CN102912644B - Skin-tendering siloxane pasty composition and preparation method thereof - Google Patents

Skin-tendering siloxane pasty composition and preparation method thereof Download PDF

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CN102912644B
CN102912644B CN201210390729.5A CN201210390729A CN102912644B CN 102912644 B CN102912644 B CN 102912644B CN 201210390729 A CN201210390729 A CN 201210390729A CN 102912644 B CN102912644 B CN 102912644B
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siloxanes
skin
tendering
skinfeel
weight
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CN102912644A (en
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张国杰
李桂军
李桂民
张锋
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HUAI'AN KAIYUE TECHNOLOGY DEVELOPMENT Co Ltd
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HUAI'AN KAIYUE TECHNOLOGY DEVELOPMENT Co Ltd
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Abstract

The invention discloses a skin-tendering siloxane pasty composition and a preparation method thereof. The skin-tendering siloxane pasty composition comprises 30-60% of silicone gel, 20-40% of high-viscosity polydimethylsiloxane, 15-20% of non-ionic surfactant and 5-10% of gas-phase white carbon black by weight percentage. The skin-tendering siloxane pasty composition does not comprises a solvent, has a simple, convenient and easily-controlled process, does not discharge waste gas, waste liquid and waste solid and does not cause environment pollution; when quantitatively added into a coating or a coating agent, the skin-tendering siloxane pasty composition can be stably dispersed in a system and has the advantage of applicability to both a solvent system and an aqueous system; and a coating film or a coating layer with the skin-tendering siloxane pasty composition has an excellent skin-tendering characteristic, so that the skin-tendering siloxane pasty composition has a wide application prospect and is beneficial to industrial production.

Description

Give siloxanes paste composition of tender skinfeel and preparation method thereof
Technical field
The present invention relates to the additive of coating and covering with paint, relate to specifically a kind of siloxanes paste composition of giving tender skinfeel and preparation method thereof, belong to organic silicon chemical field of new.
Background technology
Silicone gel strengthens elastic tactility or the skinfeel of cosmetic skin care product film as additive, see the report of domestic and international patent documentation, for example CN200510079207.3(silicone gel composition), CN200780007575.4 (silicone elastomer gels), CN201110403403.7 (silicone gel composition and preparation method thereof for a kind of daily use chemicals); The constituent of above-mentioned record is all hydrogen-containing siloxane and vinylsiloxane or propenyl polyethers to carry out hydrosilylation and makes under platinum group catalyst exists, its preparation method complexity and conditional request harshness, mainly strengthen the elastic tactility of skin care products or the additive of skinfeel as cosmetic field.Said enhancing elastic tactility or skinfeel function, not only by cosmetic field is pursued, also there is very large demand space in for example weaving of other field, leather, paint field, the rear covering with paint processing of the rear arrangement of for example some special high-grade weaving face fabrics, the high-grade leather that some are special, the application of some special high-grade paints, all there is the quality requirements that coating is required to have skinfeel, its reason is that the dermatoid feel of class or sense of touch make the mankind feel more nature and more get close to oneself, and the product with this kind of sense of touch feels that its class grade is higher seemingly by instinct.Nonetheless, also different because of thing because of people to the perception of skinfeel degree, just as the elasticity sensation of skin is felt difference because people is different with the age, the most significantly performance is divided into coarse and tender two kinds of main sensations.The tender skinfeel of statement refers to that tender elastic tactility as existing infant skin has again the sliding sense as congealed fat, about the research of the relevant siloxanes paste composition of above-mentioned non-cosmetic field, rarely has bibliographical information both at home and abroad.
Summary of the invention
The object of the invention is to: a kind of siloxanes paste composition of giving tender skinfeel and preparation method thereof is provided, the complete solvent free of said composition, simple process is easily controlled, three-waste free discharge and environmental pollution, this paste composition be quantitatively added in coating or finishing agent can stable dispersion in system, have advantages of that being both applicable to dicyandiamide solution is also applicable to water-based system, its film or coating have the excellent characteristics of giving tender skinfeel, not only have broad application prospects but also be conducive to suitability for industrialized production.
Technical solution of the present invention is: said composition comprises the silicone adhesive of 30 ~ 60% weight portions, the high viscosity dimethyl silicone polymer of 20 ~ 40% weight portions, the non-ionic surface active agent of 15 ~ 20% weight portions, the gas-phase silica of 5 ~ 10% weight portions.
Wherein, high viscosity dimethyl silicone polymer refers to that viscosity is 3 × 10 5~ 8 × 10 6the non-reacted linear polydimethylsiloxane-of normal temperature of mpa.s.
Wherein, silicone adhesive carries out partial cross-linked reaction by both-end epoxy baseline siloxanes and amino silicone and makes, and the epoxy radicals in both-end epoxy baseline siloxanes and the amino mol ratio in amino silicone are 0.5 ~ 5:100.
Wherein, both-end epoxy baseline siloxanes is the following epoxy radicals siloxanes of molecular structural formula:
Wherein, amino silicone is that nitrogen atom content is that the side chain of 0.06 ~ 0.12mol/100g is the linear polydimethylsiloxane-of aminopropyl or aminoethyl aminopropyl, and its viscosity is 500 ~ 5000mpa.s.
Wherein, gas-phase silica refer to the specific area of chlorosilane or silazane processing be 150 ~ 300m 2the hydrophobic gas-phase silica of/g.
Wherein, non-ionic surface active agent is that HLB value is a kind of or any two kinds of mixtures in 6 ~ 12 normal fatty alcohol polyoxyethylene ether, isomery fatty alcohol-polyoxyethylene ether, alkylphenol polyoxyethylene,
Wherein, non-ionic surface active agent refers to that HLB value is two kinds of mixtures of 6 ~ 12 isomery fatty alcohol-polyoxyethylene ether.
Wherein, the preparation method who gives the siloxanes paste composition of tender skinfeel comprises the following steps: under room temperature, in kneader or twin shaft planetary mixer, add amino silicone, stir, add again epoxy radicals siloxanes, add rear continuation stirring and after 10 minutes, stop stirring, every the crosslinking degree of 10 ~ 30 minutes sampling observing response things, obtain silicone adhesive; Wherein, the epoxy radicals in both-end epoxy baseline siloxanes and the amino mol ratio in amino silicone are 0.5 ~ 5:100; In silicone adhesive, add rapidly high viscosity dimethyl silicone polymer, add rear stirring 20 ~ 30 minutes, and then add again non-ionic surface active agent, continue to stir 30 ~ 60 minutes, finally add gas-phase silica, stir the siloxanes paste composition that must give tender skinfeel after 60 ~ 120 minutes; Wherein, silicone adhesive 30 ~ 60% weight portions, high viscosity dimethyl silicone polymer 20 ~ 40% weight portions, non-ionic surface active agent 15 ~ 20% weight portions, gas-phase silica 5 ~ 10% weight portions in composition.
Advantage of the present invention is: 1, this siloxanes paste composition makes an addition in coating or finishing agent, covers with paint, lacquer, colour wash, etc. in substrate surface and after being dried, and gives the tender skinfeel of film excellence; 2, simple process is easily controlled, and three-waste free discharge and environmental pollution, be conducive to suitability for industrialized production.
The specific embodiment
Further illustrate technical solution of the present invention below in conjunction with specific embodiment, these embodiment can not be interpreted as it is the restriction to technical scheme.
Embodiment 1: under room temperature, in 150 liters of kneaders, adding 59.62kg viscosity is the linear polydimethylsiloxane-that side chain that 500mpa.s, nitrogen atom content are 0.06mol/100g is aminopropyl, start stirring, adding the both-end epoxy baseline siloxanes 0.38kg(epoxy radicals of epoxide equivalent 0.46mol/100g and amino mol ratio is 5:100), add rear continuation stirring and after 10 minutes, stop stirring, every the crosslinking degree of 10 ~ 30 minutes sampling observing response things, obtain silicone adhesive; Starting stirring and adding rapidly 20kg viscosity is 3 × 10 5the non-reacted linear polydimethylsiloxane-of high viscosity normal temperature of mpa.s, add rear stirring 20 ~ 30 minutes, and then add again 10kg isomerous tridecanol polyoxyethylene (10) ether and 5kg isomerous tridecanol polyoxyethylene (5) ether, adding rear continuation stirs 30 ~ 60 minutes, the stirring of stopping, adds 5kg specific area 250m 2on the aerosil bonnet of the silazane processing of/g, the top cover of kneader fully seals, and continues stirring and after 60 ~ 120 minutes, obtains the pale siloxanes paste composition A that gives tender skinfeel of 100kg; Wherein, both-end epoxy baseline siloxane molecule structural formula is as follows:
Figure 410661DEST_PATH_IMAGE004
After tested, the siloxanes paste composition A that gives tender skinfeel is dissolved in No. 200 solvent naphthas, toluene, adopts phase conversion emulsifying to form the white emulsion of solid content 50% ~ 70%, not layering of stable dispersion in emulsion 7 days.
Embodiment 2: under room temperature, in 150 liters of kneaders, adding 29kg viscosity is that the side chain that 3000mpa.s, nitrogen atom content are 0.09mol/100g is the linear polydimethylsiloxane-of aminoethyl aminopropyl, start stirring, add the both-end epoxy baseline siloxanes 1kg(epoxy radicals of epoxide equivalent 0.05mol/100g and amino mol ratio to be about 1.9:100), add rear continuation stirring and after 10 minutes, stop stirring, every the crosslinking degree of 10 ~ 30 minutes sampling observing response things, obtain silicone adhesive; Starting stirring and adding rapidly 40kg viscosity is 3 × 10 6the non-reacted linear polydimethylsiloxane-of high viscosity normal temperature of mpa.s, add rear stirring 20 ~ 30 minutes, and then add again 15kg isomerous tridecanol polyoxyethylene (8) ether and 5kg isomerous tridecanol polyoxyethylene (4) ether, adding rear continuation stirs 30 ~ 60 minutes, the stirring of stopping, adds 10kg specific area 200m 2on the aerosil bonnet of the dimethyldichlorosilane processing of/g, the top cover of kneader fully seals, and continues stirring and after 60 ~ 120 minutes, obtains the pale siloxanes paste composition B that gives tender skinfeel of 100kg; Wherein, the molecular structural formula of both-end epoxy baseline siloxanes is as follows:
Figure 640785DEST_PATH_IMAGE006
After tested, the siloxanes paste composition B that gives tender skinfeel is dissolved in No. 200 solvent naphthas, toluene solvant, adopts phase conversion emulsifying to form the white emulsion of solid content 50% ~ 70%, not layering of stable dispersion in emulsion 7 days.
Embodiment 3: under room temperature, in 150 liters of kneaders, adding 39.4kg viscosity is that the side chain that 5000mpa.s, nitrogen atom content are 0.08mol/100g is the linear polydimethylsiloxane-of aminoethyl aminopropyl, start stirring, add the both-end epoxy baseline siloxanes 0.6kg(epoxy radicals of epoxide equivalent 0.026mol/100g and amino mol ratio to be about 0.5:100), adding rear continuation stirring stops after 10 minutes stirring, every the crosslinking degree of 10 ~ 30 minutes sampling observing response things, obtain silicone adhesive; Starting stirring and adding rapidly 32kg viscosity is 8 × 10 6the non-reacted linear polydimethylsiloxane-of high viscosity normal temperature of mpa.s, add rear stirring 20 ~ 30 minutes, and then add again 10kg isomerous tridecanol polyoxyethylene (10) ether and 10kg isomerous tridecanol polyoxyethylene (6) ether, adding rear continuation stirs 30 ~ 60 minutes, the stirring of stopping, adds 8kg specific area 250m 2on the aerosil bonnet of the dimethyldichlorosilane processing of/g, the top cover of kneader fully seals, and continues stirring and after 60 ~ 120 minutes, obtains the pale siloxanes paste composition C that gives tender skinfeel of 100kg; Wherein, the molecular structural formula of both-end epoxy baseline siloxanes is as follows:
Figure 497883DEST_PATH_IMAGE008
After tested, the siloxanes paste composition C that gives tender skinfeel is dissolved in No. 200 solvent naphthas, toluene solvant, adopts phase conversion emulsifying can form the white emulsion of solid content 50% ~ 70%, not layering of stable dispersion in emulsion 7 days.
Comparative example 4: with embodiment 1, just do not add both-end epoxy baseline siloxanes, the dosage of the linear polydimethylsiloxane-of aminopropyl changes 60kg into by 59.62kg simultaneously, and other is constant, and the pale siloxanes pastel obtaining is labeled as M.
Comparative example 5: with embodiment 1, just the linear polydimethylsiloxane-of aminopropyl changes 55kg into, and both-end epoxy baseline siloxanes changes 5kg into, and other is constant, and the pale siloxanes pastel obtaining is labeled as N.
Take SS-1010 (the solvent type polyurethane resin solution of the solid content 30% that Jiangsu De Fa resin Co., Ltd produces of 5 equal portions, toluene, DMF, n-butyl acetate mixed solvent are contained in its inside) each 950g, add respectively C, the M of 50g comparative example 4, the N of 50g comparative example 5 of B, the 50g embodiment 3 of A, the 50g embodiment 2 of 50g embodiment 1, after high-speed stirred 20 minutes, the mixture obtaining is labeled as respectively sample A1, B1, C1 and comparison specimen M1, N1.A1, B1, C1, M1, the N1 that gets respectively 10g is poured into it respectively behind the artificial leather surface of 5 15cm × 15cm and carefully strikes off with glass bar, dries and takes out afterwards for 30 ~ 60 seconds at 150 ℃, obtains sample A2, B2, C2 and comparison specimen M2, N2.Above-mentioned sample A1, B1, C1 and comparison specimen M1, N1 left standstill respectively to 1 hour simultaneously and within 7 days, observe afterwards dispersion stabilization separately.
Whether obvious and not obvious embodiment A, B, C and comparative example M, the N of distinguishing that touches effect with the tender skinfeel of sample A2, B2, C2 and comparison specimen M2, N2 gives tender skinfeel, whether with sample A1, B1, C1 and comparison specimen M1, N1, in 1 hour, whether stably dispersing is distinguished embodiment A, B, C and comparative example M, N has instant use value, whether with sample A1, B1, C1 and comparison specimen M1, N1, after 7 days, whether stably dispersing is distinguished embodiment A, B, C and comparative example M, N has practical value, and the comparing result of embodiment sample and comparative example sample is as following table.
Figure 129852DEST_PATH_IMAGE009

Claims (4)

1. the siloxanes paste composition of giving tender skinfeel, is characterized in that: said composition comprises the silicone adhesive of 30 ~ 60% weight, the high viscosity dimethyl silicone polymer of 20 ~ 40% weight, the non-ionic surface active agent of 15 ~ 20% weight, the gas-phase silica of 5 ~ 10% weight; High viscosity dimethyl silicone polymer refers to that viscosity is 3 × 10 5~ 8 × 10 6the non-reacted linear polydimethylsiloxane-of normal temperature of mpa.s; Silicone adhesive carries out partial cross-linked reaction by both-end epoxy baseline siloxanes and amino silicone and makes, and the epoxy radicals in both-end epoxy baseline siloxanes and the amino mol ratio in amino silicone are 0.5 ~ 5:100; Gas-phase silica refer to the specific area of chlorosilane or silazane processing be 150 ~ 300m 2the hydrophobic gas-phase silica of/g; Non-ionic surface active agent refers to that HLB value is two kinds of mixtures of 6 ~ 12 isomery fatty alcohol-polyoxyethylene ether.
2. the siloxanes paste composition of giving tender skinfeel according to claim 1, is characterized in that both-end epoxy baseline siloxanes is the following epoxy radicals siloxanes of molecular structural formula:
Figure 2012103907295100001DEST_PATH_IMAGE002
3. the siloxanes paste composition of giving tender skinfeel according to claim 1, it is characterized in that: amino silicone is that nitrogen atom content is that the side chain of 0.06 ~ 0.12mol/100g is the linear polydimethylsiloxane-of aminopropyl or aminoethyl aminopropyl, and its viscosity is 500 ~ 5000mpa.s.
4. give the preparation method of the siloxanes paste composition of tender skinfeel, it is characterized in that this preparation method comprises the following steps: under room temperature, in kneader or twin shaft planetary mixer, add amino silicone, stir, add again both-end epoxy baseline siloxanes, add rear continuation stirring and after 10 minutes, stop stirring, every the crosslinking degree of 10 ~ 30 minutes sampling observing response things, obtain silicone adhesive; Wherein, the epoxy radicals in both-end epoxy baseline siloxanes and the amino mol ratio in amino silicone are 0.5 ~ 5:100; In silicone adhesive, add rapidly high viscosity dimethyl silicone polymer, add rear stirring 20 ~ 30 minutes, and then add again non-ionic surface active agent, continue to stir 30 ~ 60 minutes, finally add gas-phase silica, stir the siloxanes paste composition that must give tender skinfeel after 60 ~ 120 minutes; Wherein, silicone adhesive 30 ~ 60% weight, high viscosity dimethyl silicone polymer 20 ~ 40% weight, non-ionic surface active agent 15 ~ 20% weight, gas-phase silica 5 ~ 10% weight in composition; High viscosity dimethyl silicone polymer refers to that viscosity is 3 × 10 5~ 8 × 10 6the non-reacted linear polydimethylsiloxane-of normal temperature of mpa.s; Gas-phase silica refer to the specific area of chlorosilane or silazane processing be 150 ~ 300m 2the hydrophobic gas-phase silica of/g; Non-ionic surface active agent refers to that HLB value is two kinds of mixtures of 6 ~ 12 isomery fatty alcohol-polyoxyethylene ether.
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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5061481A (en) * 1989-03-20 1991-10-29 Kobayashi Kose Co., Ltd. Cosmetic composition having acryl-silicone graft copolymer
CN101117559A (en) * 2007-05-10 2008-02-06 成都硅宝科技实业有限责任公司 Method for manufacturing mono-component water-dispersing room temperature dewatering silicon sulfide ketone seal gum
CN101525519A (en) * 2009-03-30 2009-09-09 中山大桥化工集团有限公司 Polysiloxane coating composition
CN101602918A (en) * 2009-07-23 2009-12-16 河海大学 Hydraulic structure disjoint filling silicone adhesive and preparation method thereof
CN101805562A (en) * 2010-03-26 2010-08-18 陈俊光 Silicone-type coatings and preparation method thereof

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1998018849A1 (en) * 1996-10-29 1998-05-07 Grant Industries, Inc. Grafted rubber-like silicone gel with enhanced oil compatibility and its synthetic process

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5061481A (en) * 1989-03-20 1991-10-29 Kobayashi Kose Co., Ltd. Cosmetic composition having acryl-silicone graft copolymer
CN101117559A (en) * 2007-05-10 2008-02-06 成都硅宝科技实业有限责任公司 Method for manufacturing mono-component water-dispersing room temperature dewatering silicon sulfide ketone seal gum
CN101525519A (en) * 2009-03-30 2009-09-09 中山大桥化工集团有限公司 Polysiloxane coating composition
CN101602918A (en) * 2009-07-23 2009-12-16 河海大学 Hydraulic structure disjoint filling silicone adhesive and preparation method thereof
CN101805562A (en) * 2010-03-26 2010-08-18 陈俊光 Silicone-type coatings and preparation method thereof

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