CN116473878A - Silicone gel elastomer composition for skin care and preparation method thereof - Google Patents
Silicone gel elastomer composition for skin care and preparation method thereof Download PDFInfo
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- CN116473878A CN116473878A CN202310276194.7A CN202310276194A CN116473878A CN 116473878 A CN116473878 A CN 116473878A CN 202310276194 A CN202310276194 A CN 202310276194A CN 116473878 A CN116473878 A CN 116473878A
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- 229920001296 polysiloxane Polymers 0.000 title claims abstract description 186
- 229920001971 elastomer Polymers 0.000 title claims abstract description 97
- 239000000806 elastomer Substances 0.000 title claims abstract description 97
- 239000000203 mixture Substances 0.000 title claims abstract description 87
- 238000002360 preparation method Methods 0.000 title claims abstract description 44
- -1 polysiloxane Polymers 0.000 claims abstract description 154
- 239000000499 gel Substances 0.000 claims abstract description 65
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims abstract description 57
- 229920002554 vinyl polymer Polymers 0.000 claims abstract description 57
- 239000004721 Polyphenylene oxide Substances 0.000 claims abstract description 40
- 229920000570 polyether Polymers 0.000 claims abstract description 40
- 239000002904 solvent Substances 0.000 claims abstract description 25
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000000741 silica gel Substances 0.000 claims abstract description 24
- 229910002027 silica gel Inorganic materials 0.000 claims abstract description 24
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 claims abstract description 20
- 229920000056 polyoxyethylene ether Polymers 0.000 claims abstract description 20
- 229940051841 polyoxyethylene ether Drugs 0.000 claims abstract description 20
- 229920002050 silicone resin Polymers 0.000 claims abstract description 20
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims abstract description 19
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims description 107
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 100
- 239000001257 hydrogen Substances 0.000 claims description 68
- 229910052739 hydrogen Inorganic materials 0.000 claims description 68
- 238000010438 heat treatment Methods 0.000 claims description 67
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 54
- 238000006243 chemical reaction Methods 0.000 claims description 50
- 229910052697 platinum Inorganic materials 0.000 claims description 50
- 150000002431 hydrogen Chemical class 0.000 claims description 40
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 38
- 238000000034 method Methods 0.000 claims description 37
- 230000008569 process Effects 0.000 claims description 25
- 238000010790 dilution Methods 0.000 claims description 18
- 239000012895 dilution Substances 0.000 claims description 18
- 239000011259 mixed solution Substances 0.000 claims description 17
- 238000002156 mixing Methods 0.000 claims description 17
- 238000007599 discharging Methods 0.000 claims description 16
- 238000004821 distillation Methods 0.000 claims description 9
- GVNVAWHJIKLAGL-UHFFFAOYSA-N 2-(cyclohexen-1-yl)cyclohexan-1-one Chemical compound O=C1CCCCC1C1=CCCCC1 GVNVAWHJIKLAGL-UHFFFAOYSA-N 0.000 claims description 8
- 101150065749 Churc1 gene Proteins 0.000 claims description 8
- 102100038239 Protein Churchill Human genes 0.000 claims description 8
- 238000005303 weighing Methods 0.000 claims description 8
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 150000002430 hydrocarbons Chemical class 0.000 claims description 3
- 229940057874 phenyl trimethicone Drugs 0.000 claims description 3
- LINXHFKHZLOLEI-UHFFFAOYSA-N trimethyl-[phenyl-bis(trimethylsilyloxy)silyl]oxysilane Chemical compound C[Si](C)(C)O[Si](O[Si](C)(C)C)(O[Si](C)(C)C)C1=CC=CC=C1 LINXHFKHZLOLEI-UHFFFAOYSA-N 0.000 claims description 3
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims description 2
- DSVRVHYFPPQFTI-UHFFFAOYSA-N bis(ethenyl)-methyl-trimethylsilyloxysilane;platinum Chemical compound [Pt].C[Si](C)(C)O[Si](C)(C=C)C=C DSVRVHYFPPQFTI-UHFFFAOYSA-N 0.000 claims description 2
- JUWSSMXCCAMYGX-UHFFFAOYSA-N gold platinum Chemical compound [Pt].[Au] JUWSSMXCCAMYGX-UHFFFAOYSA-N 0.000 claims description 2
- 229910052741 iridium Inorganic materials 0.000 claims description 2
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052762 osmium Inorganic materials 0.000 claims description 2
- SYQBFIAQOQZEGI-UHFFFAOYSA-N osmium atom Chemical compound [Os] SYQBFIAQOQZEGI-UHFFFAOYSA-N 0.000 claims description 2
- 229910052763 palladium Inorganic materials 0.000 claims description 2
- 229910052703 rhodium Inorganic materials 0.000 claims description 2
- 239000010948 rhodium Substances 0.000 claims description 2
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 claims description 2
- 229910052707 ruthenium Inorganic materials 0.000 claims description 2
- 239000002994 raw material Substances 0.000 abstract description 9
- 238000003860 storage Methods 0.000 abstract description 9
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 239000003795 chemical substances by application Substances 0.000 abstract description 3
- 239000011248 coating agent Substances 0.000 abstract description 3
- 238000000576 coating method Methods 0.000 abstract description 3
- 239000003921 oil Substances 0.000 description 31
- 238000003786 synthesis reaction Methods 0.000 description 22
- BANXPJUEBPWEOT-UHFFFAOYSA-N 2-methyl-Pentadecane Chemical compound CCCCCCCCCCCCCC(C)C BANXPJUEBPWEOT-UHFFFAOYSA-N 0.000 description 16
- 239000000243 solution Substances 0.000 description 14
- 239000000463 material Substances 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 11
- 229940043268 2,2,4,4,6,8,8-heptamethylnonane Drugs 0.000 description 8
- XMSXQFUHVRWGNA-UHFFFAOYSA-N Decamethylcyclopentasiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O1 XMSXQFUHVRWGNA-UHFFFAOYSA-N 0.000 description 8
- KUVMKLCGXIYSNH-UHFFFAOYSA-N isopentadecane Natural products CCCCCCCCCCCCC(C)C KUVMKLCGXIYSNH-UHFFFAOYSA-N 0.000 description 8
- 229920002545 silicone oil Polymers 0.000 description 8
- 239000000126 substance Substances 0.000 description 8
- 238000001514 detection method Methods 0.000 description 7
- 238000004132 cross linking Methods 0.000 description 6
- HNDMWPOGQFUHIL-UHFFFAOYSA-N dodecyl(silyloxysilyloxysilyloxysilyloxy)silane Chemical compound CCCCCCCCCCCC[SiH2]O[SiH2]O[SiH2]O[SiH2]O[SiH3] HNDMWPOGQFUHIL-UHFFFAOYSA-N 0.000 description 6
- 238000012360 testing method Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000007865 diluting Methods 0.000 description 3
- 238000006459 hydrosilylation reaction Methods 0.000 description 3
- 210000000697 sensory organ Anatomy 0.000 description 3
- 230000001070 adhesive effect Effects 0.000 description 2
- 230000003750 conditioning effect Effects 0.000 description 2
- 239000006071 cream Substances 0.000 description 2
- HZGRXXQQOAOFNS-UHFFFAOYSA-N dodecyl-methyl-silyloxysilyloxysilyloxysilyloxysilane Chemical compound CCCCCCCCCCCC[SiH](C)O[SiH2]O[SiH2]O[SiH2]O[SiH3] HZGRXXQQOAOFNS-UHFFFAOYSA-N 0.000 description 2
- 238000004043 dyeing Methods 0.000 description 2
- 239000006210 lotion Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- 238000010422 painting Methods 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 230000036632 reaction speed Effects 0.000 description 2
- 231100000241 scar Toxicity 0.000 description 2
- 230000001953 sensory effect Effects 0.000 description 2
- 239000002453 shampoo Substances 0.000 description 2
- 230000008591 skin barrier function Effects 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 239000004970 Chain extender Substances 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 230000001166 anti-perspirative effect Effects 0.000 description 1
- 239000003213 antiperspirant Substances 0.000 description 1
- 230000003796 beauty Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000004205 dimethyl polysiloxane Substances 0.000 description 1
- DLAHAXOYRFRPFQ-UHFFFAOYSA-N dodecyl benzoate Chemical compound CCCCCCCCCCCCOC(=O)C1=CC=CC=C1 DLAHAXOYRFRPFQ-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000008266 hair spray Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 239000012454 non-polar solvent Substances 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000000144 pharmacologic effect Effects 0.000 description 1
- 239000002798 polar solvent Substances 0.000 description 1
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 239000002884 skin cream Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/42—Block-or graft-polymers containing polysiloxane sequences
- C08G77/46—Block-or graft-polymers containing polysiloxane sequences containing polyether sequences
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/84—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
- A61K8/89—Polysiloxanes
- A61K8/891—Polysiloxanes saturated, e.g. dimethicone, phenyl trimethicone, C24-C28 methicone or stearyl dimethicone
- A61K8/894—Polysiloxanes saturated, e.g. dimethicone, phenyl trimethicone, C24-C28 methicone or stearyl dimethicone modified by a polyoxyalkylene group, e.g. cetyl dimethicone copolyol
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/84—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
- A61K8/89—Polysiloxanes
- A61K8/895—Polysiloxanes containing silicon bound to unsaturated aliphatic groups, e.g. vinyl dimethicone
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/20—Chemical, physico-chemical or functional or structural properties of the composition as a whole
- A61K2800/26—Optical properties
- A61K2800/262—Transparent; Translucent
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Veterinary Medicine (AREA)
- Public Health (AREA)
- General Health & Medical Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- Epidemiology (AREA)
- Birds (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Polymers & Plastics (AREA)
- Medicinal Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Dermatology (AREA)
- Silicon Polymers (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention provides a silicone gel elastomer composition for skin care and a preparation method thereof, and relates to the technical field of skin care agents. The silicone gel elastomer composition comprises 36-44% of silicone gel elastomer and 56-64% of solvent; the silicone gel elastomer is polymerized in a solvent system, and the raw materials for preparing the silicone gel elastomer comprise: vinyl silicone resin, vinyl-terminated polysiloxane, polyether modified hydrogen-containing polysiloxane, hydrogen-terminated polysiloxane and platinum group metal compound, wherein the polyether modified hydrogen-containing siloxane is prepared from allyl polyoxyethylene ether and hydrogen-terminated polysiloxane; the preparation method specifically comprises the following steps: s1, preparing polyether modified hydrogen-containing polysiloxane; s2, preparation of a silicone gel elastomer composition. The silica gel elastomer composition prepared by the invention has the characteristics of smooth coating hand feeling, good organoleptic properties, low viscosity, good fluidity, tight skin adhesion, good compatibility, high storage stability and low raw material loss in the production process.
Description
Technical Field
The invention relates to the technical field of skin care agents, in particular to a silicone gel elastomer composition for skin care and a preparation method thereof.
Background
Silicone materials have long been used in personal care products. As early as 1940, revlon corporation in united states introduced a silicone oil-containing skin cream "Silicare skin lotion," which was the first silicone oil used in personal care products. In the 50 s of the 20 th century, companies have incorporated silicone oils as lubricants in hair spray formulations to prevent spray head clogging. From the 1970 s, conditioning effects of silicone oils were found and increasingly emphasized, and more hair dyeing and conditioner products use silicone oils as conditioning agents for the care of hair damaged by dyeing. In 1990, the U.S. baby company introduced the first 2 in 1 shampoo containing silicone oil. Nowadays, silicone materials such as silicone oils have been widely used in daily chemical products such as creams, lotions, make-up, antiperspirants, shampoos, hair conditioners, hair films, lipsticks, shaving creams and the like.
In addition, in view of the excellent biocompatibility and unique physicochemical property advantages of the organosilicon material, the organosilicon material is widely applied to medical instrument classification catalog scar repairing materials, such as application type, gel type or spray type scar treating products, which all take polydimethylsiloxane as a main component and have no pharmacological effect.
In recent years, silicone gel elastomer compositions have been developed to meet the increasing demands of people for beauty and health. However, because the promotion and application time of the silicone gel elastomer composition is short, the conventional silicone gel elastomer composition generally has the problems of sticky and smooth coating hand feeling, poor sense, high viscosity, poor flowability, poor skin adhesion, poor compatibility, low storage stability, high raw material loss in the production process and the like, so that the development of the silicone gel elastomer composition with more excellent physicochemical properties is needed.
Disclosure of Invention
(one) solving the technical problems
Aiming at the defects of the prior art, the invention provides a silicone gel elastomer composition for skin care and a preparation method thereof, and solves the problems of poor physical properties such as sense organ, poor compatibility, low storage stability and the like of the traditional silicone gel elastomer composition.
(II) technical scheme
In order to achieve the above purpose, the invention is realized by the following technical scheme:
a first object of the present invention is to provide a silicone gel elastomer composition for skin care comprising the following components in mass ratio: 36-44% of silica gel elastomer and 56-64% of solvent; the silicone gel elastomer is polymerized in the solvent system.
Preferably, the silicone gel elastomer is synthetically prepared from the following components: vinyl silicone resin, vinyl-terminated polysiloxane, polyether modified hydrogen-containing polysiloxane, hydrogen-terminated polysiloxane and platinum group metal compound, wherein the polyether modified hydrogen-containing siloxane is prepared from allyl polyoxyethylene ether and hydrogen-terminated polysiloxane.
The second object of the invention is to provide a preparation method of a silicone gel elastomer composition for skin care, which has the advantages of simple operation method, low raw material consumption rate and low production cost, and the specific scheme comprises the following steps:
s1, preparing polyether modified hydrogen-containing polysiloxane:
firstly, uniformly stirring and mixing isopropanol, allyl polyoxyethylene ether and platinum group metal compounds, then dropwise adding end-side hydrogen-containing polysiloxane diluted by isopropanol into the mixture for reaction, and carrying out reduced pressure distillation in a vacuum environment after the reaction is finished, and cooling to obtain polyether modified hydrogen-containing polysiloxane;
s2, preparation of a silicone gel elastomer composition:
firstly, adding a solvent into a reaction system to form a solvent-containing system, then adding vinyl silicone resin, vinyl-terminated polysiloxane and platinum group metal compound into the solvent system, and stirring and heating;
weighing polyether modified hydrogen-containing polysiloxane and terminal hydrogen-containing polysiloxane, adding a proper amount of solvent for dilution, dripping the diluted mixed solution into a reaction system after uniform mixing, and discharging after the reaction is finished to obtain the silica gel elastomer composition.
Preferably, the molecular formula of the allyl polyoxyethylene ether in S1 is: CH (CH) 2 ＝CHCH 2 O(CH 2 CH 2 O) c H, wherein c=7 to 12, and the molecular weight is 400 to 600. The allyl polyoxyethylene ether can provide vinyl active sites, and the compound containing the hydrophilic polyether segment is grafted into the hydrogen-containing polysiloxane through hydrosilylation reaction, so that the hydrophilic modification of the hydrogen-containing polysiloxane is realized.
Preferably, the viscosity of the end-side hydrogen-containing polysiloxane in the S1 is 7-30 mPa.s, the hydrogen content is 0.26-1.06% (wt), and the molecular formula is:
H(CH 3 ) 2 -Si-O-[Si(CH 3 ) 2 O] a -[SiHCH 3 O] b -Si-(CH 3 ) 2 h, wherein a=10 to 30 and b=5 to 20. The terminal hydrogen-containing polysiloxane can provide more than 3 crosslinking points.
Preferably, the viscosity of the vinyl silicone resin in S2 is 5000-15000 mPa.s and the vinyl content is 0.54-0.98% (wt). The vinyl silicone resin can provide vinyl active sites, and can carry out crosslinking reaction with hydrogen-containing polysiloxane, so that the strength and toughness of the silicone gel elastomer are improved, and the adhesive property of the silicone gel elastomer is improved.
Preferably, the viscosity of the vinyl silicone resin in the S2 is 5000-8000Pa.s, and the vinyl content is 0.78-0.98% (wt).
Preferably, the viscosity of the vinyl-terminated polysiloxane in S2 is 80-2000 mPa.s, the vinyl content is 0.07-0.71% (wt), and the molecular formula is:
Vi(CH 3 ) 2 -Si-O-[Si(CH 3 ) 2 O] d -Si-(CH 3 ) 2 vi, where Vi is vinyl CH 2 =ch-, d=100 to 1000. The vinyl-terminated polysiloxane can provide vinyl active sites and can be subjected to crosslinking reaction with hydrogen-containing polysiloxane to generate the organosilicon elastomer with a reticular crosslinking structure.
Preferably, the viscosity of the vinyl-terminated polysiloxane in the S2 is 200-1000 mPa.s, and the vinyl content is 0.22-0.63% (wt).
Preferably, the viscosity of the end hydrogen-containing polysiloxane in the S2 is 8-70 mPa.s, the hydrogen content is 0.04-0.19% (wt), and the molecular formula is:
H(CH 3 ) 2 -Si-O-[Si(CH 3 ) 2 O] e -Si-(CH 3 ) 2 h, wherein e=12 to 65. The terminal hydrogen-containing polysiloxane can provide double-terminal hydrogen active sites, can be used as a chain extender in a crosslinking reaction system, can effectively reduce crosslinking density, reduce stress concentration points, improve the flexibility of a molecular chain segment of the silica gel elastomer, and enhance the toughness and adhesive force of the molecular chain segment.
Preferably, the viscosity of the hydrogen-containing polysiloxane at the middle end of the S2 is 20-50 mPa.s, and the hydrogen content is 0.07-0.12% (wt).
Preferably, the platinum group metal compound is any one of ruthenium and its complex, rhodium and its complex, palladium and its complex, osmium and its complex, iridium and its complex, platinum and its complex. The platinum in the platinum group metal compound is 0-valent, has extremely high catalytic activity and is used as a catalyst for hydrosilylation.
Preferably, the platinum group metal compound is chloroplatinic acid or platinum gold complex.
Preferably, the platinum group metal compound is a platinum-divinyl tetramethyl disiloxane complex with a platinum concentration of 2000ppm.
Preferably, the solvent is one or more of linear dimethylsiloxane, phenyl trimethicone, dimethylsiloxane ring, hydrocarbon compounds, alkyl benzoates.
Preferably, the linear dimethylsiloxane has the formula:
(CH 3 ) 3 -Si-O-[Si(CH 3 ) 2 O] f -Si-(CH 3 ) 3 f=0 to 100, and the viscosity is 0.65 to 100mpa.s.
Preferably, the phenyl trimethicone has a viscosity of 22.5mpa.s.
Preferably, the dimethylsiloxane ring has the formula [ (CH) 3 ) 2 SiO] g ，g＝3～10。
Preferably, the hydrocarbon compound is a C12-C16 isoparaffin.
Preferably, the alkyl benzoate is a C12-C15 alkyl benzoate compound.
(III) beneficial effects
The invention provides a silicone gel elastomer composition for skin care and a preparation method thereof. Compared with the prior art, the method has the following beneficial effects:
1. the silica gel elastomer composition prepared by the invention has transparent appearance, is easy to paint, has smooth painting hand feeling and has excellent organoleptic properties.
2. The silica gel elastomer composition prepared by the invention has the advantages of low viscosity, good fluidity, simple production operation, low raw material consumption rate and low production cost.
3. The silica gel elastomer composition prepared by the invention has good adhesion with skin, is not easy to peel off and separate from the surface of the skin, and can play a good role in protecting skin barrier.
4. The silicone gel elastomer composition prepared by the invention can be simultaneously matched with water-based and oil-based formulas, and has good product compatibility and high formula flexibility.
5. The silica gel elastomer composition prepared by the invention has high storage stability and long service life.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, it being obvious that the drawings in the following description are only some embodiments of the invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a process flow diagram of the preparation method of the present invention.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more clear, the technical solutions in the embodiments of the present invention are clearly and completely described, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The embodiment of the application solves the problems of poor physical properties such as sense organs, poor compatibility, low storage stability and the like of the traditional silicone gel elastomer composition by providing the silicone gel elastomer composition for skin care and the preparation method thereof, and achieves the effects of smooth smearing hand feeling, good sense organs, low viscosity, good fluidity, tight skin adhesion, good compatibility, high storage stability and low raw material loss in the production process.
In order to better understand the above technical solutions, the following detailed description will refer to the accompanying drawings and specific embodiments.
The invention relates to a silicone gel elastomer composition for skin care, which comprises the following components in percentage by mass: 36-44% of silica gel elastomer and 56-64% of solvent;
the silicone gel elastomer is polymerized in the solvent system, and the raw materials for preparing the silicone gel elastomer comprise: vinyl silicone resin, vinyl-terminated polysiloxane, polyether modified hydrogen-containing polysiloxane, hydrogen-terminated polysiloxane and platinum group metal compound, wherein the polyether modified hydrogen-containing siloxane is prepared from allyl polyoxyethylene ether and hydrogen-terminated polysiloxane;
the silicon gel elastomer composition comprises the following raw materials in percentage by weight: 3 to 9 percent of vinyl silicone resin, 28 to 33 percent of terminal vinyl polysiloxane, 1 to 5 percent of polyether modified hydrogen-containing polysiloxane, 0.5 to 2 percent of terminal hydrogen-containing polysiloxane and 0.05 to 0.15 percent of platinum group metal compound.
The preparation method of the silica gel elastomer composition comprises the following steps:
preparation of polyether modified hydrogen-containing polysiloxane: taking a clean and dry four-neck round-bottom flask, sequentially adding metered isopropanol, allyl polyoxyethylene ether and platinum complex, building a synthesis reaction device with oil bath heating, starting stirring, setting the stirring speed to be 400-600 rpm, weighing metered end-side hydrogen-containing polysiloxane, diluting with proper amount of isopropanol, slowly dripping the end-side hydrogen-containing polysiloxane isopropanol solution into the four-neck round-bottom flask through a dropping funnel in the stirring process, controlling the dripping speed to be completed within 30-60 min, setting the stirring speed to be 500-1000 rpm, and stirring for reaction for 1-2 h at normal temperature and normal pressure. After the reaction is finished, starting an oil bath for heating, heating to 70-80 ℃, connecting a vacuum system and a distillation device, decompressing and distilling for 2-3 hours to remove and collect low-boiling-point substances, and then closing vacuum and heating to naturally cool the materials in the flask to prepare the polyether modified hydrogen-containing polysiloxane.
Preparation of the silicone gel elastomer composition: taking a clean and dry four-neck round-bottom flask, sequentially adding metered solvent, vinyl silicone resin, vinyl-terminated polysiloxane and platinum complex, constructing a synthesis reaction device with oil bath heating, starting stirring and heating, setting the stirring speed to be 400-600 rpm and the temperature to be 40-50 ℃, weighing metered polyether modified hydrogen-containing polysiloxane and hydrogen-terminated polysiloxane, adding a proper amount of solvent to mix and dilute, slowly dripping the mixed solution into the four-neck round-bottom flask through a dropping funnel in the stirring process, controlling the dripping speed to be completed within 30-60 min, setting the stirring speed to be 1000-2000 rpm, and stirring for 3-4 h. And stopping heating after the reaction is finished, and discharging to obtain the silica gel elastomer composition.
Example 1
As shown in fig. 1, the preparation method of the silicone gel elastomer composition specifically comprises the following steps:
preparation of polyether modified hydrogen-containing polysiloxane SH 1: a clean and dry 250ml four-necked round bottom flask was taken and sequentially charged with 20g of isopropanol, 10g of allyl polyoxyethylene ether APEG400 (molecular weight 400, molecular formula CH) 2 ＝CHCH 2 O(CH 2 CH 2 O) 7 H) 0.1g of platinum complex (platinum effective concentration 2000 ppm), a synthesis reaction apparatus with oil bath heating was set up, stirring was started, stirring speed was set at 400rpm, and 29.4g of end-side hydrogen-containing polysiloxane (viscosity 7mPa.s, hydrogen content 0.6%, molecular formula: A)
H(CH 3 ) 2 -Si-O-[Si(CH 3 ) 2 O] 10 -[SiHCH 3 O] 5 -Si-(CH 3 ) 2 H) And weighing 20g of isopropanol for dilution, then slowly dripping the end-side hydrogen-containing polysiloxane isopropanol solution into a four-mouth round bottom flask through a dropping funnel in the stirring process, controlling the dripping speed to be completed within 30min, setting the stirring speed to be 500rpm, and stirring for reaction for 1h at normal temperature and normal pressure. After the reaction is finished, starting an oil bath for heating, heating to 70 ℃, connecting a vacuum system and a distillation device, decompressing and distilling for 2 hours to remove and collect low-boiling-point substances, and then closing vacuum and heating to naturally cool the materials in the flask to prepare the polyether modified hydrogen-containing polysiloxane.
Preparation of silicone gel elastomer composition SE 1: a clean and dry 500ml four-necked round bottom flask was taken, 160g of decamethyl cyclopentasiloxane, 10.3g of vinyl silicone resin (viscosity 6300mPa.s, vinyl content 0.96%), 79.7g of vinyl-terminated polysiloxane (viscosity 500mPa.s, vinyl content 0.43%), 0.25g of platinum complex (platinum effective concentration 2000 ppm) were sequentially added, an oil bath heated synthesis reaction device was built, stirring and heating were started, stirring speed was set at 400rpm, temperature was set at 40 ℃, 4.69g of polyether-modified hydrogen-containing polysiloxane SH1 and 4.08g of hydrogen-terminated polysiloxane (viscosity 25mPa.s, hydrogen content 0.12%) were weighed, 15.6g of decamethyl cyclopentasiloxane were added for mixing and dilution, then the mixed solution was slowly dripped into the four-necked round bottom flask through a dripping funnel in the stirring process, dripping was completed within 30min under control of the dripping speed, stirring speed was set at 1000rpm, and stirring was carried out for 4h. And stopping heating after the reaction is finished, and discharging to obtain the silica gel elastomer composition.
Example 2
The preparation method of the silicone gel elastomer composition specifically comprises the following steps:
preparation of polyether modified hydrogen-containing polysiloxane SH 2: a clean and dry 250ml four-necked round bottom flask was taken and sequentially charged with 20g of isopropanol, 10g of allyl polyoxyethylene ether APEG400 (molecular weight 400, molecular formula CH) 2 ＝CHCH 2 O(CH 2 CH 2 O) 7 H) 0.12g of platinum complex (platinum effective concentration 2000 ppm), a synthesis reaction apparatus with oil bath heating was set up, stirring was started, stirring speed was set at 400rpm, and 37g of hydrogen-containing polysiloxane (viscosity 10mPa.s, hydrogen content 0.81%, molecular formula: formula)
H(CH 3 ) 2 -Si-O-[Si(CH 3 ) 2 O] 10 -[SiHCH 3 O] 10 -Si-(CH 3 ) 2 H) And weighing 30g of isopropanol for dilution, then slowly dripping the end-side hydrogen-containing polysiloxane isopropanol solution into a four-mouth round bottom flask through a dropping funnel in the stirring process, controlling the dripping speed to be completed within 30min, setting the stirring speed to be 500rpm, and stirring for reaction for 1h at normal temperature and normal pressure. After the reaction is finished, starting an oil bath for heating, heating to 70 ℃, connecting a vacuum system and a distillation device, decompressing and distilling for 2 hours to remove and collect low-boiling-point substances, and then closing vacuum and heating to naturally cool the materials in the flask to prepare the polyether modified hydrogen-containing polysiloxane.
Preparation of silicone gel elastomer composition SE 2: a clean and dry 500ml four-necked round bottom flask was taken, 150g of decamethyl cyclopentasiloxane, 12.5g of vinyl silicone resin (viscosity 6300mPa.s, vinyl content 0.96%), 78.6g of vinyl-terminated polysiloxane (viscosity 500mPa.s, vinyl content 0.43%), 0.25g of platinum complex (platinum effective concentration 2000 ppm) were sequentially added, an oil bath heated synthesis reaction device was built, stirring and heating were started, stirring speed was set at 400rpm, temperature was set at 40 ℃, 3.48g of polyether-modified hydrogen-containing polysiloxane SH2 and 4.24g of vinyl-terminated polysiloxane (viscosity 25mPa.s, hydrogen content 0.12%) were weighed, 11.2g of decamethyl cyclopentasiloxane were added for mixing and dilution, then the mixed solution was slowly dripped into the four-necked round bottom flask through a dripping funnel in the stirring process, dripping was completed within 30min under control of the dripping speed, stirring speed was set at 1000rpm, and stirring was carried out for 4h. And stopping heating after the reaction is finished, and discharging to obtain the silica gel elastomer composition.
Example 3
The preparation method of the silicone gel elastomer composition specifically comprises the following steps:
preparation of polyether modified hydrogen-containing polysiloxane SH 3: a clean and dry 250ml four-necked round bottom flask was taken and sequentially charged with 20g of isopropanol, 10g of allyl polyoxyethylene ether APEG400 (molecular weight 400, molecular formula CH) 2 ＝CHCH 2 O(CH 2 CH 2 O) 7 H) 0.13g of platinum complex (platinum effective concentration 2000 ppm), a synthesis reaction apparatus with oil bath heating was set up, stirring was started, stirring speed was set at 500rpm, and 51.8g of end-side hydrogen-containing polysiloxane (viscosity 15mPa s, hydrogen content 1.06%, molecular formula
H(CH 3 ) 2 -Si-O-[Si(CH 3 ) 2 O] 10 -[SiHCH 3 O] 20 -Si-(CH 3 ) 2 H) And 42g of isopropanol is weighed for dilution, then the end-side hydrogen-containing polysiloxane isopropanol solution is slowly dripped into a four-mouth round bottom flask through a dripping funnel in the stirring process, the dripping speed is controlled to be within 45min, and then the stirring speed is set to be 750rpm, and the reaction is carried out for 1.5h under normal temperature and normal pressure. After the reaction is finished, starting an oil bath for heating, heating to 75 ℃, connecting a vacuum system and a distillation device, decompressing and distilling for 2.5 hours to remove and collect low-boiling-point substances, and then closing vacuum and heating to naturally cool the materials in the flask to prepare the polyether modified hydrogen-containing polysiloxane.
Preparation of silicone gel elastomer composition SE 3: a clean and dry 500ml four-necked round bottom flask was taken, 130g of dodecylpentasiloxane, 14.2g of vinyl silicone resin (viscosity 6300mPa.s, vinyl content 0.96%), 77.8g of vinyl-terminated polysiloxane (viscosity 500mPa.s, vinyl content 0.43%), 0.24g of platinum complex (platinum effective concentration 2000 ppm) were sequentially added, an oil bath heated synthesis reaction apparatus was built, stirring and heating were started, stirring speed was set at 500rpm, temperature was set at 45 ℃, 2.47g of polyether-modified hydrogen-containing polysiloxane SH3 and 2.91g of hydrogen-terminated polysiloxane (viscosity 25mPa.s, hydrogen content 0.12%) were weighed, 16.1g of dodecylpentasiloxane were added to mix and dilute, then the mixed solution was slowly dropped into the four-necked round bottom flask through a dropping funnel during stirring, dropping speed was controlled to complete within 45min, stirring speed was set at 1500rpm, and stirring reaction was carried out for 3.5h. And stopping heating after the reaction is finished, and discharging to obtain the silica gel elastomer composition.
Example 4
The preparation method of the silicone gel elastomer composition specifically comprises the following steps:
preparation of polyether modified hydrogen-containing polysiloxane SH 4: a clean and dry 250ml four-necked round bottom flask was taken and sequentially charged with 20g of isopropanol, 15g of allyl polyoxyethylene ether APEG600 (molecular weight 600, molecular formula CH) 2 ＝CHCH 2 O(CH 2 CH 2 O) 12 H) 0.17g of platinum complex (platinum effective concentration 2000 ppm), a synthesis reaction apparatus with oil bath heating was set up, stirring was started, stirring speed was set at 500rpm, and 66.4g of end-side hydrogen-containing polysiloxane (viscosity 20mPa.s, hydrogen content 0.26%, molecular formula: A)
H(CH 3 ) 2 -Si-O-[Si(CH 3 ) 2 O] 30 -[SiHCH 3 O] 5 -Si-(CH 3 ) 2 H) And weighing 62g of isopropanol for dilution, then slowly dripping the end-side hydrogen-containing polysiloxane isopropanol solution into a four-mouth round bottom flask through a dropping funnel in the stirring process, controlling the dripping speed to be completed within 45min, setting the stirring speed to 750rpm, and stirring and reacting for 1.5h at normal temperature and normal pressure. After the reaction is finished, starting an oil bath for heating, heating to 75 ℃, connecting a vacuum system and a distillation device, decompressing and distilling for 2.5h to remove and collect low-boiling-point substances, then closing vacuum and heating, and naturally cooling materials in a flask to prepare polyetherHydrogen-containing polysiloxanes.
Preparation of silicone gel elastomer composition SE 4: a clean and dry 500ml four-neck round-bottom flask was taken, 150g of dodecylpentasiloxane, 15.8g of vinyl silicone resin (viscosity 6300mPa.s, vinyl content 0.96%), 77g of terminal vinyl polysiloxane (viscosity 500mPa.s, vinyl content 0.43%), 0.27g of platinum complex (platinum effective concentration 2000 ppm) were sequentially added, an oil bath heated synthesis reaction device was built, stirring and heating were started, stirring speed was set at 500rpm, temperature was set at 45 ℃, 12.77g of polyether modified hydrogen-containing polysiloxane SH4 and 2.98g of terminal hydrogen-containing polysiloxane (viscosity 25mPa.s, hydrogen content 0.12%) were weighed, 12.8g of dodecylpentasiloxane were added for mixing and dilution, then the mixed solution was slowly dropped into the four-neck round-bottom flask through a dropping funnel during stirring, dropping was completed within 45min under control of dropping speed, stirring speed was set at 1500rpm, and stirring reaction was carried out for 3.5 hours. And stopping heating after the reaction is finished, and discharging to obtain the silica gel elastomer composition.
Example 5
The preparation method of the silicone gel elastomer composition specifically comprises the following steps:
preparation of polyether modified hydrogen-containing polysiloxane SH 5: a clean and dry 250ml four-necked round bottom flask was taken and sequentially charged with 20g of isopropanol, 15g of allyl polyoxyethylene ether APEG600 (molecular weight 600, molecular formula CH) 2 ＝CHCH 2 O(CH 2 CH 2 O) 12 H) 0.19g of platinum complex (platinum effective concentration 2000 ppm), a synthesis reaction apparatus with oil bath heating was set up, stirring was started, stirring speed was set at 600rpm, and 74g of hydrogen-containing polysiloxane (viscosity 24mPa.s, hydrogen content 0.41%, molecular formula
H(CH 3 ) 2 -Si-O-[Si(CH 3 ) 2 O] 30 -[SiHCH 3 O] 10 -Si-(CH 3 ) 2 H) 70g of isopropanol is weighed and diluted, then the end-side hydrogen-containing polysiloxane isopropanol solution is slowly dripped into a four-necked round bottom flask through a dripping funnel in the stirring process, the dripping speed is controlled to be within 60 minutes, the stirring speed is set to 1000rpm, and the reaction is carried out for 2 hours under normal temperature and normal pressure. After the reaction is finishedAnd (3) starting an oil bath for heating, heating to 80 ℃, connecting a vacuum system and a distillation device, decompressing and distilling for 3 hours to remove and collect low-boiling-point substances, and then closing vacuum and heating to naturally cool the materials in the flask to prepare the polyether modified hydrogen-containing polysiloxane.
Preparation of silicone gel elastomer composition SE 5: a clean and dry 500ml four-neck round-bottom flask is taken, 130g of isohexadecane, 18g of vinyl silicone resin (viscosity 6300mPa.s, vinyl content 0.96%), 75.7g of vinyl-terminated polysiloxane (viscosity 500mPa.s, vinyl content 0.43%), 0.26g of platinum complex (platinum effective concentration 2000 ppm) are sequentially added, a synthesis reaction device with oil bath heating is built, stirring and heating are started, stirring speed is set to 600rpm, temperature is set to 50 ℃, 7.69g of polyether modified hydrogen-containing polysiloxane SH5 and 1.54g of hydrogen-terminated polysiloxane (viscosity 25mPa.s, hydrogen content 0.12%) are weighed, 12g of isohexadecane is added for mixing and dilution, then the mixed solution is slowly dripped into the four-neck round-bottom flask through a dripping funnel in the stirring process, dripping is completed within 60min under control of dripping speed, stirring speed is set to 2000rpm, and stirring reaction is carried out for 3h. And stopping heating after the reaction is finished, and discharging to obtain the silica gel elastomer composition.
Example 6
The preparation method of the silicone gel elastomer composition specifically comprises the following steps:
preparation of polyether modified hydrogen-containing polysiloxane SH 6: a clean and dry 250ml four-necked round bottom flask was taken and sequentially charged with 20g of isopropanol, 15g of allyl polyoxyethylene ether APEG600 (molecular weight 600, molecular formula CH) 2 ＝CHCH 2 O(CH 2 CH 2 O) 12 H) 0.22g of platinum complex (platinum effective concentration 2000 ppm), a synthesis reaction apparatus with oil bath heating was set up, stirring was started, stirring speed was set at 600rpm, 88.8g of end-side hydrogen-containing polysiloxane (viscosity 30mPa.s, hydrogen content 0.62%, molecular formula
H(CH 3 ) 2 -Si-O-[Si(CH 3 ) 2 O] 30 -[SiHCH 3 O] 20 -Si-(CH 3 ) 2 H) And 85g of isopropanol are weighed for dilution, and then the isopropanol solution of the polysiloxane with hydrogen at the end side is leaked through liquid droppingAnd (3) slowly dripping the four-necked round-bottomed flask in the stirring process, controlling the dripping speed to finish dripping within 60min, setting the stirring speed to 1000rpm, and stirring and reacting for 2h at normal temperature and normal pressure. After the reaction is finished, starting an oil bath for heating, heating to 80 ℃, connecting a vacuum system and a distillation device, decompressing and distilling for 3 hours to remove and collect low-boiling-point substances, and then closing vacuum and heating to naturally cool the materials in the flask to prepare the polyether modified hydrogen-containing polysiloxane.
Preparation of silicone gel elastomer composition SE 6: a clean and dry 500ml four-necked round bottom flask was taken, 110g of isohexadecane, 19.5g of vinyl silicone resin (viscosity 6300mPa.s, vinyl content 0.96%), 75.1g of terminal vinyl polysiloxane (viscosity 500mPa.s, vinyl content 0.43%), 0.25g of platinum complex (platinum effective concentration 2000 ppm) were sequentially added, an oil bath heated synthesis reaction device was built, stirring and heating were started, stirring speed was set at 600rpm, temperature was set at 50 ℃, 4.11g of polyether modified hydrogen-containing polysiloxane SH6 and 3.15g of terminal hydrogen-containing polysiloxane (viscosity 25mPa.s, hydrogen content 0.12%) were weighed, 19.6g of isohexadecane was added for mixing and dilution, then the mixed solution was slowly dropped into the four-necked round bottom flask through a dropping funnel in the stirring process, dropping was completed in 60min under control, stirring speed was set at 2000rpm, and stirring reaction was carried out for 3h. And stopping heating after the reaction is finished, and discharging to obtain the silica gel elastomer composition.
The comparative example of the present invention is an illustration of the prior art:
the comparative example adopts vinyl-terminated polysiloxane and hydrogen-terminated polysiloxane, and the silicone elastomer composition is produced by hydrosilylation reaction in a solvent system under the catalysis of platinum complex, and the specific preparation process and steps are as follows:
taking a clean and dry four-neck round-bottom flask, sequentially adding a metered solvent, vinyl-terminated polysiloxane and platinum complex, building a synthesis reaction device with oil bath heating, starting stirring and heating, setting the stirring speed to be 400-600 rpm, setting the temperature to be 40-50 ℃, weighing the metered hydrogen-containing polysiloxane at the end side, adding a proper amount of solvent for mixing and diluting, slowly dripping the mixed solution into the four-neck round-bottom flask through a dropping funnel in the stirring process, controlling the dripping speed to be completed within 30-60 min, setting the stirring speed to be 1000-2000 rpm, and stirring for 3-4 h. And stopping heating after the reaction is finished, and discharging to obtain the organosilicon elastomer composition.
Comparative example 1
A clean and dry 500ml four-neck round-bottom flask is taken, 230g of decamethyl cyclopentasiloxane, 58.6g of vinyl-terminated polysiloxane (viscosity 500mPa.s, vinyl content 0.43%) and 0.15g of platinum complex (platinum effective concentration 2000 ppm) are sequentially added, a synthesis reaction device with oil bath heating is built, stirring and heating are started, stirring speed is set to 400rpm, temperature is set to 40 ℃, 1.87g of hydrogen-terminated polysiloxane (viscosity 7mPa.s, hydrogen content 0.6%) is weighed, 12.5g of decamethyl cyclopentasiloxane is added for mixing and dilution, then the mixed solution is slowly dripped into the four-neck round-bottom flask through a dripping funnel in the stirring process, dripping is completed within 30min under control of dripping speed, stirring speed is set to 1000rpm, and stirring reaction is carried out for 4h. And stopping heating after the reaction is finished, and discharging to obtain the organosilicon elastomer composition.
Comparative example 2
A clean and dry 500ml four-neck round-bottom flask is taken, 250g of decamethyl cyclopentasiloxane, 60.4g of vinyl-terminated polysiloxane (viscosity 500mPa.s, vinyl content 0.43%) and 0.15g of platinum complex (platinum effective concentration 2000 ppm) are sequentially added, a synthesis reaction device with oil bath heating is built, stirring and heating are started, stirring speed is set to 400rpm, temperature is set to 40 ℃, 1.43g of hydrogen-terminated polysiloxane (viscosity 10mPa.s, hydrogen content 0.81%) is weighed, 14.2g of decamethyl cyclopentasiloxane is added for mixing and dilution, then the mixed solution is slowly dripped into the four-neck round-bottom flask through a dripping funnel in the stirring process, dripping is completed within 30min under control of dripping speed, stirring speed is set to 1000rpm, and stirring reaction is carried out for 4h. And stopping heating after the reaction is finished, and discharging to obtain the organosilicon elastomer composition.
Comparative example 3
A clean and dry 500ml four-neck round-bottom flask is taken, 250g of dodecyl methyl pentasiloxane, 57.8g of vinyl-terminated polysiloxane (viscosity 500mPa.s, vinyl content 0.43%) and 0.15g of platinum complex (platinum effective concentration 2000 ppm) are sequentially added, a synthesis reaction device with oil bath heating is built, stirring and heating are started, stirring speed is set to 500rpm, temperature is set to 45 ℃, 1.04g of hydrogen-terminated polysiloxane (viscosity 15mPa.s, hydrogen content 1.06%) is weighed, 18.7g of dodecyl methyl pentasiloxane is added for mixing and dilution, then the mixed solution is slowly dripped into the four-neck round-bottom flask through a dripping funnel in the stirring process, dripping is completed within 45min under control of dripping speed, stirring speed is set to 1500rpm, and stirring reaction is carried out for 3.5h. And stopping heating after the reaction is finished, and discharging to obtain the organosilicon elastomer composition.
Comparative example 4
A clean and dry 500ml four-neck round-bottom flask is taken, 230g of dodecyl pentasiloxane, 56.3g of vinyl-terminated polysiloxane (viscosity 500mPa.s, vinyl content 0.43%) and 0.15g of platinum complex (platinum effective concentration 2000 ppm) are sequentially added, a synthesis reaction device with oil bath heating is built, stirring and heating are started, stirring speed is set to 500rpm, temperature is set to 45 ℃, 4.14g of hydrogen-terminated polysiloxane (viscosity 20mPa.s, hydrogen content 0.26%) is weighed, 12.4g of dodecyl pentasiloxane is added for mixing and dilution, then the mixed solution is slowly dripped into the four-neck round-bottom flask through a dripping funnel in the stirring process, dripping is completed within 45min under control, stirring speed is set to 1500rpm, and stirring reaction is carried out for 3.5h. And stopping heating after the reaction is finished, and discharging to obtain the organosilicon elastomer composition.
Comparative example 5
A clean and dry 500ml four-necked round bottom flask was taken, 230g of isohexadecane, 61.2g of terminal vinyl polysiloxane (viscosity 500mPa.s, vinyl content 0.43%), 0.16g of platinum complex (platinum effective concentration 2000 ppm) were sequentially added, a synthesis reaction device with oil bath heating was built, stirring and heating were started, stirring speed was set at 600rpm, temperature was set at 50 ℃, 2.85g of terminal side hydrogen polysiloxane (viscosity 24mPa.s, hydrogen content 0.41%) was weighed, 11.6g of isohexadecane was added for mixing and dilution, then the mixed solution was slowly dripped into the four-necked round bottom flask through a dripping funnel in the stirring process, the dripping speed was controlled to be completed within 60min, stirring speed was set at 2000rpm, and stirring reaction was carried out for 3h. And stopping heating after the reaction is finished, and discharging to obtain the organosilicon elastomer composition.
Comparative example 6
A clean and dry 500ml four-necked round bottom flask was taken, 210g of isohexadecane, 62.7g of vinyl-terminated polysiloxane (viscosity 500mPa.s, vinyl content 0.43%), 0.16g of platinum complex (platinum effective concentration 2000 ppm) were sequentially added, a synthesis reaction device with oil bath heating was built, stirring and heating were started, stirring speed was set at 600rpm, temperature was set at 50 ℃, 1.93g of hydrogen-terminated polysiloxane (viscosity 30mPa.s, hydrogen content 0.62%) was weighed, 19.7g of isohexadecane was added for mixing and dilution, then the mixed solution was slowly dropped into the four-necked round bottom flask through a dropping funnel in the stirring process, dropping speed was controlled to complete within 60min, stirring speed was set at 2000rpm, and stirring reaction was carried out for 3h. And stopping heating after the reaction is finished, and discharging to obtain the organosilicon elastomer composition.
Performance detection and result analysis
The performance detection method comprises the following steps:
1. appearance and smearing hand feeling detection: sensory inspection.
2. And (3) viscosity detection: measured using a rotational viscometer.
3. Peel strength detection: and (3) uniformly smearing a proper amount of sample on the stainless steel plate, standing for 24 hours at room temperature to prepare a film with the thickness of about 0.3mm, and then using an electronic universal testing machine to conduct 180-degree peeling test on the film on the stainless steel plate.
4. Recipe compatibility detection: and mixing a proper amount of samples with polar solvents (water or alcohols, wherein pure water needs to be added with 5% of nonionic surfactant) and nonpolar solvents (alkanes, oils and siloxanes) respectively, and evaluating the compatibility between the samples and the solvents.
5. Storage stability detection: taking a proper amount of sample, bottling and sealing, storing in a constant temperature test box at 70 ℃ for 1 month, taking out the sample, naturally cooling, and testing the viscosity of the sample by using a rotary viscometer.
TABLE 1 Performance test data for the silica gel elastomer compositions of examples 1-6, comparative examples 1-6
As can be seen from the data in table 1:
in examples 1-6, the polyether modified hydrogen-containing siloxane with different molecular structures is prepared from allyl polyoxyethylene ether with different structures and terminal hydrogen-containing polysiloxane, and 6 polyether modified hydrogen-containing siloxanes with different structures are applied to the preparation of the silicone gel elastomer, so that the prepared product has the advantages of good sensory properties, low viscosity, difficult falling off, smooth coating hand feeling, high formula compatibility (namely high compatibility), high storage stability and the like.
The silicone gel elastomer compositions prepared in comparative documents 1 to 6 were compared with the silicone gel elastomer compositions prepared in examples 1 to 6: the preparation method of the comparative documents 1 to 6 is a preparation method of a silicone gel elastomer composition commonly used in the market at present, which shows that the physicochemical properties of the silicone gel elastomer composition prepared by the preparation method of the invention are superior to those of the silicone gel elastomer composition in the market at present.
In summary, compared with the prior art, the method has the following beneficial effects:
1. the silica gel elastomer composition prepared by the invention has transparent appearance, is easy to paint, has smooth painting hand feeling and has excellent organoleptic properties.
2. The silica gel elastomer composition prepared by the invention has the advantages of low viscosity, good fluidity, simple production operation, low raw material consumption rate and low production cost.
3. The silica gel elastomer composition prepared by the invention has good adhesion with skin, is not easy to peel off and separate from the surface of the skin, and can play a good role in protecting skin barrier.
4. The silicone gel elastomer composition prepared by the invention can be simultaneously matched with water-based and oil-based formulas, and has good product compatibility and high formula flexibility.
5. The silica gel elastomer composition prepared by the invention has high storage stability and long service life.
6. In the preparation method S1 of the invention, allyl polyoxyethylene ether and platinum complex are firstly mixed, and then end-side hydrogen-containing polysiloxane is dripped, and the addition sequence is that even if platinum complex is not added, allyl polyoxyethylene ether and end-side hydrogen-containing polysiloxane can react, but the reaction speed is relatively slow, the reaction speed can be greatly improved after the platinum complex is added, if allyl polyoxyethylene ether and end-side hydrogen-containing polysiloxane are firstly mixed, and then platinum complex is dripped, the explosion polymerization reaction can be caused, so that the reaction is uneven and insufficient, and the synthesis of polyether modified hydrogen-containing polysiloxane is influenced, so that the quality of the finished product of the finally prepared silicone gel elastomer composition is reduced. In the S2 of the preparation method, the solvent, the vinyl silicone resin, the terminal vinyl polysiloxane and the platinum complex are uniformly mixed, and then the operation sequence of dripping the diluted solution of the polyether modified hydrogen polysiloxane and the terminal hydrogen polysiloxane is the same, wherein the polyether modified hydrogen polysiloxane and the terminal hydrogen polysiloxane are mixed because the polyether modified hydrogen polysiloxane and the terminal hydrogen polysiloxane are both hydrogen silicone oil in nature, the mixture has synergistic effect, and the operation of diluting after the mixture is used for reducing the viscosity of the mixed solution. The finished silicone gel elastomer composition produced in the above manner has more excellent quality.
It is noted that relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising one … …" does not exclude the presence of other like elements in a process, method, article, or apparatus that comprises the element.
The above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. A silicone gel elastomer composition for skin care comprising the following components in mass ratio: 36-44% of silica gel elastomer and 56-64% of solvent; the silicone gel elastomer is polymerized in the solvent system.
2. A silicone gel elastomer composition for skin care characterized in that the silicone gel elastomer is synthetically prepared from the following components: vinyl silicone resin, vinyl-terminated polysiloxane, polyether modified hydrogen-containing polysiloxane, hydrogen-terminated polysiloxane and platinum group metal compound, wherein the polyether modified hydrogen-containing siloxane is prepared from allyl polyoxyethylene ether and hydrogen-terminated polysiloxane.
3. A process for the preparation of a silicone gel elastomer composition for skin care, characterized in that it comprises in particular the following steps:
s1, preparing polyether modified hydrogen-containing polysiloxane:
firstly, uniformly stirring and mixing isopropanol, allyl polyoxyethylene ether and platinum group metal compounds, then dropwise adding end-side hydrogen-containing polysiloxane diluted by isopropanol into the mixture for reaction, and carrying out reduced pressure distillation in a vacuum environment after the reaction is finished, and cooling to obtain polyether modified hydrogen-containing polysiloxane;
s2, preparation of a silicone gel elastomer composition:
firstly, adding a solvent into a reaction system to form a solvent-containing system, then adding vinyl silicone resin, vinyl-terminated polysiloxane and platinum group metal compound into the solvent system, and stirring and heating;
weighing polyether modified hydrogen-containing polysiloxane and terminal hydrogen-containing polysiloxane, adding a proper amount of solvent for dilution, dripping the diluted mixed solution into a reaction system after uniform mixing, and discharging after the reaction is finished to obtain the silica gel elastomer composition.
4. The method of preparing a silicone gel elastomer composition for skin care according to claim 3, wherein the allyl polyoxyethylene ether of S1 has a molecular formula of:
CH 2 ＝CHCH 2 O(CH 2 CH 2 O) c h, wherein c=7 to 12, and the molecular weight is 400 to 600.
5. A method of preparing a silicone gel elastomer composition for skin care according to claim 3, wherein the end-side hydrogen-containing polysiloxane in S1 has a viscosity of 7 to 30mpa.s and a hydrogen content of 0.26 to 1.06% (wt) and has a molecular formula of: h (CH) 3 ) 2 -Si-O-[Si(CH 3 ) 2 O] a -[SiHCH 3 O] b -Si-(CH 3 ) 2 H, wherein a=10 to 30 and b=5 to 20.
6. A method of preparing a silicone gel elastomer composition for skin care according to claim 3, wherein the viscosity of the vinyl silicone resin in S2 is 5000 to 15000mpa.s and the vinyl content is 0.54 to 0.98% (wt); preferably, the vinyl silicone resin has a viscosity of 5000 to 8000Pa.s and a vinyl content of 0.78 to 0.98% (wt).
7. A process for the preparation of a silicone gel elastomer composition for skin care according to claim 3, wherein the vinyl terminated polysiloxane in S2 has a viscosity of 80 to 2000mpa.s and a vinyl content of 0.07 to 0.71% (wt) and has the formula:
Vi(CH 3 ) 2 -Si-O-[Si(CH 3 ) 2 O] d -Si-(CH 3 ) 2 vi, where Vi is vinyl CH 2 =ch-, d=100 to 1000; preferably, the vinyl-terminated polysiloxanes have a viscosity of 200 to 1000mPa.s and a vinyl content of 0.22 to 0.63% (wt).
8. A method of preparing a silicone gel elastomer composition for skin care according to claim 3, wherein the hydrogen-containing polysiloxane at the end of S2 has a viscosity of 8 to 70mpa.s and a hydrogen content of 0.04 to 0.19% (wt) and has a molecular formula: h (CH) 3 ) 2 -Si-O-[Si(CH 3 ) 2 O] e -Si-(CH 3 ) 2 H, wherein e = 12-65; preferably, the terminal hydrogen-containing polysiloxanes have a viscosity of from 20 to 50mPa.s and a hydrogen content of from 0.07 to 0.12% (wt).
9. A method of preparing a silicone gel elastomer composition for skin care according to claim 3, wherein the platinum group metal compound is any one of ruthenium and its complex, rhodium and its complex, palladium and its complex, osmium and its complex, iridium and its complex, platinum and its complex, preferably chloroplatinic acid or platinum gold complex, more preferably platinum-divinyl tetramethyl disiloxane complex, and the platinum concentration is 2000ppm.
10. A method of preparing a silicone gel elastomer composition for skin care according to claim 3, wherein the solvent is a mixture of one or more of linear dimethylsiloxane, phenyl trimethicone, dimethylsiloxane ring, hydrocarbon compounds, alkyl benzoates.
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| US6423322B1 (en) * | 1999-05-22 | 2002-07-23 | Wacker Silicones Corporation | Organopolysiloxane gels for use in cosmetics |
| CN109758794A (en) * | 2019-03-20 | 2019-05-17 | 南京瑞思化学技术有限公司 | A kind of preparation method of silicon composition |
| CN112915046A (en) * | 2021-01-28 | 2021-06-08 | 广州市仲沅其新型材料有限公司 | Organic silicon elastomer gel and preparation method and application thereof |
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| US6423322B1 (en) * | 1999-05-22 | 2002-07-23 | Wacker Silicones Corporation | Organopolysiloxane gels for use in cosmetics |
| CN109758794A (en) * | 2019-03-20 | 2019-05-17 | 南京瑞思化学技术有限公司 | A kind of preparation method of silicon composition |
| CN112915046A (en) * | 2021-01-28 | 2021-06-08 | 广州市仲沅其新型材料有限公司 | Organic silicon elastomer gel and preparation method and application thereof |
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