
group bonded to silicon through a carbon atom and Ph denotes an
optionally substituted aromatic group, are particularly preferred,
for example 2-phenylpropyl, benzyl, 2-phenylethyl or
2-(t-butylphenyl)ethyl. Such aralkyl groups may for example be
present in 10 to 80%, preferably 20 to 50% of the siloxane units of
the waxy cyclopolysiloxane, usually as methyl aralkyl siloxane
units. The waxy cyclopolysiloxane preferably has a melting point in
the range 10-200.degree. C., most preferably 30 to 80.degree.
C.
[0022] The waxy cyclopolysiloxane can in general be produced by the
reaction of a cyclopolysiloxane containing SiH groups such as
tetramethylcyclotetrasiloxane or pentamethylcyclopentasiloxane with
a long chain alpha-olefin of the formula R'CH.dbd.CH.sub.2 in the
presence of a hydrosilylation catalyst such as a platinum group
metal compound. Aralkyl and/or cycloalkyl groups can be introduced
by the reaction of such compounds as alpha-methylstyrene, styrene
or vinylcyclohexane with the cyclopolysiloxane before,
simultaneously with or following reaction of the long chain
alpha-olefin. The waxy cyclopolysiloxane may contain some residual
SiH groups, or any such residual SiH groups can be reacted with a
short chain olefin, for example with ethene to introduce ethyl
groups. The waxy cyclopolysiloxane can be produced by the addition
of olefin(s) sequentially or concurrently to SiH containing
silicone or by the addition of SiH to olefin(s).
[0023] The waxy cyclopolysiloxanes containing aralkyl groups are
new materials. The invention thus includes a wax of melting point
10-200.degree. C. which is a cyclopolysiloxane in which at least
20% of the silicon atoms in the cyclopolysiloxane have an alkyl
substituent having 16 to 100 carbon atoms and 10 to 80% of the
silicon atoms of the cyclopolysiloxane have a silicon-bonded
substituent of the formula X-Ph, wherein X denotes a divalent
aliphatic organic group bonded to silicon through a carbon atom and
Ph denotes an aromatic group.
[0024] The waxy cyclopolysiloxane can be mixed with a liquid
silicone, for example a polydiorganosiloxane, a branched liquid
polysiloxane, a silicone polyether copolymer or an
aminopolysiloxane. Particularly preferred liquid polysiloxanes are
those containing aryl, for example phenyl, or aralkyl, for example
benzyl, 2-phenylethyl or 2-phenylpropyl groups in addition to alkyl
groups such as methyl. The liquid polydiorganosiloxane can be
linear or cyclic; cyclic siloxanes such as
tetra(2-phenylpropyl)tetramethylcyclotetrasiloxane may be
preferred. The liquid polysiloxane can contain functional groups,
for example it can contain hydroxyl groups such as terminal silanol
groups in a linear polydiorganosiloxane such as
polydimethylsiloxane, alkoxy groups such as methoxy, ethoxy or
propoxy bonded to silicon, or amino, amido, alcohol or alkoxy
groups substituted in an organic group bonded to silicon. The waxy
hydrophobic mixture of the waxy cyclopolysiloxane and the liquid
silicone is preferably a solid, for example it preferably has a
melting point in the range 10-200.degree. C., but can alternatively
be a viscous liquid. The liquid silicone can for example be used at
up to 100% or even higher based on the weight of the wax, such as
up to 200 or 300%, particularly if the blend of wax and liquid
silicone is solid at 10.degree. C., although the liquid silicone if
used is preferably present at 1 to 60%, most preferably 10 to 30%,
based on the weight of wax. An organic liquid, for example liquid
paraffin or a naphthenic oil, can be used alternatively or
additionally if it is compatible with the blend of active material
and waxy cyclopolysiloxane.
[0025] The blend of active material and waxy cyclopolysiloxane can
incorporate a further wax, for example a linear polysiloxane wax or
an organic which does not contain silicon, although the waxy
cyclopolysiloxane preferably forms at least 50% by weight of the
wax component of the blend. Suitable linear polysiloxane waxes
generally contain methyl alkyl siloxane units ((CH3)(R')SiO2/2) as
described above and can contain other substituents such as aralkyl,
aryl, alkyl or cycloalkyl groups as described above for the waxy
cyclopolysiloxane.
[0026] In one preferred form of the invention the composition for
controlled release of active material, for example fragrance, forms
the disperse phase of an oil-in-water emulsion. Most preferably,
the continuous phase of the emulsion comprises an aqueous solution
of concentration at least 0.1 molar of a salt capable of ionic
disassociation in water. We have found that the high ionic strength
of the continuous phase increases the partition coefficient between
the continuous phase and the waxy cyclopolysiloxane matrix, so that
the active material tends to stay in the wax phase rather than
diffusing into the continuous phase.
[0027] The salt present in the continuous phase can for example be
an alkali metal, ammonium or alkaline earth metal salt. It can be
an inorganic salt such as a chloride, sulphate or phosphate but is
preferably an organic salt, particularly a carboxylate. The salt
can be a monocarboxylate such as an acetate or propionate, for
example sodium acetate, or a di- or poly-carboxylate salt, for
example a succinate, phthalate or citrate. The salt can be a
polyelectrolyte, for example a salt of a polymeric acid such as a
polycarboxylate, e.g. a polyacrylate or polymethacrylate or a salt
of an acrylic or methacrylic acid copolymer. Examples of such
polyelectrolyte salts are sold under the Trade Mark `Sokolan`. The
salt in the continuous phase can alternatively be a salt of a
polycation such as a polymer having pendant quaternary ammonium
groups. An example of such a cationic polymer is sold under the
Trade Mark `Merquat` and contains dimethyl diallyl ammonium
chloride or methacrylamidopropyl trimethyl ammonium chloride
groups. The salt preferably has no surfactant properties; in
general, the salt should not contain any organic group which has a
chain of 8 or more carbon atoms unsubstituted by polar groups. The
concentration of the salt in the aqueous solution which forms the
continuous phase of the emulsion is preferably at least 0.1 M
(molar), more preferably at least 1 M, up to 5 or 10 M. In the case
of a salt of a polyelectrolyte, the concentration is measured as
the concentration of the non-polymeric ion of the salt.
[0028] The emulsion can conveniently be formed by melting the blend
of active material and waxy cyclopolysiloxane, and liquid silicone
if used, and emulsifying it in the continuous phase using at least
one surfactant. The surfactant is preferably immiscible with the
said blend. The surfactant can be a cationic, anionic, nonionic or
amphoteric surfactant, although the ionic surfactants are more
likely to be immiscible with a perfume wax blend. Cationic
surfactants are particularly preferred because of their propensity
to adsorb at surfaces, in particular onto fabrics. Examples of
suitable cationic surfactants include alkylamine salts, quaternary
ammonium salts, sulphonium salts and phosphonium salts. Especially
preferred cationic surfactants are quaternary ammonium materials
containing at least one ester group ("esterquats"). The ester group
is preferably a linking group in the quaternary ammonium molecule.
Preferred esterquats comprise a quaternary ammonium moiety
containing one, two or three higher molecular weight groups, for
example of 12 to 22 carbon atoms, containing at least one ester
linkage, and three, two or one lower molecular weight alkyl groups.
Such esterquats are described in U.S. Pat. No. 4,137,180, for
example 1,2-bis(hardened tallowoyloxy)-3-trimethylammonium-propane
chloride and/or 1-hardened
tallowoyloxy-2-hydroxy-3-trimethylammonium-propane chloride,
di(tallowoyloxyethyl) dimethyl ammonium chloride, or
di(tallowoyloxyethyl) methyl hydroxyethyl methosulphate. We have
found that use of esterquat surfactants in the emulsion of active
material and waxy cyclopolysiloxane can reduce the level of
silicone wax needed to give controlled fragrance delivery, for
example in a rinse cycle softener used in home laundry.
[0029] The emulsion can alternatively be made by emulsifying the
waxy cyclopolysiloxane in the absence of the active material. The
active material, for example a fragrance or sunscreen composition
is post-added to the emulsion, which is then heated above the
melting point of the waxy cyclopolysiloxane and left standing at
this temperature, preferably for a period of at least 10 minutes,
for example 30-60 minutes, allowing the active material to diffuse
within the hydrophobic waxy cyclopolysiloxane droplet.
[0030] The composition for controlled release of active material
can be produced in various forms. For example in the case of
fragrances, for some applications the controlled release fragrance
composition can simply be mixed with a cleaning or cosmetic
composition. The controlled release fragrance composition can be
produced in particulate form, which may be preferred for blending
with a solid cleaning product such as a powder detergent. An
emulsion as described above can be deposited on a particulate solid
carrier or can be spray dried. Alternatively the blend of fragrance
composition, waxy cyclopolysiloxane and optionally liquid silicone
can be melted and the melt can be deposited on a particulate solid
carrier or can be spray dried. Examples of suitable solid carriers
include soda ash (sodium carbonate), zeolites and other
aluminosilicates or silicates, for example magnesium silicate,
phosphates, for example powdered or granular sodium
tripolyphosphate, sodium sulphate, sodium carbonate, sodium
perborate, cellulose derivatives such as sodium
carboxymethylcellulose, granulated or native starch and clay.
[0031] The carrier particles are preferably mixed while being
treated in a granulation process which produces agglomerated
granules. In one preferred process, the particles are agitated in a
vertical, continuous high shear mixer in which an emulsion of the
composition for controlled release of fragrance is sprayed onto the
particles. If needed to improve the granulation process, the
emulsion can be diluted with for example water, molten polyethylene
glycol or an aqueous solution of polyelectrolyte. One example of
such a mixer is a Flexomix mixer supplied by Hosokawa Schugi. The
spraying and mixing produces agglomerated granules. Alternative
mixers may be used, for example horizontal mixers such as pin
mixers or paddle mixers, ploughshare mixers, twin counter-rotating
paddle mixers, or intensive mixers including a high shear mixing
arm within a rotating cylindrical vessel. Alternatively a fluid bed
coating procedure can be used. Advantageously a process of
granulation by mixing can be followed by cooling and drying in a
continuous fluid bed.
[0032] Granules produced from an emulsion whose continuous phase is
an aqueous solution of a polyelectrolyte salt may be post-coated
with a material, for example a polymer, of opposite charge to the
polyelectrolyte. If the salt in the continuous phase of the
emulsion is a cationic polyelectrolyte salt, for example, the
granules can be post-coated with an anionic polyelectrolyte. Such
post-coating may improve the deposition of the perfume on a fabric
which is subsequently washed or rinsed in the presence of the
granules.
[0033] Granules with a perfume content of up to 15%, for example
8-12%, by weight can readily be produced by the process of the
invention. An emulsion according to the invention can have a
perfume content of up to 30 or 40% or even 50% by weight.
[0034] In an alternative process according to the invention for
producing a fragrant powdered cleaning product, the emulsion
described above is deposited on a powdered cleaning product, for
example by spraying the emulsion onto a detergent powder
composition, and is subsequently dried.
[0035] In a process according to the invention for producing a
fragrant liquid cleaning product, for example a liquid laundry
detergent, household cleaning product, fabric softener, hair
shampoo or soap or shower gel for personal washing, or a roll-on or
spray deodorant, an emulsion as described above is dispersed in the
liquid cleaning product, or the blend of a fragrance composition,
waxy cyclopolysiloxane and optionally liquid silicone can be
emulsified in the liquid cleaning product. When producing a
cleaning product or personal care product in gel form, for example
a stick deodorant, an emulsion as described above can be
incorporated in the product when it is in liquid form, or the blend
of a fragrance composition, wax and liquid silicone can be
emulsified in the product when it is in liquid form, before it is
gelled. A tumble drier sheet can be produced by impregnating a
textile material with an emulsion as described above.
[0036] A textile treatment composition according to the present
invention may be any composition for treating fibrous material
including leather or paper as well as natural or synthetic fibre
textile materials such as woven, nonwoven or knitted fabrics. In
addition to tumble drier sheets mentioned above, release of
fragrance can be controlled from fabric softeners, fabric and
garment finishing compositions, leather finishing compositions or
paper tissue for personal or household cleaning use. Release of
drugs (pharmaceutically active materials) such as menthol or
camphor can be controlled from handkerchiefs or tissues.
[0037] The delayed release fragrance composition of the invention
can alternatively be applied as a coating to a substrate to give
sustained release of perfume from the surface. The coating can for
example be an emulsion as described above.
[0038] Where the active material is a sunscreen composition, the
controlled release composition can for example be prepared in the
form of an emulsion as described above. The emulsion can then be
mixed into a skin care or other cosmetic composition, or into a
fabric care composition. For example, a lipophilic screening
agent(s) can be present in a skin care composition according to the
invention at 0.5 to 30%, preferably from 0.5 to 20%, of the total
weight of the composition. A hydrophilic screening agent(s) can be
present in the skin care composition at 0.1 to 20%, preferably from
0.2 to 10%, by weight of the composition. The skin care composition
can additionally contain pigments, preferably nanopigments (average
primary particle size: generally between 5 nm and 100 nm,
preferably between 10 and 50 nm) of coated or uncoated metal
oxides, such as nanopigments of titanium oxide (amorphous or
crystallized in rutile and/or anatase form), of iron oxide, of zinc
oxide, of zirconium oxide or of cerium oxide, which are all
photoprotective agents which act by physically blocking (reflection
and/or scattering) UV radiation. Examples of coating agents for the
metal oxide pigments are alumina and/or aluminium stearate, and
silicones.
[0039] The advantages of incorporating a UV absorbing sunscreen in
a laundry detergent are described in a paper by M. Schaumann et al
entitled "Sun Protection via Laundry Products" presented at
5.sup.th World Conference on Detergents, 13-17 Oct. 2002 in
Montreux, Switzerland. The UV transmittance of a fabric is reduced
by washing in such a detergent. It is desirable that the sunscreen
should survive storage in the cleaning composition and should not
be lost in the aqueous phase during the washing cycle so that it is
deposited on the fabric. Blending the sunscreen with a waxy
cyclopolysiloxane according to the invention increases the
proportion of sunscreen deposited on the fabric.
[0040] The invention is illustrated by the following Examples:
EXAMPLE 1
[0041] A waxy cyclopolysiloxane (WCP) of melting point 50.degree.
C. was prepared by reacting an olefin mixture consisting of 50% by
weight C26 and C28 olefins and 50% alpha-methylstyrene with
tetramethylcyclotetrasiloxane (cyclic SiH compound). The waxy
cyclopolysiloxane was miscible in weight ratio 1:1 with the
fragrance compounds benzaldehyde, benzyl acetate or cineole. The
waxy cyclopolysiloxane was melted and blended with an equal weight
of cineole. The blend was then placed in an oven at 35.degree. C.
for a weight loss assessment.
[0042] In a comparative experiment 1a, a linear silicone wax (LSW)
was prepared by reacting a linear poly(methylhydrogensiloxane)
having a degree of polymerisation of 60 units with the same olefin
mixture. The wax produced had melting point 63.degree. C. and was
not miscible in weight ratio 1:1 with benzaldehyde or benzyl
acetate. The wax was melted and blended with an equal weight of
cineole and placed in an oven at 35.degree. C. for a weight loss
assessment. The results are shown in Table 1 below. TABLE-US-00001
TABLE 1 Ra- Time Systems tios (days) 1 3 6 16 pure cineole --
Residual 0.0 0.0 0.0 0.0 Example 1a cineole/LSW 1/1 perfume 49.0
10.0 3.4 2.3 Example 1 cineole/WCP 1/1 percentage 73.4 56.1 42.1
22.5
[0043] Table 1 clearly shows that the waxy cyclopolysiloxane gave a
more prolonged release of cineole than the linear silicone wax.
EXAMPLE 2
[0044] A waxy cyclopolysiloxane (WCP 2) of melting point 66.degree.
C. was prepared by reacting an olefin mixture consisting
predominantly of C26 and C28 olefins with
tetramethylcyclotetrasiloxane. 20 g of the waxy cyclopolysiloxane
was melted and blended with 5 g cineole. The blend was then placed
in an oven at 35.degree. C. for a weight loss assessment, the
results of which are shown in Table 2. TABLE-US-00002 TABLE 2
Systems Ratios Time (days) 5 14 21 cineole/WCP2 1/4 Residual 88.1
44.9 27.0 perfume percentage
EXAMPLE 3
[0045] 8 g of cineole, 32 g of the waxy cyclopolysiloxane prepared
in Example 2, 25 g of a cationic polymer sold under the Trade Mark
`Merquat 2001 N` which contains methacrylamidopropyl trimethyl
ammonium chloride groups, 13.5 g of Arquad 16-29 cationic
surfactant and 6.0 g of NaCl were weighed in a reactor and heated
to 70.degree. C. When the mixture was molten, it was emulsified and
diluted with 50 g of water to produce an emulsion having a disperse
phase of a blend of cineole and waxy cyclopolysiloxane in an
aqueous continuous phase having high ionic strength from the
dissolved NaCl and `Merquat 2001 N`.
[0046] 0.42 g of the emulsion was pre-mixed with 1.42 g of fabric
softener based on a cationic surfactant and then diluted with 350
mL of soft water. 70 mL of this solution was poured in a B chner
funnel equipped with a piece of towel as filter (about 3.00 g of
towel). The towel was then line dried and the odour intensity was
monitored subjectively in a panel test. In a comparative test, the
same process was followed using 0.025 g of pure perfume instead of
the emulsion. The odour of the sample with free perfume is
perceivable during approximately 1.5 hours while the odour of the
sample with perfume blended with waxy cyclopolysiloxane is
perceivable during about 24 h.
EXAMPLES 4 and 5
[0047] 16 g and 24 g respectively of the waxy cyclopolysiloxane of
Example 2 were melted and blended with 4 g benzaldehyde.
EXAMPLE 6
[0048] 5 g of benzaldehyde was blended with 10 g of the waxy
cyclopolysiloxane of Example 2 and 10 g of a liquid
phenyl(trimethylsiloxy)silane sold under the Trade Mark `Dow
Corning DC 556`.
EXAMPLE 7
[0049] 16 g of the silicone wax was melted and blended with 4 g
benzaldehyde and 8 g DC556 liquid silicone.
EXAMPLE 8
[0050] A liquid silicone consisting mainly of
tetra(2-phenylpropyl)tetramethylcyclotetrasiloxane was prepared by
reacting alpha-methylstyrene with tetramethylcyclotetrasiloxane. 10
g of the waxy cyclopolysiloxane wax of Example 2 was melted and
blended with 5 g benzaldehyde and 10 g of the liquid silicone
prepared above.
[0051] Each of the blends of Examples 4 to 8 was then placed in an
oven at 35.degree. C. for a weight loss assessment. The results are
shown in Table 3. TABLE-US-00003 TABLE 3 Systems Ratios Time (days)
1 2 8 15 pure benzaldehyde -- Residual 26.1 24.7 21.8 19.9 (BZA)
perfume Example 4 1/4 percentage 87.4 68.9 8.7 3.9 (BZA/wax)
Example 5 1/6 96.0 83.8 31.8 14.1 (BZA/wax) Example 6 1/2/2 99.0
85.8 27.8 6.2 (BZA/wax/liquid) Example 7 1/4/2 98.0 94.7 52.7 24.5
(BZA/wax/liquid) Example 8 1/2/2 94.2 79.9 31.5 14.4
(BZA/wax/liquid)
EXAMPLE 9
[0052] A suncare composition was prepared by combining the
following components utilizing conventional mixing techniques.
TABLE-US-00004 TABLE 4 Ingredient Wt. % Trade Name/Supplier 1.
Cyclopentasiloxane (and) PEG/PPG- 11 Dow Corning .RTM. 5225C 18/18
Dimethicone FORMULATION AID 2. Cyclomethicone 8 Dow Corning .RTM.
245 FLUID 3. Dow Corning .RTM. waxy Cyclopolysiloxane 4 containing
alkyl substituents and Aryl substituents in emulsion form 4. Octyl
Methoxycinnamate sunscreen 7 Parsol .RTM. MCX/Roche Vitamins Inc.
5. Zinc Oxide (and) Dimethicone 5 Z-Cote HP-1/BASF 6. Butylene
Glycol/Sea Parsley Extract 0.5 Sea Parsley/Collaborative Group 7.
Sodium Chloride 2 8. Polysorbate 20 0.4 Tween 20 Enzyme
Grade/Fisher Chemical Company 9. Water (and) cyclomethicone (and) 3
Melarrest/Collab. Lab. Liquorice extract (and) Butylene glycol
(and) Phospholipids 10. Deionised Water 58.8 11. Diazolidinyl
urea/propylene 0.5 Liquid Germal Plus/ISP glycol/iodopropynul
butylcarbamate
[0053] The waxy cyclopolysiloxane (3) was melted and blended with
the sunscreen (4). The resulting blend was emulsified at a
temperature above the melting point of the waxy cyclopolysiloxane
in an aqueous phase comprising ingredients (6) to (10). The Z-Cote
(5) 5 was added to a mixture of the siloxane fluids (1 and 2) and
mixed until homogeneous, then added to the emulsion with turbulent
mixing. The biocide (11) was added and mixing was continued for 15
minutes
EXAMPLE 10
[0054] A suncare composition was prepared by combining the
following components utilizing conventional mixing techniques.
TABLE-US-00005 TABLE 5 Ingredient Wt. % Trade Name/Supplier 1.
Sucrose Palmitate & Glyceryl Stearate 1 Arlatone V-175/Uniqema
& Glyceryl Stearate Citrate & Sucrose & Mannan &
Xanthan Gum 2. Deionised Water 65.2 3. Glycerin 5 Glycerin/Lambert
Riviere 4. Methyldibromoglutaronitrile & 0.7 Euxyl K400/S&M
Phenoxyethanol 5. Disodium EDTA 0.1 Dissolvine Na2/Akzo Nobel
Chemicals, Inc. 6. EthylHexyl Methoxycinnamate 7 Neo Heliopan
AV/Haarmann & sunscreen Reimer 7. Butyl Methoxydibenzoylmethane
2 Neo Heliopan 357/Haarmann & sunscreen Reimer 8.
4-Methylbenzylidene Camphor 3 Neo Heliopan MBC/Haarmann &
sunscreen Reimer 9. Cyclomethicone 3 Dow Corning .RTM. 345 FLUID
10. C12-15 Alkyl Benzoate 5 Finsolv TN/Witco Corporation 11. C15-19
Alkane 3 Gemseal 40/Total 12. Dow Corning waxy cyclopolysiloxane 5
containing alkyl substituents and Aryl substituents
[0055] The emulsifier (1) was added to water (2) under strong
agitation and mixed for 10 minutes. Ingredients (3) to (5) were
added while continuing mixing and the aqueous mixture was heated to
80.degree. C. The waxy cyclopolysiloxane (12) was melted at
80.degree. C. and blended with the sunscreens (6 to 8). The
resulting blend was emulsified in the hot aqueous mixture. The
diluents (9 to 11) were mixed into the emulsion and homogenised in
a Silverson (Trade Mark) mixer.
EXAMPLE 11
[0056] A hand and body lotion was prepared by combining the
following components TABLE-US-00006 TABLE 6 Ingredient Wt. %
Supplier/Trade Name 1. Stearic acid 2 Henkel-Emery .RTM. 120 2.
Glyceryl stearate, PEG-100 2 Uniqema-Arlacel .RTM. 165 stearate 3.
Cetyl alcohol 3 Henkel-Lanette .RTM. 16NF 4. Mineral oil 5
Crompton-Carnation .RTM. White Mineral Oil 5. Waxy
cyclopolysiloxane 4 containing long chain alkyl substituents 6.
Vitamin A palmitate 1 Roche-Retinyl Palmitate 7. Deionized Water
77.2 8. Glycerin 5 Fisher Chemicals-Glycerin 9. Triethanolamine 0.8
Fisher Chemicals- Triethylamine
[0057] The aqueous phase consisting of glycerin (8),
triethanolamine (9), and water (7) was combined and heated to
70.degree. C. The waxy cyclopolysiloxane (5) and retinyl palmitate
(6) were melted at 70.degree. C., mixed together, and added to the
heated aqueous phase. The Emery.RTM. 120 (1), Arlacel.RTM. 165 (2),
Lanette.RTM. 16NF (3) and Carnation.RTM. white mineral oil (4) were
melted (.about.70.degree. C.) and mixed using a Lightnin.RTM. mixer
(.about.1376 rpm). The water phase with the waxy cyclopolysiloxane
and retinyl palmitate was slowly added to ingredients 1-4 and mixed
until homogenous. The mixing was continued for 15 minutes and then
the batch was cooled to room temperature with continued mixing.
[0058] This procedure was repeated using vitamin E in place of the
retinyl palmitate.
[0059] The procedure was also repeated using a vitamin mixture of
Vitamin A, Vitamin E and Vitamin C in caprylic/capric triglycerides
(sold by BASF as RetiSTAR.RTM.) replacing the retinyl
palmitate.
[0060] In all three experiments release of the vitamin was
controlled by the waxy cyclopolysiloxane.
EXAMPLE 12
[0061] The process of Example 11 was repeated using a waxy
cyclopolysiloxane containing aryl substituents as well as alkyl
substituents in place of the wax used in Example 11. Release of the
vitamin was controlled by the waxy cyclopolysiloxane.
EXAMPLE 13
[0062] A facial moisturizer with sunscreen composition was prepared
by combining the following components TABLE-US-00007 TABLE 7
Ingredient Wt. % Supplier/Trade Name 1. Glycerin 4 Fisher
Chemicals-Glycerin 2. DM DM Hydantoin 0.3 Lonza-Glydant .RTM. 3.
Deionized Water 77.7 4. Octyl Methoxycinnamate 5 BASF-Uvinul .RTM.
MC 80 5. Dimethicone, Dimethicone 5 Dow Corning-9041 Crosspolymer
6. Dow Corning .RTM. waxy 4 Cyclopolysiloxane alkyl substituents
and aryl substituents 7. Vitamin A Palmitate or 1 Roche-Retinyl
Palmitate Vitamin E or Vitamin A, Roche-Tocopherol Vitamin E,
Vitamin C in BASF-RetiSTAR .RTM. Caprylic/Capric Triglycerides 8.
Polyacrylamide, C.sub.13-14 3 Seppic-Sepigel .RTM. 305 Isoparaffin,
Laureth-7
[0063] The water phase consisting of glycerin (1), Glydant (2), and
water (3) was blended using a Lightening.RTM. mixer (.about.300
rpm). Ingredients (4) to (5) were added while continuing mixing and
the mixture was heated to 80.degree. C. The waxy cyclopolysiloxane
(6) and retinyl palmitate (7) were melted at 80.degree. C. and
blended with ingredients (1 to 5). The Sepigel.RTM. 305 was added
to the mixture and the Lightnin.RTM. mixer speed was increased
(.about.1376 rpm) with the thickening of the emulsion. The mixing
was continued for 10 minutes and then the batch was cooled to room
temperature with continued mixing.
[0064] This procedure was repeated using vitamin E in place of the
retinyl palmitate and also with the vitamin mixture (RetiSTAR)
replacing the retinyl palmitate.
[0065] In all three experiments release of the vitamin was
controlled by the waxy cyclopolysiloxane. These experiments were
not designed to control release of the Octyl Methoxycinnamate by
the waxy cyclopolysiloxane.
EXAMPLE 14
[0066] A silicone wax was prepared by reacting an olefin mixture
(C26-C45 alkyl chain length) with tetramethylcyclotetrasiloxane to
form a cyclic poly(methylalkylsiloxane) wax.
[0067] An aqueous thickening solution was prepared by dispersing
3.51 g xanthan gum (Keltrol RD (Trade Mark) and 9.66 g
hydroxyethylcellulose (Natrosol 250 LR(Trade Mark)) in 382.64 g of
demineralised water and adding. 0.69 g sorbic acid, 1.36 g benzoic
acid and 3.15 g of a 10% solution of sulfuric acid.
[0068] 47 g of the thickening solution, 4.5 g of Volpo (Trade Mark)
S2 and 3.9 g of Volpo S20 ethoxylated stearyl alcohol nonionic
surfactants, 14.3 g of sodium chloride, 26 g of Arquad 16-29 and
57.4 g of the silicone wax were loaded in a stirred reactor and
heated to 80.degree. C. 14.42 g of the highly volatile perfume mix
was then added. After 20 minutes, the heating was stopped. 31 g of
the thickening solution followed by 104 g of demineralised water
were finally added to form an emulsion of a blend of perfume and
wax in weight ratio 1:4.
EXAMPLE 15
[0069] 62.6 g of the thickening solution, 6 g of Volpo S2, 5 g of
Volpo S20, 18.6 g of sodium chloride, 34.5 g of Arquad 16-29 and
84.5 g of the cyclic poly(methylalkylsiloxane) wax of Example 14
were loaded in a stirred reactor and heated to 80.degree. C. 11.08
g of the highly volatile perfume mix was then added. After 20
minutes, the heating was stopped. 41 g of the thickening solution
followed by 137 g of demineralised water were finally added to form
an emulsion of a blend of perfume and wax in weight ratio
1:7.6.
[0070] The emulsions of Examples 14 and 15 were each incorporated
in a rinse cycle fabric softener at a level corresponding to 3%
perfume in the softener. They were evaluated in a Miele 934 front
loading washing machine, loaded with 4 terry towels and 5
pillowcases. For the main wash at 40.degree. C., 30 g of a
detergent powder and 17 litres of water were used. The softener was
incorporated in the rinse. After line drying, the odour of the
towels was followed for eight days. Example 15 was found to give
more intense odour during the 8 days of testing than Example 14,
demonstrating that for this perfume used in a rinse cycle, a 1/7.6
perfume/wax provides a better control of fragrance release than the
1/4 ratio.
EXAMPLE 16
[0071] 59.5 g of the thickening solution, 30 g of esterquat
cationic surfactant (Tetranyl L1/90 (Trade Mark)), 33 g of Arquad
16-29 and 64 g of the cyclic poly(methylalkylsiloxane) wax of
Example 14 were loaded in a stirred reactor and heated to
80.degree. C. to form an oil-in-water emulsion. 15.8 g of a highly
volatile perfume mix was then added to the emulsion. After 20
minutes, the heating was stopped. 37.5 g of the thickening solution
followed by 129 g of demineralised water were finally added. The
product was an emulsion of a blend of perfume and wax in weight
ratio 1:4.
[0072] The emulsions of Examples 15 and 16 were compared according
to the same protocol as Examples 14 and 15. This time, the Example
16 emulsion of 1/4 perfume/wax ratio gave a more sustained odour
than Example 15, showing the advantages of the use of
esterquats.
EXAMPLE 17
[0073] A silicone wax was prepared by reacting an olefin mixture
(C26-C45 alkyl chain length) with tetramethylcyclotetrasiloxane to
form a cyclic poly(methylalkylsiloxane) wax.
[0074] An aqueous thickening solution was prepared by dispersing
3.51 g xanthan gum (Keltrol RD (Trade Mark) and 9.66 g
hydroxyethylcellulose (Natrosol 250 LR(Trade Mark)) in 382.64 g of
demineralised water and adding. 0.69 g sorbic acid, 1.36 g benzoic
acid and 3.15 g of a 10% solution of sulfuric acid.
[0075] 62.6 g of the thickening solution, 6 g of Volpo S2, 5 g of
Volpo S20, 18.6 g of sodium chloride, 34.5 g of Arquad 16-29 and
84.5 g of the silicone wax were loaded in a stirred reactor and
heated to 80.degree. C. 11.29 g of a highly volatile perfume mix
was then added. After 20 minutes, the heating was stopped. 41.2 g
of the thickening solution followed by 137 g of demineralised water
were finally added to form an emulsion.
[0076] The emulsion was incorporated into a shower gel comprising
the ingredients (%) shown in Table 8 below: TABLE-US-00008 TABLE 8
Empicol ESB-3 (Trade Mark) surfactant 30 Oramix NS 10 (Trade Mark)
surfactant 5 Amonyl 380 BA (Trade Mark) surfactant 10 Brij 30
(Trade Mark) surfactant 2 Sepigel 305 2 Emulsion of Example 17
17.73 Water 33.27 KOH (10%) q.s.
[0077] Panellists were treated with two shower gels: one with the
emulsion of Example 17 as described above or a control comprising
0.5% free perfume. The perfume intensity on their forearms were
evaluated on a scale of 1 to 20 (20 is highest intensity). The
results are shown in Table 9 TABLE-US-00009 TABLE 9 Odour after 2
Odour after 1 Odour after 3 Odour after 5 minutes hour hours hours
control 0 4 2 1 Shower gel 18 13 15 16 of Example 17
[0078] The same two composition was applied on hair as shampoo.
Panellists were asked to evaluate the perfume intensity on the
hair. The results are shown in Table 10 below TABLE-US-00010 TABLE
10 Time (hours) Control Example 17 0 3 15 2 1 17 4 0 18 6 1 15
* * * * *