SILICONE POLYMER EMULSIONS
20180237720 ยท 2018-08-23
Inventors
- Kathleen Barnes (Midland, MI, US)
- Jary David JENSEN (Beaverton, MI, US)
- Walker L. ROCHLITZ (Midland, MI, US)
- Andreas STAMMER (Pont-a Celles, BE)
Cpc classification
A61K8/891
HUMAN NECESSITIES
International classification
A61K8/891
HUMAN NECESSITIES
Abstract
Silicone oil-in-water emulsions containing a polysiloxane containing polymer is prepared by first preparing a polysiloxane containing polymer by the polymerisation of siloxane containing monomers and/or oligomers in the presence of an inert organopoly siloxane and/or an organic fluid, a suitable catalyst and optionally an end-blocking agent; and quenching the reaction if required. If required one or more surfactants may be introduced into the polysiloxane containing polymer to form a homogenous oil phase. Water is then added (in an amount of 0.1-10 percent by weight based on total oil phase weight) to the homogenous oil phase to form a water-in-oil emulsion. Shear is applied to the water-in-oil emulsion to cause inversion of the water-in-oil emulsion to an oil-in-water emulsion. Finally, if required the oil-in-water emulsion can be diluted by adding more water.
Claims
1-15. (canceled)
16. A silicone oil-in-water emulsion comprising: an inert organopolysiloxane and/or an organic fluid; and a polysiloxane containing polymer comprising the reaction product of siloxane containing monomers and/or oligomers in the presence of a catalyst and the inert fluid; wherein the polysiloxane containing polymer is of the following general formula
R.sub.(3-a)R.sup.1.sub.aSiO[(R.sub.2SiO).sub.b(RR.sup.1SiO).sub.c]SiR.sub.(3-a)R.sup.1.sub.a(1) wherein each R is the same or different and is an alkyl group containing 1 to 8 carbon atoms, a substituted alkyl group containing 1 to 6 carbon atoms, or a phenyl group; R.sup.1 is a hydroxy group, a hydrolysable group, or an unsaturated organic group; a is zero or 1; b is an integer; c is zero or an integer; and the sum of b+c is equal to a value of at least 200.
17. The emulsion according to claim 16, wherein the sum of b+c is equal to a value of at least 500, optionally is equal to a value of at least 1500.
18. The emulsion according to claim 16, wherein the inert fluid is retained within the polysiloxane containing polymer in an amount of not more than 70% w/w.
19. The emulsion according to claim 18, wherein the inert fluid is retained within the polysiloxane containing polymer in an amount of from 5 to 70% w/w.
20. The emulsion according to claim 16, wherein the polysiloxane containing polymer comprises a degree of branching of less than 10%, optionally a degree of branching of less than 2%.
21. The emulsion according to claim 16, wherein the inert fluid is selected from the group of an organic extender, a plasticizer, a natural oil, and combinations thereof.
22. The emulsion according to claim 16, wherein the inert fluid is a cyclic siloxane comprising between 3 to 20 silicon atoms.
23. The emulsion according to claim 22, wherein the polysiloxane containing polymer is a polydimethyl gum.
24. The emulsion according to claim 16, wherein the inert fluid is a trialkylsilyl terminated polydialkylsiloxane or a derivative thereof, and optionally has a viscosity of from 0.65 to 10000 mPa.Math.s at 25 C.
25. The emulsion according to claim 16, wherein the polysiloxane containing polymer is prepared via a reaction process selected from the group of polycondensation, chain extension, polyaddition, and ring opening.
26. The emulsion according to claim 16, further comprising a surfactant, and optionally wherein the catalyst is part of the surfactant.
27. The emulsion according to claim 26, wherein the polysiloxane containing polymer is prepared via a polycondensation reaction and the catalyst is dodecylbenzenesulphonic acid.
28. The emulsion according to claim 16, wherein a homogenous oil phase is from 1000 to 100000 mPa.Math.s at 25 C.
29. The emulsion according to claim 16, prepared by a method comprising the steps of: (i) preparing the polysiloxane containing polymer by the polymerization of siloxane containing monomers and/or oligomers in the presence of the inert fluid and catalyst and optionally an end-blocking agent; (ii) optionally quenching the polymerization process; wherein the inert fluid is retained within the resulting polysiloxane containing polymer; (iii) optionally introducing one or more surfactants into the polysiloxane containing polymer to form a homogenous oil phase; (iv) adding water to the homogenous oil phase to form a water-in-oil emulsion, the water being added in an amount of 0.1 to 10 percent by weight based on the total oil phase weight; (v) applying shear to the water-in-oil emulsion to cause inversion of the water-in-oil emulsion to an oil-in-water emulsion; and (vi) optionally diluting the oil-in-water emulsion by adding more water.
30. The emulsion according to claim 29, wherein the sum of b+c is equal to a value of at least 500, optionally at least 1500.
31. The emulsion of claim 29, wherein the inert fluid is retained within the polysiloxane containing polymer in an amount of not more than 70% w/w, optionally in an amount of from 5 to 70% w/w.
32. The emulsion according to claim 29, wherein the inert fluid has a viscosity of from 0.65 mPa.Math.s to 10000 mPa.Math.s at 25 C. and is selected from an organopolysiloxane extender or plasticizer, an organic extender or plasticizer, or a cyclic siloxane comprising between 3 and 20 silicon atoms.
33. The emulsion according to claim 29, wherein the siloxane containing monomers and/or oligomers comprise hydroxyl-terminated organopolysiloxanes.
34. A personal care product comprising the emulsion according to claim 16.
35. The emulsion according to claim 16 in paints, construction applications, textile fibre treatments, leather lubrication, fabric softening, fabric care for laundry applications, healthcare, homecare, personal care, release agents, water based coatings, oil drag reduction, lubrication, and facilitation of cutting cellulose materials.
Description
EXAMPLES
[0150] The following Examples are provided so that one skilled in the art will more readily understand the invention. Unless otherwise indicated, all parts and percents are by weight and all viscosities are at 25 C. Viscosity measurements of the polymer products were carried out using a Brookfield Viscometer, spindle 6, 10 rpm. All Particle size values were determined using a Malvern Mastersizer 2000.
Example 1
[0151] A polymer was prepared by polymerising 80 g of dimethyl hydroxyl terminated polydimethylsiloxane having 71 mPa.Math.s at 25 C. in 80 g of trimethylsilyl terminated polydimethylsiloxane (PDMS) having a viscosity of 100 mPa.Math.s at 25 C. using 2.4 g of dodecylbenzenesulphonic acid (DBSA) as catalyst for the condensation reaction. The polymerisation was stopped once a viscosity of 10500 mPa.Math.s at 25 C. was reached by the addition of 1.12 g of Triethanolamine (TEA).
[0152] To 36 g of the above polymer the following surfactants were added, 1.1 g Brij 30 and 1.9 g Brij 35 L. These were added and mixed for 30 s at 3000 rpm in Hausschild dental mixer. 1.2 g water was added and mixing was repeated for 30 s at 3000 rpm. Another 0.4 g water was added and the mixing was repeated again under the same conditions. After the second water addition the mixture had phase inverted and was diluted to a polymer content of 60%. The so obtained emulsion has a particle size of D(v, 0.5) m=0.81 and D(v, 0.9) m=1.14. The emulsion remained intact for a period of at least 6 months.
[0153] Brij 30/Brij 35 L are non-ionic polyoxyethylene fatty ether (POE) surfactants. Brij 30 is POE(4) lauryl ether with a hydrophile-lipophile balance (HLB) of 9.7. Brij 35 L is a POE (23) lauryl ether with an HLB of 16.9.
Example 2
[0154] A polymer was prepared polymerising 128 g of dimethyl hydroxyl terminated polydimethylsiloxane having a viscosity of 71 mPa.Math.s at 25 C. in 32 g of PDMS having a viscosity of 100 mPa.Math.s at 25 C. using 5.12 g of DBSA as the condensation catalyst. The polymerisation was stopped, once a viscosity of 171000 mPa.Math.s at 25 C. was reached, by the addition of 2.39 g of TEA.
[0155] To 36 g of the above polymer the following surfactants were added, 1.1 g Brij 30 and 1.9 g Brij 35 L. These were added and mixed for 30 s at 3000 rpm in Hausschild dental mixer. 0.5 g water was added mixing was repeated for 30 s at 3000 rpm. After mixing the mixture had phase inverted and was diluted to a polymer content of 60%. The so obtained emulsion has a particle size of D(v, 0.5) m=1.77 and D(v, 0.9) m=4.28. The emulsion remained intact for a period of at least 6 months.
Example 3
[0156] A polymer was prepared polymerising 128 g of dimethyl hydroxyl terminated polydimethylsiloxane polydimethylsiloxane having a viscosity of 71 mPa.Math.s at 25 C. in 32 g of PDMS 100 mPa.Math.s at 25 C. using 4.48 g of DBSA. The polymerisation was stopped once a viscosity of 171000 mPa.Math.s at 25 C. was reached by the addition of 2.09 g of TEA.
[0157] To 36 g of the above polymer the following two surfactants were added: 1.3 g Brij 30 and 2.4 g Brij 35 L. The surfactants and polymer were mixed for 30 s at 3000 rpm in Hausschild dental mixer. After mixing the mixture had phase inverted and was diluted to a polymer content of 60%. The so obtained emulsion has a particle size of D(v, 0.5) m=2.07 and D(v, 0.9) m=2.58. The emulsion remained intact for a period of at least 6 months.
Example 4
[0158] To 36 g of the polymer prepared in example 3, were added the following surfactants, 2.25 g of Arquad 16-29 Arquad 16-29 (Akzo Nobel) and 2.25 g TergitolTMN-6 (Dow Chemical). No additional water was introduced as Arquad 16-29 contains 70% by weight of water and 2.25 g TMN-6 contains 10% by weight of water. These were added and mixed for 30 s at 3000 rpm in Hausschild dental mixer. After mixing the mixture had phase inverted and was diluted to a polymer content of 60%. The so obtained emulsion has a particle size of D(v, 0.5) m=1.23 and D(v, 0.9) m=1.7. The emulsion remained intact for a period of at least 6 months.
Example 5
[0159] To 36 g of the polymer prepared in example 3 the following surfactants were added, 2.25 g Arquad 16-29 and 2.25 g TMN-6 together with 0.5 g water. These were mixed for 30 s at 3000 rpm in Hausschild dental mixer. After mixing the mixture had phase inverted and was diluted to a polymer content of 60%. The so obtained emulsion has a particle size of D(v, 0.5) m=1.28 and D(v, 0.9) m=1.96.
[0160] Arquad 16-29 is a cationic quaternary surfactant. TMN-6 is a non-ionic ethoxylated alcohol with an HLB=13.1
Example 6
[0161] To 36 g of the polymer prepared in example 3 the following surfactants were added, 1 g Biosoft N300 and 2 g Brij 30 (No additional water added). The surfactants were mixed with the polymer for 30 s at 3000 rpm in Hausschild dental mixer. After mixing the mixture had phase inverted and was diluted to a polymer content of 60%. The so obtained emulsion has a particle size of D(v, 0.5) m=2.14 and D(v, 0.9) m=3.14
Example 7
[0162] A polymer was prepared polymerising a 1 to 1 mixture of dimethyl hydroxyl terminated polydimethylsiloxane having a viscosity of 70 mPa.Math.s at 25 C. and of an organic extender (Hydroseal G 250H (sold by Total) using 2.4% of DBSA as a catalyst. The polymerisation was stopped, by the addition of 1.54% of TEA, once a viscosity of 40000 mPa.Math.s at 25 C. was reached.
[0163] To 40 g of the above polymer 1 g water was added and mixed for 30 s at 3000 rpm in a Hausschild dental mixer. After mixing the mixture had phase inverted. Additional 9 g water were added and mixing repeated under the same conditions. The mixture was then diluted to a polymer content of 40%. The so obtained emulsion has a particle size of D(v, 0.5) m=1.46 and D(v, 0.9) m=2.22
[0164] In this example no additional surfactant was required because the condensation catalyst DBSA used in the preparation of the polymer functioned as the required surfactant.
Example 8
[0165] 40 g of the polymer prepared in example 7 and 1 g water where mixed for 30 s at 3000 rpm in Hausschild dental mixer. After mixing the mixture had phase inverted. An additional 1 g water was then added and mixing repeated under the same conditions. The mixture was then diluted to a polymer content of 50%. The so obtained emulsion has a particle size of D(v, 0.5) m=1.75 and D(v, 0.9) m=2.76
[0166] In this example no additional surfactant was required because the condensation catalyst DBSA used in the preparation of the polymer functioned as the required surfactant.
Example 9
[0167] A polymer was prepared by polymerising a 1:1 mixture of dimethyl hydroxyl terminated polydimethylsiloxane having a viscosity of 70 mPa.Math.s at 25 C. and of decamethylcyclopentasiloxane which has a viscosity of 3.8 mPa.Math.s at 25 C. using 2.4% of DBSA as a catalyst. The polymerisation was stopped once a viscosity of 27000 mPa.Math.s at 25 C. was reached by the addition of 1.54% of TEA. In this case the DBSA catalyst used in the polymerisation step above additionally functioned as the surfactant in the preparation of emulsions as described below.
[0168] 0.3 g water was added to 36 g of the above polymer and mixed for 30 s at 3000 rpm in a Hausschild dental mixer. Another 0.9 g water were subsequently added and mixed under the same conditions. After mixing the mixture had phase inverted. A further 1.9 g of water was then added and mixing repeated under the same conditions. The resulting mixture was then diluted to a polymer content of 50%. The resulting emulsion has a particle size of D(v, 0.5) m=1.46 and D(v, 0.9) m=2.34.
Example 10
[0169] A polymer was prepared by polymerising a 4:1 mixture of dimethyl hydroxyl terminated polydimethylsiloxane having a viscosity of 70 mPa.Math.s at 25 C. in an organic extender (Hydroseal G 250H) using 2.4% g of DBSA as a catalyst. The polymerisation was stopped once a viscosity of 40000 mPa.Math.s at 25 C. was reached by the addition of 1.54% g of TEA.
[0170] 1 g water was added to 40.2 g of the above polymer and mixed for 30 s at 3000 rpm in a Hausschild dental mixer. After mixing the mixture had phase inverted. An additional 1.1 g of water was added and mixing repeated under the same conditions. The resulting mixture was then diluted to a polymer content of 50%. The so obtained emulsion has a particle size of D(v, 0.5) m=1.46 and D(v, 0.9) m=2.26.
Example 11
[0171] 1.1 g water was added and mixed with 40.2 g of the polymer prepared in Example 10 for 30 s at 3000 rpm in a Hausschild dental mixer. After mixing the resulting mixture had phase inverted. An additional 1.4 g of water was added and mixing repeated under the same conditions. A still further 2.5 g of water was subsequently added and mixing repeated under the same conditions. The resulting mixture was then diluted to a polymer content of 80%. The resulting viscous cream (emulsion) had a particle size of D(v, 0.5) m=1.26 and D(v, 0.9) m=1.84.
Example 12
[0172] A polymer was prepared by polymerising a 1:1 mixture of dimethyl hydroxyl terminated polydimethylsiloxane having a viscosity of 70 mPa.Math.s at 25 C. in cosmetic grade organic fluid (Isopar M, sold by Exxon) using 20 parts per million (ppm) of a phosphonitrile catalyst. The polymerisation was stopped once a viscosity of 51000 mPa.Math.s at 25 C. was reached by the addition of trihexylamine. The polymer had a number average molecular weight of 198000 g/mol and a polydispersity index of 1.54.
[0173] 1.1 g Volpo L3, 1.6 g Volpo L23 and 1.1 g water was added to 50.2 g of the polymer prepared as described above and the resulting mixture was mixed for 60 s at 3000 rpm in a Hausschild dental mixer. An additional 1.0 g of water was added and mixing repeated under the same conditions. A still further 1.0 g of water was added and the same mixing process was repeated again. After mixing the resulting mixture had phase inverted. Further 2.2 g of water was subsequently added and mixing repeated under the same conditions. The resulting mixture was then diluted to a polymer/fluid content of 50%. The resulting emulsion had a particle size of D(v, 0.1) m=1.23, D(v, 0.5) m=2.67 and D(v, 0.9) m=5.01 and henceforth is referred to as sample 12.1 emulsion.
[0174] The resulting emulsion was introduced into a selection of personal care formulations, including fruity gel blushers, eye shadow, water in oil skin creams, hair care conditioners, leave-on and the following:
Cold Mix Lotion
[0175] This lotion was prepared with the ingredients depicted in Table 12(a) below by initially mixing the phase B ingredients together and then introducing phase A into the phase B and then mixing the resulting product until it is homogeneous.
TABLE-US-00001 TABLE 12(A) Ingredients INCI Name % Phase A Sample 12.1 emulsion 20 Phase B Water 78 Phenochem Phenoxyethanol (and) Methylparaben (and) 1 Butylparaben (and) Ethylparaben (and) Propylparaben (and) Isobutylparaben Keltrol Xanthan Gum 1
It was found that the sample 12.1 emulsion could be easily incorporated in a lotion type product and the resulting lotion was found to have a significant impact on sensory profile, in upon testing using 18 panelists. Significant differences in >95% of results was found for speed of absorption, gloss, film residue, greasiness. This indicates that sample 12.1 emulsion could significantly impact the sensory of lotion prepared as described herein, making it richer and more nourishing.
Water in Silicone Skin Cream
[0176] The above was prepared using the ingredients identified in Table 12(b) below:
TABLE-US-00002 TABLE 12(B) Ingredients INCI Name % Phase A Dow Corning5225C Cyclopentasiloxane (and) 10 Formulation Aid PEG/PPG-18/18 Dimethicone Dow Corning245 Cyclopentasiloxane 18.6 Fluid Phase B Sample 12.1 emulsion 2.3 Sodium Chloride 2 Water 67.1 Viscosity: Spindle 7, 20 rpm 11800 mPa .Math. s
[0177] The ingredients of phase A were mixed together. The ingredients of phase B were mixed together. Phase B was then introduced dropwise into the phase A mixture whilst continuously agitation the resulting mixture and finally the resulting mixture was homogenized using a high shear mixer.
[0178] Sensory tests were carried out using 18 panelists to determine the performance of the resulting cream as described above, containing 2.3% by weight of Sample 12.1 emulsion in comparison to an identical cream in the absence of the sample 12.1 emulsion. Significant differences >95% were identified with respect to speed of absorption, gloss, film residue and greasiness demonstrating that the presence of Sample 12.1 emulsion at levels as low as 2.3% impact significantly the sensory of the cream making it richer and more nourishing.
Opaque Shampoo
[0179] The above was prepared using the ingredients identified in Table 12(c) below:
TABLE-US-00003 TABLE 12(C) Ingredients INCI Name % Phase A Water 60.5 Crothix liquid PEG-150 Pentaerythrityl 1.5 Tetrastearate and PEG-6 Caprylic/Capric Glycerides and Water Empicol ESB-3 Sodium Laureth Sulfate 12 Texapon A 400 Ammonium Lauryl Sulfate 10 Amonyl 380BA Cocamidopropyl Betaine 8 Comperlan KD Cocamide DEA 4 Phase B Sample 12.1 emulsion 4 Phase C Citric Acid q.s Nipaguard DMDMH DMDM Hydantoin q.s Viscosity: Spindle 7, 20 rpm 41600 mPa .Math. s
[0180] Water was heated to 70 C. The ingredients of phase A were mixed together. Phase B was inter-mixed with phase A with gentle mixing and then phase C was introduced and the resulting composition was allowed to cool.
[0181] Several panelists were asked to comb slightly bleached hair tresses washed with the resulting shampoo. The time to wet detangle the hair tresses was measured. As a direct comparison the panelists also undertook the same process with slightly bleached hair tresses using the same shampoo formulation without any emulsion. The results indicate a slight decrease in the detangling time with the shampoo containing the sample 12.1 emulsion. This indicates an improvement in the conditioning effect in the shampoo when the emulsions in accordance with the present invention were present.
Example 13
[0182] A range of polymers Examples 13(a) to 13(i) were prepared by polymerising mixtures of dimethyl hydroxyl terminated polydimethylsiloxane having a viscosity of 70 mPa.Math.s at 25 C. and sunflower seed oil using DBSA as a catalyst (as indicated in Table 13(a). All ingredients were mixed at 1500 rpm for 30 s (Hausschild dental mixer). The polymerisation was stopped after different times by adding TEA and mixing again under the same conditions.
TABLE-US-00004 TABLE 13A Example a b c d e f g h I Silox- 45 45 45 40 40 40 35 35 35 ane (g) Sun- 5 5 5 10 10 10 15 15 15 flower Oil (g) DBSA 1.5 2 2.5 1.5 2 2.5 1.5 2 2.5 (g) TEA (g) 0.94 1.25 1.56 0.94 1.25 1.56 0.94 1.25 1.56 Re- 35 31 20 34 29 21 33 29 21 action time (min)
[0183] Subsequent to completion of polymerisation, emulsions were prepared using the following process:
Firstly 1 g water was directly added to the polymerisation product and the resulting mixture was mixed at 3000 rpm for 60 s. The water addition step was repeated was repeated with 1 g water added and mixed at 3000 rpm for 60 s, then, a further 8 g of water was added and mixed at 3000 rpm for 60 s and finally 40 g of water was added and mixed at 1500 m for 30 s.
[0184] The resulting emulsions were analysed for Molecular weight (obtained by GPC) and cyclic siloxane content (D.sub.4-D.sub.12) by gas chromatography. The results are provided in Table 13(b) below
TABLE-US-00005 TABLE 13(B) Example a b c d e f g h i D(v, 0.1) 0.5 0.33 0.6 0.53 0.36 0.26 0.21 0.22 0.23 Mm D(v, 0.5) 0.77 2.49 0.99 0.94 1.14 1.7 0.77 1.09 1.67 Mm D(v, 0.9) 1.05 6.11 1.61 1.48 1.91 3.8 1.91 2.39 4.01 Mm Mn 82 158 229 98 162 211 129 174 205 kg/mol Mw 112 220 312 142 229 296 183 252 300 kg/mol D.sub.4 (%) 0.06 0.09 0.09 0.07 0.07 0.07 0.05 0.06 0.06 D.sub.5 (%) 0.04 0.06 0.06 0.05 0.05 0.05 0.04 0.04 0.04 D.sub.6 (%) 0.05 0.07 0.06 0.06 0.06 0.05 0.05 0.05 0.05 D.sub.7 (%) 0.06 0.07 0.06 0.07 0.07 0.06 0.06 0.06 0.05 D.sub.8 (%) 0.05 0.07 0.05 0.06 0.06 0.05 0.05 0.05 0.04 D.sub.9 (%) 0.05 0.06 0.05 0.06 0.05 0.05 0.05 0.05 0.04 D.sub.10 (%) 0.04 0.05 0.04 0.05 0.05 0.04 0.05 0.05 0.04 D.sub.11 (%) 0.04 0.05 0.03 0.04 0.04 0.04 0.04 0.04 0.03 D.sub.12 (%) 0.04 0.05 0.04 0.04 0.04 0.04 0.04 0.04 0.04
[0185] The resulting emulsions prepared in accordance with the above and identified as Example 13b, Example 13e and Example 13h were introduced into a selection of personal care formulations, including fruity gel blushers, water in oil and water in silicone skin creams, hair care shampoo, leave-on, and the following:
Ethnic Hair Care: Conditioner
[0186] The above was prepared using the ingredients identified in Table 13(c) below:
TABLE-US-00006 TABLE 13(C) Ingredients INCI Name % Phase A Water 79.47 Natrosol 250 HHR Hydroxyethylcellulose 1.5 Arquad 16-29 Cetrimonium Chloride 0.7 Phase B Lanette Wax O Cetearyl Alcohol 4 Arlacel 165 Glyceryl Stearate and PEG-100 1 Stearate Phase C Propylene Glycol 4 Glycerin 4 Phase D Gluadin W20 Hydrolyzed Wheat Protein 1 Germaben II Propylene Glycol and 1 Diazolidinyl Urea and Methylparaben and Propylparaben Phase E Example 13e Emulsion 3.33 Viscosity: Spindle 7, 20 rpm 45200 mPa .Math. s
[0187] The ingredients of phase A were mixed together and then heated to 75 C. Phase B was then added whilst mixing and the mixture was allowed to commence cooling. Phase C was then introduced and the resulting mixture was allowed to cool to 50 C. Phase D was then added and the mixture was cooled to room temperature. Phase E was then added and finally water was introduced to compensate for water loss during heating phase.
[0188] Several panelists were asked to comb slightly bleached hair tresses washed with the resulting conditioner to determine the time taken to detangle the wet hair. In comparison the participants had to comb slightly bleached hair tresses which had been washed with the same conditioner formulation without any emulsion. The results indicate a significant decrease (>99%) into the detangling time when using the conditioner containing example 13e emulsion indicating a positive impact on hair conditioning.
Shower Gel
[0189] The above was prepared using the ingredients identified in Table 13(d) below:
TABLE-US-00007 TABLE 13(D) Ingredients INCI Name % Phase A Empicol ESB-3 Sodium Laureth Sulfate 30 Oramix NS10 Decyl Glucoside 5 Amonyl 380BA Cocamidopropyl Betaine 10 Brij 30 Laureth-4 2 Sepigel 305 Polyacrylamide and C13-14 2 Isoparaffin and Laureth-7 Water 42.7 Phase B Example 13e Emulsion 8.3 Phase C Sodium Chloride q.s Viscosity: Spindle 5, 100 rpm 4000 mPa .Math. s
[0190] The ingredients of phase A were initially mixed until homogeneous, after which phase B was introduced whilst mixing was continued. Phase C was then introduced to adjust the viscosity of the final mixture to the required value. It was found that emulsions in accordance with the present invention, such as example 13e emulsion, can be easily added to shower gel formulations and provide stable formulations.
Smooth Stay Shadow (Eye Make-Up)
[0191] The above was prepared using the ingredients identified in Table 13(e) below:
TABLE-US-00008 TABLE 13(E) Ingredients INCI Name % Phase A Glycerin 8 Propylene Glycol 8 Phase B Covacryl RH Sodium Polyacrylate 0.7 Phase C Water 42 Nipaguard DMDMH DMDM Hydantoin 0.3 Phase D Example 13b Emulsion 6 Covacryl E14 Acrylates Copolymer 20 Phase E Covapearl light brown 830 AS Mica and CI 77491 and 4 Triethoxycaprylysilane Covapearl satin 931 AS Mica and CI 77891 and 11 Triethoxycaprylysilane
[0192] Phase B was first dispersed in phase A. The resulting mixture of Phases A and B were then mixed into phase C under agitation. Phase D was then added to the mixture and was mixed until homogeneous. Finally phase E was added and the final formulation was mixed until homogeneous.
[0193] It was found that that emulsions such as Example 13b emulsion as hereinbefore described can be easily incorporated into a eye shadow formulations with high pigment levels. 18 panelists compared the eye shadow formulation with example 13b emulsion in comparison with the same formulation in the absence of said emulsion. It was identified that the formulation containing Example 13b emulsion increased the tackiness of the formulation without significantly impacting the gloss and spreadability of the formulation thereby improving adhesion and retention of the formulation on the skin.
SkinshieldWater in Oil Skin Cream
[0194] The above was prepared using the ingredients identified in Table 13(f) below:
TABLE-US-00009 TABLE 13(F) Ingredients INCI Name % Phase A Dow Corning5200 Formulation Lauryl PEG/PPG-18/18 Methicone 2 Aid Mineral Oil 8 Dow Corning2-1184 Fluid Trisiloxane and Dimethicone 4.5 Dow Corning9040 Silicone Cyclopentasiloxane and Dimethicone 5 Elastomemr Blend Crosspolymer Escalol 557 Ethylhexyl Methoxycinnamate 2 Dekaben (as sold by Jan Dekker Phenoxyethanol and Methylparaben and 0.5 company) Ethylparaben and Propylparaben and Butylparaben Phase B Water 61.94 Sodium Chloride 1 Propylene Glycol 5 Glycofilm Biosaccharide Gum-4 5 Example 13h Emulsion 5 Phase C D&C Red 28 (0.5% in water) D&C red 28/LCW 0.06 Viscosity: Spindle 7, 20 rpm 27400 mPa .Math. s
[0195] The ingredients of phase A were mixed until homogeneous. The phase B ingredients were then mixed together with sufficient agitation to obtain a homogeneous mixture. Phase C was then introduced into phase B whilst mixing was continued and then the phases B and C mixture was introduced into phase A whilst mixing. After the complete addition mixing was continued for a further 15 minutes
Cold Mix Lotion
[0196] The above was prepared using the ingredients identified in Table 13(g) below:
TABLE-US-00010 TABLE 13(G) Ingredients INCI Name % % Phase A Example 13h Emulsion 20 Phase B Water 78 78 Phenochem Phenoxyethanol (and) Methylparaben 1 1 (and) Butylparaben (and) Ethylparaben (and) Propylparaben (and) Isobutylparaben Keltrol Xanthan Gum 1 1
[0197] The ingredients of phase B were initially mixed together and then the resulting mixture was introduced into phase A and was mixed until homogeneous.
Example 14
[0198] A polymer was prepared by polymerising a 1:1 mixture of dimethyl hydroxyl terminated polydimethylsiloxane having a viscosity of 70 mPa.Math.s at 25 C. and an organic extender (Hydroseal G 250H) using 20 ppm of a phosphonitrile catalyst. The polymerisation was stopped once a viscosity of 100000 mPa.Math.s at 25 C. was reached by the addition of trihexylamine. The polymer had a number average molecular weight of 235000 g/mol and a polydispersity index of 1.48.
[0199] 1.75 g Volpo L4, 1.25 g and Volpo L23 was added to 30 g of the polymer/extender blend described above and mixed for 20 s at 3000 rpm in a Hausschild dental mixer. An additional 2.0 g of water was added and mixing repeated under the same conditions. Further additions of 2.0 g of water were repeated four more times. The resulting mixture was then diluted with additional 30 g of water.
[0200] The above emulsion was evaluated in a fabric softener consisting of: [0201] 55.6 g Tetranyl L1/90 standard [0202] 8 g MgCl.sub.2.6H.sub.2O solution @ 20% [0203] 936.4 g of water [0204] Total=1000 g.fwdarw.5% active Quat
[0205] The Tetranyl L1/90 standard was first melted at 55 C. The resulting liquid was then poured whilst being continuously stirred into in hot water and the resulting mixture was allowed to cool with continued stirring. During the cooling period, again with continuous stirring the magnesium chloride salt and the emulsion prepared in accordance with the invention were introduced.
[0206] The fabric (cotton towels) was treated by adding the softener using a Miele washing machine and a washing it with commercial detergent powder (DASH). Softness of towels was determined in a panel test and rated from 1-10 (10=softest). While the fabric softener described above was rated at 5.0, the fabric softener containing the emulsion in accordance with the present invention was rated at 5.5.
[0207] The water absorbency of the treated fabric was tested by dropping a 2 cm*2 cm sample into 250 ml water. The time until the fabric is sinking is recorded. The result was 9 s for the sample treated with softener containing the emulsion as described above and 128 s for a sample treated with a softener only, showing therefore improved water absorbency