Patent Application
20160166492
The present invention relates to a process for making a benefit delivery composition. The process provides a benefit delivery composition having excellent silicone deposition, and excellent product stability profiles.
Silicones are incorporated into a variety of compositions, such as consumer goods products. In some applications, such as laundry treatment, hair treatment, and skin treatment, it is desirable for these silicones to be delivered onto the surface to be treated during the treatment process. However, silicones are typically incorporated into these consumer goods products at very low levels, and the efficiency of silicone deposition onto the treated surface during the treatment process is also low. There remains a need to improve the deposition of silicone onto a treated surface during the treatment process. A benefit delivery composition comprising silicone, surfactant and a fatty amphiphile can be used to deposit the silicone onto a treated surface during a treatment process.
The Inventors have found that the stability of a resultant benefit delivery composition is significantly improved when a benefit delivery composition is prepared by a process that (i) forms a lamellar phase from a surfactant and fatty amphiphile under specific conditions. Such a process provides a benefit delivery composition that exhibits excellent silicone deposition, and excellent product stability.
Such benefit delivery compositions can be incorporated into consumer goods products such as fabric treatment compositions (including laundry detergent compositions), hair treatment compositions (including shampoos and conditioners) and skin treatment compositions (including moisturizer creams and shaving creams).
US2012/0093757 relates to a hair conditioner comprising silicone and a conditioning gel phase.
US2003/0223952 relates to a shampoo comprising detersive surfactant, fatty alcohol gel network and an aqueous carrier.
WO2003/15736 relates to an aqueous composition comprising surfactant, silicone and perfume. In the examples of this reference, the composition is formed by mixing the ingredients together (c.f. example 1). No pre-mixes were formed, and the surfactant was not contacted to a fatty amphiphile at the elevated temperature required to form a lamellar phase composition.
WO2004/24114 relates to a composition comprising a fragrance composition and a silicone in water emulsion comprising at least one surfactant. In the examples of this reference, the silicone is contacted with the surfactant to form the emulsion, and then perfume is mixed with the emulsion. The surfactant was not contacted to a fatty amphiphile at the elevated temperature required to form a lamellar phase composition.
WO2006/012767 relates to a fluid personal care product comprising a fragrance that is dissolved in a silicone oil. In this reference, a silicone/perfume premix is formed, which can then be contacted to a surfactant, e.g. to form an emulsion or to contact with a surfactant phase prior to blending the premix with the other ingredients to give the fluid product (c.f. page 4, lines 12-18). In this reference, the silicone was not contacted with a lamellar phase composition. In this reference, no lamellar phase composition was formed: the surfactant was not contacted to a fatty amphiphile at the elevated temperature required to form a lamellar phase composition.
WO2008/110590 relates to a liquid surfactant composition comprising a cleansing surfactant, polymeric cationic material and an anionic or non-ionic emulsion of a fragrance composition blended with a waxy silicone material. In this reference, a perfume is blended with a silicone. In paragraph 0022, this blend can be formed by emulsification using a surfactant. In the examples (c.f. paragraph 0034), the silicone was contacted with the surfactant, and then perfume was added to this mixture. In this reference, no lamellar phase composition was formed: the surfactant was not contacted to a fatty amphiphile at the elevated temperature required to form a lamellar phase composition.
The present invention provides a process for making a consumer goods product comprising a benefit delivery composition, wherein the process comprises the steps of:
(a) contacting a surfactant and a fatty amphiphile to form a lamellar phase composition;
(b) contacting the lamellar phase composition with silicone to form the benefit delivery composition,
(c) contacting the benefit delivery composition with at least three different consumer goods product ingredients to form a consumer goods product,
wherein the fatty amphiphile has a melting point of at least 40° C., wherein in step (a) the fatty amphiphile is at a temperature above its melting point when it is contacted with the surfactant, wherein the fatty amphiphile is subsequently cooled to a temperature below its melting point, wherein the benefit delivery composition comprises greater than 10 wt % silicone, and wherein the fatty amphilie is selected from fatty acid, fatty alcohol and mixtures thereof.
The benefit delivery composition comprises silicone and a lamellar phase composition. It may be preferred for the benefit delivery composition to consist essentially only of the lamellar phase composition and silicone. The silicone and lamellar phase composition are described in more detail below. The benefit delivery composition comprises silicone, surfactant and fatty amphiphile: these ingredients are described in more detail below. The benefit delivery composition preferably comprises water. The benefit delivery composition may comprise perfume and other ingredients. These other ingredients are described in more detail below.
Preferably, the benefit delivery composition comprises from 50 wt % to less than 90 wt % lamellar phase composition, more preferably from 60 wt % to 80 wt % lamellar phase composition. Preferably, the benefit delivery composition comprises from greater than 10 wt % to 50 wt % silicone, more preferably from 20 wt % to 40 wt % silicone. Preferably, the weight ratio of lamellar phase composition to silicone present in the benefit delivery agent is in the range of from 1:1 to 8:1, preferably from 2:1 to 6:1, or from 2:1 to 4:1.
Preferably, the benefit delivery composition comprises from greater than 10 wt % to 48 wt % silicone, more preferably from 20 wt % to 35 wt % silicone.
Preferably, the benefit delivery composition comprises from 2 wt % to 10 wt % perfume, more preferably from 4 wt % to 8 wt % perfume. Without wishing to be bound by theory, high perfume levels can disrupt the formation of the lamellar phase composition and break down the lamellar phase.
Preferably, the benefit delivery composition comprises from 10 wt % to 30 wt % surfactant, more preferably from 10 wt % to 20 wt % surfactant. Preferably, the benefit delivery composition comprises from 5 wt % to 20 wt % fatty amphiphile, more preferably from 5 wt % to 10 wt % fatty amphiphile. The benefit delivery composition may also comprise water, preferably from 0 wt % water to 75 wt % water, more preferably 20 wt % to 75 wt % water, or even from 50 wt % to 75 wt % water.
Upon dissolution with deionized water at a temperature of 25° C. and a dilution of 1 g/l, the benefit delivery composition forms droplets, wherein the droplets have a volume average droplet size in the range of from 20 μm to 1000 μm, more preferably from 20 μm to 500 μm, or from 20 μm to 150 μm. Without wishing to be bound by theory, ensuring this droplet size distribution leads to good surface deposition, especially on fabric surfaces. Preferably, less than 50% by volume of the droplets have a droplet size greater than 150 μm micrometers, more preferably less than 25%, or less than 10% or even less than 5% by volume of the droplets have a droplet size greater than 150 μm. Without wishing to be bound by theory, by controlling the droplet size in this manner, the benefit delivery composition exhibits good surface deposition without the unwanted visual appearance of oily deposits on the surface. The method for measuring the droplet size of the benefit delivery composition is described in more detail below.
Process for Making a Benefit Delivery Composition:
The process comprises the steps of: (a) contacting a surfactant and a fatty amphiphile to form a lamellar phase composition; (b) contacting the lamellar phase composition and a silicone to form the benefit delivery composition.
Steps (a) and (b) are described in more detail below.
The process can be a continuous process or can be a batch process. In a batch process, it may be preferred for steps (a) and (b) to be carried out in the same equipment. It may also be preferred for steps (a) and (b) to be carried out in separate equipment. For example, the lamellar phase composition is formed in a separate mixer to that used to dose the silicone.
Step (a). Forming a Lamellar Phase Composition:
During step (a), a surfactant is contacted to a fatty amphiphile to form a lamellar phase composition. During step (a), the fatty amphiphile is at a temperature above its melting point when it is contacted with the surfactant. Preferably, the surfactant is at a temperature above the melting point of the fatty amphiphile when it is contacted with the fatty amphiphile. If present, preferably the water is at a temperature above the melting point of the fatty amphiphile when it is contacted to the fatty amphiphile.
The surfactant and fatty amphiphile may be contacted at a temperature of at least 40° C., or even at least 70° C. Preferred heating means include hot water jacketing and/or hot oil jacketing. Other heating means include direct heat, electrical tracing, steam heating.
Suitable equipment for contacting the surfactant to the fatty amphiphile include mixers such as DPM range of high torque mixers from Charles Ross & Son Company, Hauppauge, N.Y.
Preferably, step (a) is carried out at a pH in the range of from 4.0 to 7.0, more preferably from 5.0 to 6.0. When the fatty amphiphile is a fatty acid, preferably step (a) is carried out at a pH that corresponds to, or is similar to, the pKa of the fatty acid. When the fatty amphiphire is a fatty acid, preferably step (a) is carried out at a pH no greater than 0.5 pH units above the pKa of the fatty acid, and no less than 0.5 pH units below the pKa of the fatty acid.
Step (b). Forming a Benefit Delivery Composition:
During step (b), the lamellar phase composition is contacted to silicone to form the benefit delivery composition.
Preferably, the step (b) is carried out under conditions of low shear, typically having a maximum tip speed of 2.5 ms−1, preferably 2.0 ms−1, or even 1.5 ms−1. Preferably, step (b) is carried out at a maximum shear rate of 500 s−1, or from 400 s−1 or even 300 s−1. Without wishing to be bound by theory, carefully controlling the shear conditions in this manner result in a benefit delivery composition having a good surface deposition profile: high shear rates can lead to undesirably small droplet sizes of the resultant benefit delivery composition upon contact with water, which in turn lead to a poor deposition profile. Suitable equipment for carrying out step (b) include DPM range of high torque mixers from Charles Ross & Son Company, Hauppauge, N.Y.
Optional Process Step. Forming a Premix Composition:
It may be preferred for the silicone to be contacted to a perfume to form a premix composition prior to contacting the silicone to the lamellar phase composition. Suitable vessels for this premixing process step include mixers such as the SPP series of mixers from IKA Werke GmbH & Co. KG, Staufen, Germany.
If this optional process step is included in the process, then it may be preferred that prior to this optional process step, the lamellar phase composition is cooled to a temperature below its melting point. Suitable cooling means include water jacketing and a stirred vessel.
Lamellar Phase Composition:
The lamellar phase composition comprises surfactant and fatty amphiphile, preferably the lamellar phase composition comprises water. Preferably, the lamellar phase composition consists essentially only of surfactant, fatty amphile and water. Preferably, the molar ratio of surfactant to fatty amphiphile present in the lamellar phase composition is in the range of from 1:1 to 2.5:1, more preferably 1:1 to 1.5:1. Without wishing to be bound by theory, by controlling the molar ratio in this manner, the resultant droplet size of the benefit delivery composition upon contact with water can be controlled. Without wishing to be bound by theory, increasing the molar amount of fatty amphiphile relative to the molar amount of surfactant increases the resultant droplet size of the benefit deliver composition upon contact with water.
Preferably, the lamellar phase composition has a packing parameter in the range of from 0.5 to 1.0. The packing parameter and method for determining the packaging parameter is described in more detail below.
Optional Premix Composition:
The optional premix composition comprises silicone and perfume. Preferably the premix composition consists essentially only of silicone and perfume.
Preferably, the weight ratio of silicone to perfume present in the premix composition is in the range of from 3:1 to 20, more preferably from 3:1 to 10:1.
Surfactant:
Suitable surfactants include anionic surfactants, non-ionic surfactants, zwitterionic surfactants and amphoteric surfactants.
Suitable anionic detersive surfactants include sulphate and sulphonate detersive surfactants.
Suitable sulphonate detersive surfactants include alkyl benzene sulphonate, such as C10-13 alkyl benzene sulphonate. Suitable alkyl benzene sulphonate (LAS) is obtainable, or even obtained, by sulphonating commercially available linear alkyl benzene (LAB); suitable LAB includes low 2-phenyl LAB, such as those supplied by Sasol under the tradename Isochem® or those supplied by Petresa under the tradename Petrelab®, other suitable LAB include high 2-phenyl LAB, such as those supplied by Sasol under the tradename Hyblene®. Another suitable anionic detersive surfactant is alkyl benzene sulphonate that is obtained by DETAL catalyzed process, although other synthesis routes, such as HF, may also be suitable.
Suitable sulphate detersive surfactants include alkyl sulphate, such as C8-18 alkyl sulphate, or predominantly C12 alkyl sulphate. The alkyl sulphate may be derived from natural sources, such as coco and/or tallow. Alternative, the alkyl sulphate may be derived from synthetic sources such as C12-15 alkyl sulphate.
Another suitable sulphate detersive surfactant is alkyl alkoxylated sulphate, such as alkyl ethoxylated sulphate, or a C8-18 alkyl alkoxylated sulphate, or a C8-18 alkyl ethoxylated sulphate. The alkyl alkoxylated sulphate may have an average degree of alkoxylation of from 0.5 to 20, or from 0.5 to 10. The alkyl alkoxylated sulphate may be a C8-18 alkyl ethoxylated sulphate, typically having an average degree of ethoxylation of from 0.5 to 10, or from 0.5 to 7, or from 0.5 to 5 or from 0.5 to 3.
The alkyl sulphate, alkyl alkoxylated sulphate and alkyl benzene sulphonates may be linear or branched, substituted or un-substituted.
The anionic detersive surfactant may be a mid-chain branched anionic detersive surfactant, such as a mid-chain branched alkyl sulphate and/or a mid-chain branched alkyl benzene sulphonate. The mid-chain branches are typically C1-4 alkyl groups, such as methyl and/or ethyl groups.
Another suitable anionic detersive surfactant is alkyl ethoxy carboxylate.
The anionic detersive surfactants are typically present in their salt form, typically being complexed with a suitable cation. Suitable counter-ions include Na+ and K+. Suitable non-ionic detersive surfactants are selected from the group consisting of: C8-C18 alkyl ethoxylates, such as, NEODOL® non-ionic surfactants from Shell; C6-C12 alkyl phenol alkoxylates wherein optionally the alkoxylate units are ethyleneoxy units, propyleneoxy units or a mixture thereof; C12-C18 alcohol and C6-C12 alkyl phenol condensates with ethylene oxide/propylene oxide block polymers such as Pluronic® from BASF; C14-C22 mid-chain branched alcohols; C14-C22 mid-chain branched alkyl alkoxylates, typically having an average degree of alkoxylation of from 1 to 30; alkylpolysaccharides, such as alkylpolyglycosides; polyhydroxy fatty acid amides; ether capped poly(oxyalkylated) alcohol surfactants; and mixtures thereof. Suitable nonionic detersive surfactants include secondary alcohol-based detersive surfactants. Other suitable non-ionic detersive surfactants include EO/PO block co-polymer surfactants, such as the Plurafac® series of surfactants available from BASF, and sugar-derived surfactants such as alkyl N-methyl glucose amide.
Preferred surfactants include alkyl benzene sulphonate, alkyl ethoxylated sulphate, and mixtures thereof. Preferred surfactants include C10-C13 alkyl benzene sulphonate, C12-C15 alkyl ethoxylated sulphate having an everage degree of ethoxylation in the range of from 1.0 to 5.0 and mixtures thereof. Preferably the surfactant is an anionic surfactant having a cationic counter-ion selected from sodium or calcium. Preferably, the surfactant has a HLB in the range of from 30 to 40.
Fatty Amphiphile:
Suitable fatty amphiphiles are selected from fatty acid, fatty alcohol and mixtures thereof. Preferred fatty amphiphiles are selected from C8-C16 fatty acid, C8-C16 fatty alcohol and mixtures thereof. A highly preferred fatty amphiphile is C12 fatty acid. Preferably, the fatty amphiphile has a melting point of at least 40° C., more preferably at least 50° C. or even at least 60° C.
Preferably, the fatty amphiphile is a fatty acid having a pKa in the range of from 6 to 8. Preferably, the fatty amphiphile has a HLB in the range of from 10 to 20.
Silicone:
Suitable silicones are selected from the group consisting of cyclic silicones, polydimethylsiloxanes, aminosilicones, cationic silicones, silicone polyethers, silicone resins, silicone urethanes, and mixtures thereof.
A preferred silicone is a polydialkylsilicone, alternatively a polydimethyl silicone (polydimethyl siloxane or “PDMS”), or a derivative thereof.
Preferably, the silicone has a viscosity at a temperature of 25° C. and a shear rate of 1000 s−1 in the range of from 10 Pa s to 100 Pa s. Without wishing to be bound by theory, increasing the viscosity of the silicone improves the deposition of the perfume onto the treated surface. However, without wishing to be bound by theory, if the viscosity is too high, it is difficult to process and form the benefit delivery composition. A preferred silicone is AK 60000 from Wacker, Munich, Germany
Other suitable silicones are selected from an aminofunctional silicone, amino-polyether silicone, alkyloxylated silicone, cationic silicone, ethoxylated silicone, propoxylated silicone, ethoxylated/propoxylated silicone, quaternary silicone, or combinations thereof.
Suitable silicones are selected from random or blocky organosilicone polymers having the following formula:
[R1R2R3SiO1/2](j+2)[(R4Si(X—Z)O2/2]m[R4R4SiO2/2]m[R4SiO3/2]j
wherein:
with the proviso that when Z is a quat, Q cannot be an amide, imine, or urea moiety and if Q is an amide, imine, or urea moiety, then any additional Q bonded to the same nitrogen as said amide, imine, or urea moiety must be H or a C1-C6 alkyl, in one aspect, said additional Q is H; for Z An− is a suitable charge balancing anion. In one aspect An− is selected from the group consisting of Cl−, Br−, I−, methylsulfate, toluene sulfonate, carboxylate and phosphate; and at least one Q in said organosilicone is independently selected from —CH2—CH(OH)—CH2—R5;
and wherein each v in said organosilicone is an integer from 1 to about 10, in one aspect, v is an integer from 1 to about 5 and the sum of all v indices in each Q in the said organosilicone is an integer from 1 to about 30 or from 1 to about 20 or even from 1 to about 10.
In another embodiment, the silicone may be chosen from a random or blocky organosilicone polymer having the following formula:
[R1R2R3SiO1/2](j+2)[(R4Si(X—Z)O2/2]k[R4R4SiO2/2]m[R4SiO3/2]j
wherein
At least one Z in the said organosiloxane is selected from the group consisting of R5;
provided that when X is
then Z=−OR5 or
provided that when X is
then Z=—OR5 or
A suitable silicone is a blocky cationic organopolysiloxane having the formula:
MwDxTyQz
wherein:
M=[SiR1R2R3O1/2],[SiR1R2G1O1/2],[SiR1G1G2O1/2], [SiG1G2G3O1/2], or combinations thereof;
D=[SiR1R2O2/2], [SiR1G1O2/2], [SiG1G2O2/2] or combinations thereof;
T=[SiR1O3/2], [SiG1O3/2] or combinations thereof;
w=is an integer from 1 to (2+y+2z);
x=is an integer from 5 to 15,000;
y=is an integer from 0 to 98;
z=is an integer from 0 to 98;
R1, R2 and R3 are each independently selected from the group consisting of H, OH, C1-C32 alkyl, C1-C32 substituted alkyl, C5-C32 or C6-C32 aryl, C5-C32 or C6-C32 substituted aryl, C6-C32 alkylaryl, C6-C32 substituted alkylaryl, C1-C32 alkoxy, C1-C32 substituted alkoxy, C1-C32 alkylamino, and C1-C32 substituted alkylamino;
at least one of M, D, or T incorporates at least one moiety G1, G2 or G3, and G1, G2, and G3 are each independently selected from the formula:
wherein:
X comprises a divalent radical selected from the group consisting of C1-C32 alkylene, C1-C32 substituted alkylene, C5-C32 or C6-C32 arylene, C5-C32 or C6-C32 substituted arylene, C6-C32 arylalkylene, C6-C32 substituted arylalkylene, C1-C32 alkoxy, C1-C32 substituted alkoxy, C1-C32 alkyleneamino, C1-C32 substituted alkyleneamino, ring-opened epoxide, and ring-opened glycidyl, with the proviso that if X does not comprise a repeating alkylene oxide moiety then X can further comprise a heteroatom selected from the group consisting of P, N and O;
each R4 comprises identical or different monovalent radicals selected from the group consisting of H, C1-C32 alkyl, C1-C32 substituted alkyl, C5-C32 or C6-C32 aryl, C5-C32 or C6-C32 substituted aryl, C6-C32 alkylaryl, and C6-C32 substituted alkylaryl;
E comprises a divalent radical selected from the group consisting of C1-C32 alkylene, C1-C32 substituted alkylene, C5-C32 or C6-C32 arylene, C5-C32 or C6-C32 substituted arylene, C6-C32 arylalkylene, C6-C32 substituted arylalkylene, C1-C32 alkoxy, C1-C32 substituted alkoxy, C1-C32 alkyleneamino, C1-C32 substituted alkyleneamino, ring-opened epoxide and ring-opened glycidyl, with the proviso that if E does not comprise a repeating alkylene oxide moiety then E can further comprise a heteroatom selected from the group consisting of P, N, and O;
E′ comprises a divalent radical selected from the group consisting of C1-C32 alkylene, C1-C32 substituted alkylene, C5-C32 or C6-C32 arylene, C5-C32 or C6-C32 substituted arylene, C6-C32 arylalkylene, C6-C32 substituted arylalkylene, C1-C32 alkoxy, C1-C32 substituted alkoxy, C1-C32 alkyleneamino, C1-C32 substituted alkyleneamino, ring-opened epoxide and ring-opened glycidyl, with the proviso that if E′ does not comprise a repeating alkylene oxide moiety then E′ can further comprise a heteroatom selected from the group consisting of P, N, and O;
p is an integer independently selected from 1 to 50;
n is an integer independently selected from 1 or 2;
when at least one of G1, G2, or G3 is positively charged, A−t is a suitable charge balancing anion or anions such that the total charge, k, of the charge-balancing anion or anions is equal to and opposite from the net charge on the moiety G1, G2 or G3, wherein t is an integer independently selected from 1, 2, or 3; and k<(p*2/t)+1; such that the total number of cationic charges balances the total number of anionic charges in the organopolysiloxane molecule; and wherein at least one E does not comprise an ethylene moiety.
Perfume:
Suitable perfumes comprise perfume materials selected from the group: (a) perfume materials having a C log P of less than 3.0 and a boiling point of 250° C. or greater (herein: “quadrant 2 perfume materials”); (b) perfume materials having a C log P of 3.0 or greater and a boiling point of less than 250° C. (herein: “quadrant 3 perfume materials”); (c) perfume materials having a C log P of 3.0 or greater and a boiling point of 250° C. or greater (herein: “quadrant 4 perfume materials”); and (d) mixtures thereof.
Suitable perfumes comprise, based on total perfume weight, at least 60 wt %, preferably at least 80 wt %, or even at least 95 wt % perfume materials selected from quadrant 2 perfume materials, quadrant 3 perfume materials and quadrant 4 perfume materials.
Suitable perfumes comprise, based on total perfume weight, at least 50 wt %, preferably at least 70 wt %, or even at least 90 wt % perfume materials selected from, quadrant 3 perfume materials and quadrant 4 perfume materials.
It may be preferred for the perfume to be in the form of a perfume delivery technology. Such delivery technologies further stabilize and enhance the deposition and release of perfume materials from treated substrate. Such perfume delivery technologies can also be used to further increase the longevity of perfume release from the treated substrate. Suitable perfume delivery technologies are selected from the group consisting of: perfume microcapsule, pro-perfume, polymer assisted delivery, molecule assisted delivery, fiber assisted delivery, amine assisted delivery, cyclodextrin, starch encapsulated accord, zeolite and other inorganic carrier, and mixtures thereof:
A suitable perfume delivery technology is a perfume microcapsule formed by at least partially surrounding, preferably completely surrounding, the perfume with a wall material. Suitable wall materials are selected from melamine, polyacrylamide, silica, polystyrene, polyurea, polyurethanes, polyacrylate based materials, gelatin, styrene malic anhydride, polyamides, and mixtures thereof. Suitable melamine wall materials are selected from melamine crosslinked with formaldehyde, melamine-dimethoxyethanol crosslinked with formaldehyde, and mixtures thereof. Suitable perfume microcapsules may be coated with a deposition aid. Suitable deposition aids are selected from cationic polymer, non-ionic polymer, anionic polymer, and mixtures thereof. Suitable polymers are selected from the group consisting of: polyvinylformaldehyde, partially hydroxylated polyvinylformaldehyde, polyvinylamine, polyethyleneimine, ethoxylated polyethyleneimine, polyvinylalcohol, polyacrylates, cationically modified hydroxyethyl cellulose and combinations thereof.
Other Ingredients:
The benefit delivery composition may comprise other ingredients. Suitable ingredients are selected from petrolatum and/or sensate. Suitable sensates are compounds that provide a cooling, warming, tingling or refreshing sensation, either through the endothermic or exothermic processes of physical lowering or raising of temperature; or through the physiological cooling process associated with, e.g., cold menthol receptor (TRPM8), or any other receptors generally located at or near nerve endings. Suitable sensates include menthol and derivatives thereof. Suitable menthol derivatives include menthyl lactate (available under the trade name Frescolat ML from Symrise GmbH & Co., Holzminden, Germany), menthol with a carboxamide derivative, menthol with a cyclohexanecarboxamide derivative, dimethyl menthyl succinimide, menthone glycerin acetal (available under the trade name Frescolat MGA from Symrise GmbH & Co., Holzminden, Germany), menthoxypropanediol (commercially available under the trade name Coolact 10 and Coolact P (−)-isopulegol from Takasago Int'l Corp., Tokyo, Japan); neoisomenthol, neomenthol, isomenthol, PMD 38 p-menthane-3,8,-diol, (2R)-3-(1-menthoxy)propane-1,2-diol, (2RS)-3-(1-menthoxy)propane-1,2-diol; N-ethyl-p-menthane-3-carboxamide (WS-3), ethyleneglycol p-menthane-3-carboxylate (WS-4), ethyl 3-(p-menthane-3-carboxamido)acetate (WS-5), N-(4-methoxyphenyl)-p-menthane-3-carboxamide (WS-12), N-t-butyl-p-menthane-carboxamide (WS-14), 2-isopropyl-N-2,3-trimethylbutyramide (WS-23), 1-glyceryl p-menthane-3-carboxylate (WS-30) (all commercially available from Millennium Chemicals, Hunt Valley, Md., USA). Other suitable sensates include phenol derivatives, such as thymol and eugenol, Icilin (Phoenix Pharmaceuticals, Belmont, Calif., USA), 2(5H)-MPF (Nestec, Vevey, Switzerland), 4-methyl-3-(1-pyrrolidinyl)2[5H]-furanone, MPD vanillyl acetal (Takasago Int'l Corp., Tokyo, Japan) Hotact VBE (Lipo Chemicals, Inc., Paterson, N.J., USA) and capsaicin (derivative of cayenne pepper).
Application of the Benefit Delivery Composition:
The benefit delivery composition can be incorporated into a variety of consumer goods products, such as laundry detergent compositions, dish-washing detergent compositions, hard surface cleaning compositions, fabric enhancer compositions, shampoo, hair conditioners, skin creams, skin lotions, razor strips and cartridge compositions, shaving creams, foams and gels, body wash compositions, and dentifrice compositions.
The benefit delivery composition is contacted with at least three different consumer goods products ingredients to form the consumer goods product. Suitable consumer goods product ingredients are those typically found in the consumer goods product. For example, enzymes, bleach, polymers for detergent consumer goods products.
Packing Parameter:
The surfactant Packing Parameter (N), is calculated from various molecular descriptors of the surfactant molecule's chemical structure, as described in more detail below. The surfactant Packing Parameter (N) is defined as:
N=v/1a0
The volume of the hydrocarbon core of a saturated chain (v), in cubic nanometers, is determined according to the following equation:
v=0.027(nc+nMe)
The maximum length of a fully extended hydrocarbon chain (1) (in nanometers) is calculated according to the following equation:
1=0.15+0.127 nc
The 0.15 nm in this equation comes from van der Waals radius of the terminal methyl group (0.21 nm) minus half the bond length of the first atom not contained in the hydrocarbon core (0.06 nm). The 0.127 nm is the carbon-carbon bond length (0.154 nm) projected onto the direction of the chain in the all-trans configuration.
The area of the surfactant head-group at the interface of the hydrophobic core (a0), is determined according to the calculations described in the following published article: “Theory of Self-Assembly of Hydrocarbon Amphiphiles into Micelles and Bilayers” 1976, J. Chem. Soc., Faraday Trans. 2, 72, 1525-1568, Jacob N. Israelachvili, D. John Mitchell and Barry W. Ninham.
C log P:
The log P values of many perfume materials have been reported; for example, the Pomona92 database, available from Daylight Chemical Information Systems, Inc. (Daylight CIS, Irvine, Calif.), contains many, along with citations to the original literature. However, the log P values are most conveniently calculated by the “C LOG P” program, also available from Daylight CIS. The “calculated log P” (C log P) 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). The fragment approach is based on the chemical structure of each perfume ingredient, and takes into account the numbers and types of atoms, the atom connectivity, and chemical bonding.
Boiling Point:
The boiling point of perfume material is measured according to standard test method ASTM D2887-04a, “Standard Test Method for Boiling Range Distribution of Petroleum Fractions by Gas Chromatography,” (ASTM International, West Conshohocken, Pa., USA”.
Melting Point:
The Melting Point value is determined using the widely used standard Differential Scanning calorimetry methodology described in the following published article: “Comprehensive Evaluation of the Melting Points of Fatty Acids and Esters Determined by Differential Scanning calorimetry”. J. Am. Oil Chem. Soc. (2009). 86:843-856A.
pKa:
The pKa value is the negative log (base 10) of the acid dissociation constant. The acid dissociation constant, Ka, is the equilibrium constant for the acid-base dissociation reaction. The equilibrium of acid dissociation can be written symbolically as:
HAA−+H+
where HA is a generic acid that dissociates by splitting into A−, known as the conjugate base of the acid, and the hydrogen ion or proton, H. The dissociation constant is usually written as a quotient of the equilibrium concentrations (in mol/L), denoted by [HA], [A−] and [H+]:
The logarithmic constant, pKa, which is equal to −log10 Ka, is sometimes also referred to as an acid dissociation constant:
pKa=−log10Ka
HLB:
Hydrophilic-Lipophilic Balance (HLB) values are calculated according to the widely used standard methodology contained in the following published article: “The HLB System”, 1987, ICI Americas Inc., Wilmington, Del., USA.
Method for Measuring Droplet Size:
A Malvern Mastersizer 2000 (Malvern Instruments GmbH, Rigipsstr. 19 Herrenberg 71083 Germany), is used to measure the droplet size of the lamellar gel sample dispersed in filtered deionized (DI) water. The Mastersizer 2000 uses the technique of laser diffraction to measure the size of particles. It does this by measuring the intensity of light scattered as a laser beam passes through a dispersed particulate sample. The sample dispersion is prepared by dissolving 1 g of the lamellar gel sample in 0.8 L filtered deionized water at 40° C., with a mixing speed of 1500 rpm. If this concentration is not sufficient to achieve 20% obscuration in the Mastersizer instrument using the following settings, then additional sample material is added in order to achieve 20% obscuration. The change in droplet size is monitored over a period of 30 minutes. This data is then analyzed to calculate the size of the particles that created the scattering pattern, using the following two refractive indices: 1.333 (dispersant=water), and 1.469 (hydrophobic active materials), and the adsorption parameter of the system is set to 1. The average droplet size is expressed as the mean volume average diameter.
Method for Measuring Viscosity:
The viscosity is measured by the following method, which generally represents the zero-shear viscosity (or zero-rate viscosity). Viscosity measurements are made with an AR2000 Controlled-Stress Rheometer (TA Instruments, New Castle, Del., U.S.A.), and accompanying software version 5.7.0. The instrument is outfitted with a 40 mm stainless steel parallel plate (TA Instruments catalog no. 511400.901) and Peltier plate (TA Instruments catalog no. 533230.901). The calibration is done in accordance with manufacturer recommendations. A refrigerated, circulating water bath set to 25° C. is attached to the Peltier plate.
Measurements are made on the instrument with the following procedures: Conditioning Step (pre-condition the sample) under “Settings” label, initial temperature: 25° C., pre-shear at 5.0 s−1 for 1 minute, equilibrate for 2 minutes; Flow-Step (measure viscosity) under “Test” Label, Test Type: “Steady State Flow”, Ramp: “shear rate 1/s” from 0.001 s−1 and 1000 s−1, Mode: “Log”, Points per Decade: 15, Temperate: 25° C., Percentage Tolerance: 5, Consecutive with Tolerance: 3, Maximum Point Time: 45 sec, Gap set to 1000 micrometers, Stress-Sweep Step is not checked; Post-Experiment Step under “Settings” label; Set temperature: 25° C.
More than 1.25 ml of the test sample of the component to be measured is dispensed through a pipette on to the center of the Peltier plate. The 40 mm plate is slowly lowered to 1100 micrometers, and the excess sample is trimmed away from the edge of the plate with a rubber policeman trimming tool or equivalent. Lower the plate to 1000 micrometers (gap setting) prior to collecting the data.
Discard any data points collected with an applied rotor torque of less than 1 micro-N′m (e.g. discard data less than ten-fold the minimum torque specification). Create a plot of viscosity versus shear rate on a log-log scale. These plotted data points are analyzed in one of three ways to determine the viscosity value:
first, if the plot indicates that the sample is Newtonian, in that all viscosity values fall on a plateau within +/−20% of the viscosity value measured closest to 1 micro-N′m, then the viscosity is determined by fitting the ‘Newtonian’ fit model in the software to all the remaining data;
second, if the plot reveals a plateau in which the viscosity does not change by +/−20% at low shear rates and a sharp, nearly-linear decrease in viscosity in excess of the +/−20% at higher shear rates, then the viscosity is determined by applying the “Best Fit Using Viscosity vs. Rate” option from the “Analysis Toolbar”;
third, if the plot indicates that the sample is only shear-thinning, in that there is only a sharp, nearly-linear decrease in viscosity, then the material is characterized by a viscosity which is taken as the largest viscosity in the plotted data, generally a viscosity measured close to 1 micro-N·m of applied torque.
Report the average value of the replicates as the viscosity of the component, in units of Pa·s.
The following samples are prepared by the processes described below. Sample 2 is in accordance with the present invention. Sample 1 is a comparison example where the perfume and silicone are not pre-mixed prior to addition to the linear alkyl benzene sulphonate (LAS). Sample 3 is a comparison example where the fatty amphiphile (dodecanoic acid) is not melted when it is contacted to the LAS.
LAS Paste Neutralization:
72.38 g of LAS paste (45% active) is heated to 60° C. and continuously stirred at 1000 rpm in a heat resistant beaker and HCl (10 M) is added drop wise until a pH of 7.0 is obtained. The LAS paste is then stored in an oven at 50° C. tightly sealed to avoid water evaporation.
Process of Making Sample 1 (Comparison Example, No Silicone/Perfume Premix):
18.98 g dodecanoic acid is placed in a plastic container in an oven at 50° C. (above its melting point of 43.2° C.). A stirrer blade is warmed in the oven at 50° C. for at least one hour and then the blade is placed and locked in an overhead stirrer. 72.38 g LAS Paste (prepared as described above) is shaken vigourously and dosed into the overhead stirrer and 60 g silicone (PDMS) is added to the overhead stirrer and the mixture is stirred at 50° C. at 1000 rpm for 5 minutes. 18.98 g molten dodecanoic acid (prepared as described above) is added and the mixture stirred at 50° C., 350 rpm for 5 minutes to form a gel. 0.196 g sodium carbonate and 0.160 g sodium bicarbonate are added to 37.284 g deionized water and mixed to form a buffer. 37.64 g buffer is heated to 50° C. and then added to the gel (prepared as described above) and stirred for 5 minutes at 350 rpm. The gel is then cooled to room temperature. 10 g perfume is then added to the gel and the gel is stirred at room temperature for 15 minutes at 350 RPM.
Process of Making Sample 2 (in Accordance with the Present Invention):
18.98 g dodecanoic acid is placed in a plastic container in an oven at 50° C. (above its melting point of 43.2° C.). A stirrer blade is warmed in the oven at 50° C. for at least one hour and then the blade is placed and locked in an overhead stirrer. 72.38 g LAS Paste (prepared as described above) is shaken vigourously and dosed into the overhead stirrer. 18.98 g molten dodecanoic acid (prepared as described above) is added to the overhead stirrer and the mixture is stirred at 50° C., 350 rpm for 5 minutes to form a gel. 0.196 g sodium carbonate and 0.160 g sodium bicarbonate are added to 37.284 g deionized water and mixed to form a buffer. 37.64 g buffer is heated to 50° C. and added to the gel (prepared as described above) and stirred for 5 minutes at 350 rpm. The gel is then cooled to room temperature. 60 g silicone (PDMS) and 10 g perfume are mixed in a high speed mixer (Siemens Speed Mixer DAC150 FVZK) at 2700 rpm for 3 minutes to form a premix. The premix is then added to the gel (prepared as described above) and the gel is stirred at room temperature for 15 minutes at 350 RPM.
Process of Making Sample 3 (Comparison Example, Fatty Amphiphile not Melted):
18.98 g dodecanoic acid is placed in a plastic container at room temperature (20° C.). A stirrer blade at room temperature is placed and locked in an overhead stirrer. 72.38 g LAS Paste (prepared as described above) is cooled to room temperature, shaken vigorously, and dosed into the overhead stirrer. 18.98 g dodecanoic acid (prepared as described above) is added to the overhead stirrer and the mixture is stirred at room temperature, 350 rpm for 5 minutes to form a gel. 0.196 g sodium carbonate and 0.160 g sodium bicarbonate are added to 37.284 g deionized water and mixed to form a buffer. 37.64 g buffer is then added to the gel (prepared as described above) at room temperature and stirred for 5 minutes at 350 rpm. 60 g silicone (PDMS) and 10 g perfume are mixed in a high speed mixer (Siemens Speed Mixer DAC150FVZK) at 2700 rpm for 3 minutes to form a premix. The premix is then added to the gel (prepared as described above) and the gel is stirred at room temperature for 15 minutes at 350 RPM.
Test Protocol:
Each of the above described samples 1, 2 and 3 were tested for softening, freshness and spotting performance on fabric using the following test protocol.
The samples were added into a mini washing system along with a laundry detergent (Ariel UK unscented laundry powder). The mini washing system is a 8 L water volume mini replica of a top loading automatic washing machine. The hardness of the water used was 8 gpg (54.88 mg calcium/L).
The following fabrics are added into mini-washer pots: 3× Christy Softness Swatches 20 cm×20 cm; 2×1/8th Tonrose Towel 6.25 cm×12.5 cm; 1× Asda Poly-cotton Sheet 25 cm×25 cm. These fabrics are supplied by Asda Stores Ltd., Leeds, UK or Optima Cotton Wear 8050 East Crystal Drive, Anaheim, Calif. 92807. The loaded mini-washer pots are agitated for 30 seconds and 60 g laundry detergent (Ariel unscented laundry powder, UK) and 2.3 g sample are then added to the miniwasher pot. A reference leg of 60 g unscented laundry detergent (Ariel unscented laundry powder UK) and 0.12 g perfume oil was also placed in one of the mini-washer pots. The mini-washer then performed a 12 min wash cycle, 2 min spin cycle, 2 min rinse cycle and a further 2 min spin cycle. The treated fabric are dried at 21° C., 55% relative humidity for 15 hours. The fabrics are then graded to assess the fabric's softness, freshness and spotting characteristics.
Softeness Paneling:
Panel grading is used to assess the softness characteristics. The panelists are trained and calibrated and panel the fabrics versus the reference fabric using the following panel score units (PSU) where −4 is described as significantly very poor versus reference, −3 is poor versus reference, −2 is slightly poor versus reference, −1 is unsure about negative difference versus reference, 0 is no difference versus reference, +1 is unsure about positive difference versus reference, +2 is slightly better versus reference, +3 is suprerior verus reference and +4 is significantly superior versus reference. Four replica fabrics are prepared for each sample, and each fabric is paneled once by three different panelists and the average panel score is calculated.
Spotting Performance:
Spotting performance is evaluated by counting the number of oily spots visibly observed per cm2 on the polycotton fabrics. Two replica fabrics are prepared for each sample, and each fabric is evaluated by one panelist.
Freshness Performance:
Panel grading is used to assess the freshness characteristics. The panelists are trained and calibrated and panel the fabrics versus the reference fabric using the following primavera scale where +2.5 indicates a meaningful but not consumer noticeable positive difference versus reference, +5.0 indicates a meaningful and consumer noticeable positive difference versus reference, and +7.5 indicates a meaningful and highly consumer noticeable positive difference versus reference. A difference of 2.5 is considered to be a technical difference on the primavera scale. Four replica fabrics are prepared for each sample, and each fabric is paneled by two different panelists.
Sample 2 (in accordance with the present invention) has superior softeness performance and freshness performance, and showed the least amount of spotting compared to the comparison example samples 1 and 3.
Sample 1 can be used as a liquid fabric enhancer composition
1 Mirapol AT-1, Copolymer of Acrylamide(AM) and TRIQUAT, MW = 1,000,000; CD = 1.6 meq./gram; 10% active; Supplier Rhodia
2 Jaguar C500, MW—500,000, CD = 0.7, supplier Rhodia
3 Mirapol 100S, 31.5% active, supplier Rhodia
4 Sodium Laureth Sulfate, 28% active, supplier: P&G
5 Sodium Lauryl Sulfate, 29% active supplier: P&
6 Tegobetaine F-B, 30% active supplier: Goldschmidt Chemicals
7 Monamid CMA, 85% active, supplier Goldschmidt Chemical
8 Ethylene Glycol Distearate, EGDS Pure, supplier Goldschmidt Chemical
9 Sodium Chloride USP (food grade), supplier Morton; note that salt is an adjustable ingredient, higher or lower levels may be added to achieve target viscosity.
1 Jeenate ™ 3H polyethylene wax from Jeen ™
2 Stearyl Dimethicone. Available from Dow Corning.
3 Hexamidine diisethionate, available from Laboratoires Serobiologiques.
4 Additionally or alternatively, the composition may comprise one or more other skin care actives, their salts and derivatives, as disclosed herein, in amounts also disclosed herein as would be deemed suitable by one of skill in the art.
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”.
Every document cited herein, including any cross referenced or related patent or application and any patent application or patent to which this application claims priority or benefit thereof, is hereby incorporated herein by reference in its entirety unless expressly excluded or otherwise limited. The citation of any document is not an admission that it is prior art with respect to any invention disclosed or claimed herein or that it alone, or in any combination with any other reference or references, teaches, suggests or discloses any such invention. Further, 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.
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.
| Number | Date | Country | Kind |
|---|---|---|---|
| 14197591.2 | Dec 2014 | EP | regional |
