CN110028793A - A kind of elastomer silicone, preparation method and the silicone elastomer gels comprising it - Google Patents
A kind of elastomer silicone, preparation method and the silicone elastomer gels comprising it Download PDFInfo
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- CN110028793A CN110028793A CN201910319703.3A CN201910319703A CN110028793A CN 110028793 A CN110028793 A CN 110028793A CN 201910319703 A CN201910319703 A CN 201910319703A CN 110028793 A CN110028793 A CN 110028793A
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- 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
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- A61Q19/00—Preparations for care of the skin
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Abstract
The present invention provides a kind of elastomer silicone, preparation method and include its silicone elastomer gels.The raw material for preparing of the elastomer silicone includes: the organic hydrogen polysiloxanes containing at least three Si-H unit in a component molecular, average unsaturated fatty hydrocarbons class of the unsaturated group number greater than 1, the polysiloxanes containing at least two unsaturated fatty hydrocarbons bases, d component unsaturated polyether and e component hydrosilylation catalysts in c component molecular in b component molecular.The silicone elastomer gels include carrier fluid and the particle for dispersing the elastomer silicone therein.Silicone elastomer gels provided by the invention both had good compatibility with grease, moisture self-emulsifying can be absorbed again to be used in aqueous care product or cosmetics, and there is good organic-philic silicone oil, transparency, the skin sense that spreadability and silty, silk are sliding, moisten.
Description
Technical field
The invention belongs to organosilicon material technical fields, and in particular to a kind of elastomer silicone, preparation method and packet
Containing its silicone elastomer gels.
Background technique
Silicone elastomer gels are due to special physical performance, for that can make product in personal care product
Sense of touch smooth, as velvet is obtained, while can effectively change the viscosity of product and film forming sense is provided, therefore be widely used in shield
The every field such as skin, color make-up have the biggish market demand.
Elastomer silicone is usually by the polysiloxanes containing Si-H unit and the chemical combination containing unsaturated groups such as vinyl
Object is generated by cross-linking reaction.It is solidifying that CN 1177615A discloses a kind of elastomer comprising volatile low-molecular-weight siloxane
Glue, the raw material used disclose for the linear polysiloxane containing unsaturated alkyl and hydrogeneous MQ silicone resin, CN 106633076A
A kind of silicone elastomer gels and preparation method thereof, the raw material used block poly- silicon for organic hydrogen polysiloxanes and divinyl
Oxygen alkane.The two is that the cross-linking reaction first in the presence of carrier fluid through polysiloxanes prepares harder elastomer silicone,
Then it is dispersed into little particle under shear action, forms silicone elastomer gels.Such product skin sense is more thick and heavy, is often semi-transparent
Bright texture.
CN 108003353A discloses a kind of daily use chemicals elastomer silicone powder and its preparation method and application, with
Hydrogen containing siloxane and bi-vinyl sealing end unsaturated compound be raw material, first pass through emulsion polymerization prepare it is lesser organic
Silicone elastomer particle adds carrier solvent and is swollen to form elastomer gel.This product silk smooth felling is stronger, but transparency compared with
Difference.
It is formed moreover, above-mentioned elastomer silicone using unsaturated polysiloxanes as crosslinking agent, absorbs carrier fluid
The ability of gel is poor.In addition, usually added with the addition such as grease, wax class, active material in personal care product or cosmetics
Agent, above-mentioned silicone elastomer gels property compatible is bad, influences product quality.
In addition, a part of personal care product is water-based system at present, this just also needs silicone elastomer gels to have
Certain hydrophily.CN 101808610A discloses a kind of siloxanes-containing the silicone elastomer being crosslinked from polyoxyalkylene
The personal care composition of organogel, CN 102271655A disclose a kind of silicone paste compositions, CN 101432340A
Disclose a kind of silicone polyether elastomer gels, be all made of unsaturated polyether be crosslinking agent, by with organic hydrogen polysiloxanes
Reaction prepares gel.Containing hydrogen silicone oil is utilized unsaturated polyether by CN 1185314A, CN 1169515C in the presence of an organic
Thickening, then remove after solvent and crosslinking agent reaction prepares gel.Although such silicone elastomer gels have preferable hydrophily,
But slight milky or milky is usually presented in sample, transparency is poor, and skin sense is also poor, and gel has special polyethers
Smell or organic solvent smell, are unfavorable for products application.
Therefore, a kind of with having both the organic of good oleophylic lipid, hydrophily and transparency up for researching and developing in this field
Silicone elastomer gel, to adapt to the application needs of different type care product or cosmetics.
Summary of the invention
In view of the deficiencies of the prior art, the present invention intends to provide a kind of elastomer silicone, its preparation side
Method and silicone elastomer gels comprising it.The silicone elastomer gels not only had good compatibility with grease, but also can
It is used in aqueous care product or cosmetics with absorbing moisture self-emulsifying, and there is good organic-philic silicone oil, transparency, paving
The skin sense that malleability and silty, silk are sliding, moisten.
To achieve this purpose, the present invention adopts the following technical scheme:
In a first aspect, the present invention provides a kind of elastomer silicone, the raw material for preparing of the elastomer silicone includes:
A component: intramolecular contains the organic hydrogen polysiloxanes of at least three Si-H unit；
B component: intramolecular be averaged unsaturated group number be greater than 1 unsaturated fatty hydrocarbons class；
C component: intramolecular contains the polysiloxanes of at least two unsaturated fatty hydrocarbons bases；
D component: unsaturated polyether；
E component: hydrosilylation catalysts；
Si-H unit and the b component in a component and the molar ratio of the unsaturated group in c component are 0.7-3:
1；The b component and the molar ratio of the unsaturated group in the c component are 0.5-1.5:1；Si-H unit in a component
Molar ratio with the unsaturated group in the d component is 1-20:1.
In the present invention, mole of Si-H unit and the b component and the unsaturated group in c component in a component
Than can be 0.7:1,0.8:1,0.9:1,1:1,1.1:1,1.2:1,1.3:1,1.4:1,1.5:1,1.6:1,1.7:1,1.8:
1,1.9:1,2.2:1,2.3:1,2.5:1,2.6:1,2.8:1 or 3:1 etc.；
The b component and the molar ratio of the unsaturated group in the c component can be 0.5:1,0.6:1,0.7:1,
0.8:1,0.9:1,1:1,1.1:1,1.2:1,1.3:1,1.4:1 or 1.5:1 etc.；
Si-H unit in a component and the molar ratio of the unsaturated group in the d component can be 1:1,2:1,
3:1、4:1、5:1、5.5:1、6:1、6.5:1、7:1、7.5:1、8:1、8.5:1、9:1、9.5:1、10:1、11:1、12:1、13:
1,14:1,15:1,16:1,17:1,18:1,19:1 or 20:1 etc..
The present invention uses above-mentioned each component as raw material, under the action of hydrosilylation catalysts, organic poly- silicon oxygen of hydrogen
Si-H in alkane can occur addition reaction with unsaturated groups such as carbon-carbon double bonds and be crosslinked, to form elastomer silicone.
By the mutual cooperation between each raw material, the elastomer silicone made not only had good compatibility with grease, but also had
Good hydrophily, and there is transparent texture, it is conveniently used in all kinds of care products or cosmetic formulations.
A component, b component, the ratio of the Si-H unit in c component and unsaturated group directly affect elastomer silicone
The degree of cross linking.If b component and the ratio of the unsaturated group in c component are excessively high, the elastomer silicone degree of cross linking is too low, then it is strong
Spend poor, product is more greasy, and skin sense is poor, or even is difficult to that silicone elastomer gels are made；If the insatiable hunger in b component and c component
Too low with the ratio of group, then the degree of cross linking of elastomer silicone is excessively high, and the particle that is formed is harder after shearing dispersion, skin sense compared with
Difference.The present invention helps to have silicone elastomer gels by the ratio of selection suitable Si-H unit and unsaturated group
The skin sense for having silty, silk sliding.
C component can form cross-linked structure with organic hydrogen polysiloxanes, and contain unsaturated fatty hydrocarbons base
Polysiloxanes chain length is longer, and the cross-linking system after reacting with organic hydrogen polysiloxanes is capable of providing greater room, improves organosilicon
The elasticity of elastomer improves comfort.If but its too high levels, the anti-of organic hydrogen polysiloxanes and unsaturated polyether can be unfavorable for
It answers, to influence the hydrophily of elastomer silicone.Unsaturated fatty hydrocarbons class helps to improve elastomer silicone and grease
Compatibility, but in the care product or cosmetics of application elastomer silicone the usual additive amount of organosilicon products such as silicone oil compared with
More, if the content of unsaturated fatty hydrocarbons class is excessive, the elastomer silicone that will lead to and organic silicone oil compatibility become
Difference.
Unsaturated polyether helps to improve the hydrophily of elastomer silicone, if its additive amount is very few, what is obtained is organic
The hydrophily of silicone elastomer is poor；But if its additive amount is excessive, and the transparency that will lead to elastomer silicone is poor.
As the preferred technical solution of the present invention, the structural formula of the organic hydrogen polysiloxanes is R3SiO(R1R2SiO)y
(R1HSiO)zSiR3；
Wherein, R1、R2It is each independently phenyl or containing 1-20 (such as 1,2,3,4,5,6,8
A, 10,12,13,15,16,18 or 20 etc.) carbon atom alkyl；
R be hydrogen atom, phenyl or containing 1-20 (such as 1,2,3,4,5,6,8,10,12,
13,15,16,18 or 20 etc.) alkyl of carbon atom；
Y is the integer of 0-400, for example, can be 0,5,10,15,20,30,40,50,60,80,100,120,150,180,
200,250,300,350 or 400 etc.；
Z is the integer of 3-200, for example, can be 3,4,5,6,8,10,12,13,15,16,18,20,30,50,60,80,
100,120,140,150,160,180 or 200 etc..
Preferably, it is 0.05-0.9% that the H in the Si-H unit, which accounts for the weight percent of a component,；Such as it can be with
0.05%, 0.06%, 0.08%, 0.1%, 0.15%, 0.2%, 0.25%, 0.3%, 0.35%, 0.4%, 0.45%,
0.5%, 0.55%, 0.6%, 0.65%, 0.7%, 0.75%, 0.8%, 0.85% or 0.9% etc..
As the preferred technical solution of the present invention, the b group is divided into the mixing of b1 component or b1 component and b2 component
Object, the b1 group are divided into the aliphatic hydrocarbon that intramolecular contains at least two unsaturated groups, and the b2 group is divided into intramolecular and contains
There is the mixture of the aliphatic hydrocarbon of a unsaturated group.
Preferably, the b1 group be selected from intramolecular contain 6-20 (such as 6,7,8,9,10,11,
12,13,14,15,16,17,18,19 or 20) alkadienes, diyne or the eneyne chemical combination of carbon atom
One of object or at least two combination.
Preferably, the b1 group is selected from 1,7- octadiene, 1,9- decadinene, 1,11-, 12 diene, 1,13- 14 pairs
One of alkene, 20 diene of 1,19- or 1,5- hexadiine or at least two combination.
Preferably, the b2 group is selected from the monoolefine or single alkynes that intramolecular contains 10-18 carbon atom.
Preferably, the molar ratio of the b2 component and b1 component is less than 0.3:1.
The usual smell of aliphatic hydrocarbon b1 component containing multiple unsaturated groups is heavier, if addition is excessive, will affect product
Quality；A part of b1 component is replaced by using b2 component, while guaranteeing elastomer silicone and gel compatibility, again
Its smell can be mitigated.If but the too high levels of b2 component, the degree of cross linking of elastomer silicone can be reduced, elastomer silicone is influenced
The skin sense of gel.
As the preferred technical solution of the present invention, the c group is selected from in the polymer such as following formula I or Formula II structure
One kind or at least two combination:
In Formulas I and Formula II, R3For monovalence unsaturated fatty hydrocarbons base；
U is the integer of 10-400, for example, can be 10,15,20,25,30,40,50,60,80,100,120,150,180,
200,220,250,280,300,320,350,380 or 400 etc.；
V is the integer of 2-20, such as can be 2,3,4,5,6,8,10,12,13,15,16,18 or 20 etc..
Preferably, R3Selected from CH2=CH-, CH2=CHCH2-、CH2=C (CH3)CH2Or one of CH ≡ C-.
Preferably, the integer that u is 10-300 in Formulas I and Formula II.
Preferably, the molar ratio of the Si-H unit in a component and the b component and the unsaturated group in c component
For 0.9-2:1.
As the preferred technical solution of the present invention, the d group is selected from one in the polymer with following formula III structure
Kind or at least two combination:
In formula III, R4For unsaturated fatty hydrocarbons base；
R5Selected from hydroxyl, allyloxy, containing 1-20 (such as 1,2,3,4,5,6,8,10,
12,13,15,16,18 or 20 etc.) alkoxy of carbon atom or contain 1-20 carbon atom (such as 1,2
A, 3,4,5,6,8,10,12,13,15,16,18 or 20 etc.) one of ester group；
N, m is the integer more than or equal to 0 and n+m=4~50.
It should be noted that d component can be one or more of the compound with formula III structure in the present invention
Mixture.For a kind of specific unsaturated polyether, ethylene glycol unit or propylene glycol units can be free of in strand, i.e.,
N or m can be 0.
Preferably, R4For allyl.
Preferably, n+m=8~20.
Preferably, the molar ratio of ethylene glycol unit and propylene glycol units is 0.8-14:1 in the d component, such as be can be
0.8:1、0.9:1、1:1、1.5:1、2:1、2.5:1、3:1、3.5:1、4:1、4.5:1、5:1、5.5:1、6:1、6.5:1、7:1、
7.5:1,8:1,8.5:1,9:1,9.5:1,10:1,10.5:1,11:1,11.5:1,12:1,12.5:1,13:1,13.5:1 or
14:1 etc.；Further preferably 2-9:1.
Unsaturated polyether helps to improve the hydrophily of elastomer silicone.Ethylene glycol unit is more in d component, hydrophilic
Property it is better, but reactivity it is poor；Propylene glycol units are more in d component, and reactivity is better, but hydrophily is poor.The present invention is to d
The ratio of ethylene glycol unit and propylene glycol units carries out preferably, not only having ensure that the hydrophily of elastomer silicone, but also protect in component
The abundant progress of reaction is demonstrate,proved.
Preferably, the type of unsaturated polyether is no more than 3 kinds in the d component, and any one unsaturated polyether is in institute
The molar content in d component is stated not less than 5%.
Most polyethers product all has faint odor, and due to the reactivity of different polyethers difference, excessive product
It is unstable kind to will lead to reaction rate, transformation efficiency decline.
Preferably, the Si-H unit in a component and the molar ratio of the unsaturated group in the d component are 5-10:
1。
Although unsaturated polyether helps to improve the hydrophily of elastomer silicone, if its additive amount is excessive, can lead
Cause the transparency of elastomer silicone poor.
Preferably, the e group is selected from the complex compound of chloroplatinic acid, platinum black or chloroplatinic acid and unsaturated organosilicon.
Preferably, the pt atom in the e component accounts for the quality of a component, b component, c component and d component gross mass
Score is 1-1000ppm；Such as can be 1ppm, 5ppm, 10ppm, 20ppm, 50ppm, 100ppm, 200ppm, 300ppm,
500ppm, 600ppm, 800ppm or 1000ppm etc..
Second aspect, the present invention provide a kind of preparation method of above-mentioned elastomer silicone, the preparation method is that:
A component, b component, c component, d component and e component are mixed, temperature reaction obtains the elastomer silicone.
As the preferred technical solution of the present invention, the mixed method are as follows: first by a component, b component, c component and d group
Point mix at normal temperature, then heat to 35-60 DEG C (such as 35 DEG C, 38 DEG C, 40 DEG C, 42 DEG C, 45 DEG C, 48 DEG C, 50 DEG C, 52 DEG C,
55 DEG C, 58 DEG C or 60 DEG C etc.), e component is added and is mixed.
Unless otherwise specified, " room temperature " each means 20-23 DEG C in the present invention.The present invention prepares the process of elastomer silicone
Solvent is not added, each raw material is not easy to disperse, and by first mixing a component, b component, c component and d component at normal temperature, then rises
Temperature is mixed with e component, is facilitated each raw material and is uniformly mixed, reaction is promoted sufficiently to carry out.
Preferably, the temperature of the reaction is 70-90 DEG C, such as can be 70 DEG C, 72 DEG C, 73 DEG C, 75 DEG C, 76 DEG C, 78
DEG C, 80 DEG C, 82 DEG C, 83 DEG C, 85 DEG C, 86 DEG C, 88 DEG C or 90 DEG C etc.；Time is 0.5-1.5h, for example, can be 0.5h, 0.6h,
0.8h, 0.9h, 1h, 1.2h, 1.3h or 1.5h etc..
Preferably, also proceed as follows after the completion of reaction: by reaction product 90-105 DEG C (such as 90 DEG C, 91 DEG C,
92 DEG C, 95 DEG C, 96 DEG C, 98 DEG C, 100 DEG C, 102 DEG C, 103 DEG C or 105 DEG C etc.) under dry 8-12h (such as 8h, 8.5h, 9h,
9.5h, 10h, 10.5h, 11h, 11.5h or 12h etc.).
It is thermally dried processing after reaction, assists in removing remaining volatile materials, mitigates the smell of product.
The third aspect, the present invention provide a kind of silicone elastomer gels, including carrier fluid and are scattered in the carrier
Silicone elastomer particles in fluid；
The silicone elastomer particles are dispersed by elastomer silicone that first aspect present invention provides is clipped.
The present invention is not particularly limited the method for the shearing dispersion, illustratively, can be mechanical using crusher
Dispersion.
As the preferred technical solution of the present invention, partial size≤5 μm of the silicone elastomer particles.
Preferably, it is 1-50mm that the carrier fluid, which is selected from alcohols, hydro carbons, esters, fatty oil or viscosity,2The low viscosity silicon of/s
One of oxygen alkane or at least two combination.
Preferably, the alcohols is selected from the group of one of ethyl alcohol, cyclohexanol, propylene glycol or glycerine or at least two
It closes.
Preferably, the hydro carbons is selected from the combination of one of Permethyl 99A, isohexadecane or mineral oil or at least two.
Preferably, the fatty oil is selected from one of corn oil, soya-bean oil, olive oil, coconut oil or shea butter or at least
Two kinds of combination.
Preferably, the low viscosity silicone is selected from linear alkyl siloxanes and/or cyclic alkyl siloxane.
Preferably, the linear alkyl siloxanes is selected from hexamethyldisiloxane, octamethyltrisiloxane, four silicon of decamethyl
One of oxygen alkane or seven Methyl Octyl trisiloxanes or at least two combination.
Preferably, the cyclic alkyl siloxane is selected from trimethyl cyclotrisiloxane, octamethylcy-clotetrasiloxane, decamethyl
One of six siloxanes of cyclopentasiloxane or ten diformazan basic rings or at least two combination.
Fourth aspect, the present invention provide a kind of purposes of above-mentioned silicone elastomer gels, and the elastomer silicone is solidifying
Glue is used for care product or cosmetics.Illustratively, antiperspirant, BB frost, skin cream, lipstick, foundation emulsion or concealing be may be used as
Carrier and/or thickener in cream.
Compared with prior art, the invention has the following advantages:
Silicone elastomer gels provided by the invention not only have good compatibility with grease, but also moisture can be absorbed certainly
Emulsification is used in aqueous care product or cosmetics, and has good organic-philic silicone oil, transparency, spreadability and powder
Sliding, the moist skin sense of matter, silk, can be used for preparing transparent care product or cosmetics.
Specific embodiment
Below by specific embodiment to further illustrate the technical scheme of the present invention.Those skilled in the art should be bright
, the described embodiments are merely helpful in understanding the present invention, should not be regarded as a specific limitation of the invention.
Embodiment 1
The present embodiment provides a kind of silicone elastomer gels, and it is as follows to prepare raw material:
A component: intramolecular contains the organic hydrogen polysiloxanes of at least three Si-H unit:
Average formula is Me3SiO(Me2SiO)300(MeHSiO)15SiMe3；
B component: intramolecular be averaged unsaturated group number be greater than 1 unsaturated fatty hydrocarbons class:
17 diene of 1,16-；
C component: intramolecular contains the polysiloxanes of at least two unsaturated fatty hydrocarbons bases:
D component: unsaturated polyether: CH2=CHCH2O(C2H4O)8(C3H6O)4H；
E component: hydrosilylation catalysts: aqueous isopropanol (the concentration 1000mg/kg, with H of chloroplatinic acid2PtCI6Concentration
It calculates).
Preparation step is as follows:
(1) 100g a component, 3g b component, 160g c component and 10g d component is added under room temperature in the reaction vessel, it is high
Speed is stirred；50 DEG C are then heated to, 3g e component is added, is warming up to 80 DEG C after mixing, is reacted 1 hour, then 105
It is sufficiently 8 hours dry at DEG C, obtain elastomer silicone；
(2) the elastomer silicone crusher strength that step (1) obtains is crushed to partial size≤5 μm, 125g six is added
Tetramethyldisiloxane is stirred mixing, and silicone elastomer gels are generated when being vigorously stirred, and flies viscosimeter with rich strangle
Measuring its viscosity is about 700000mm2/s。
Embodiment 2
The present embodiment provides a kind of silicone elastomer gels, and it is as follows to prepare raw material:
A component: intramolecular contains the organic hydrogen polysiloxanes of at least three Si-H unit:
Average formula is Me3SiO(Me2SiO)205(MePhSiO)20(MeHSiO)15SiMe3；
B component: intramolecular be averaged unsaturated group number be greater than 1 unsaturated fatty hydrocarbons class:
Including b1 component 1,7- octadiene and b2 component laurylene；
C component: intramolecular contains the polysiloxanes of at least two unsaturated fatty hydrocarbons bases:
D component: unsaturated polyether: CH2=CHCH2O(C2H4O)10(C3H6O)3CH3；
E component: hydrosilylation catalysts: aqueous isopropanol (the concentration 1000mg/kg, with H of chloroplatinic acid2PtCI6Concentration
It calculates).
Preparation step is as follows:
(1) 100g a component, 1.5g b1 component, 0.3g b2 component, 200g c group is added under room temperature in the reaction vessel
Divide and 10g d component, high-speed stirred mix；50 DEG C are then heated to, 5g e component is added, is warming up to 80 DEG C after mixing,
Reaction 45 minutes, then sufficiently dried 8 hours at 105 DEG C, obtain elastomer silicone；
(2) the elastomer silicone crusher strength that step (1) obtains is crushed to partial size≤5 μm, it is different that 150g is added
Dodecane and 30g coconut oil are stirred mixing, and silicone elastomer gels are generated when being vigorously stirred, and fly to glue with rich strangle
Degree measure its viscosity is about 600000mm2/s。
Embodiment 3
The present embodiment provides a kind of silicone elastomer gels, and it is as follows to prepare raw material:
A component: intramolecular contains the organic hydrogen polysiloxanes of at least three Si-H unit:
Average formula is Me3SiO(Me2SiO)255(MeHSiO)10SiMe3；
B component: intramolecular be averaged unsaturated group number be greater than 1 unsaturated fatty hydrocarbons class:
Including 20 diene of b1 component 1,19- and b2 component hexadecylene；
C component: intramolecular contains the polysiloxanes of at least two unsaturated fatty hydrocarbons bases:
D component: unsaturated polyether: CH2=CHCH2O(C2H4O)15(C3H6O)5CH3；
E component: hydrosilylation catalysts: aqueous isopropanol (the concentration 1000mg/kg, with H of chloroplatinic acid2PtCI6Concentration
It calculates).
Preparation step is as follows:
(1) be added in the reaction vessel under room temperature 120g a component, 3g b1 component, 0.5g b2 component, 60g c component and
10g d component, high-speed stirred mixing；50 DEG C are then heated to, 5g e component is added, is warming up to 80 DEG C after mixing, reaction
1.5 hours, then sufficiently dried 8 hours at 105 DEG C, obtain elastomer silicone；
(2) the elastomer silicone crusher strength that step (1) obtains is crushed to partial size≤5 μm, 100g seven is added
Methyl Octyl trisiloxanes is stirred mixing, and silicone elastomer gels are generated when being vigorously stirred, and flies to glue with rich strangle
Degree measure its viscosity is about 580000mm2/s。
Embodiment 4
The present embodiment provides a kind of silicone elastomer gels, and it is as follows to prepare raw material:
A component: intramolecular contains the organic hydrogen polysiloxanes of at least three Si-H unit:
Average formula is Me3SiO(Me2SiO)310(MeHSiO)15SiMe3；
B component: intramolecular be averaged unsaturated group number be greater than 1 unsaturated fatty hydrocarbons class:
Including b1 component 1,5- hexadiine and b2 component laurylene；
C component: intramolecular contains the polysiloxanes of at least two unsaturated fatty hydrocarbons bases:
D component: unsaturated polyether: CH2=CHCH2O(C2H4O)12(C3H6O)2CH3；
E component: hydrosilylation catalysts: aqueous isopropanol (the concentration 1000mg/kg, with H of chloroplatinic acid2PtCI6Concentration
It calculates).
Preparation step is as follows:
(1) 160g a component, 1.5g b1 component, 0.6g b2 component, 150g c group is added under room temperature in the reaction vessel
Divide and 10g d component, high-speed stirred mix；50 DEG C are then heated to, 10g e component is added, is warming up to 80 DEG C after mixing,
Reaction 1.5 hours, then sufficiently dried 12 hours at 105 DEG C, obtain elastomer silicone；
(2) the elastomer silicone crusher strength that step (1) obtains is crushed to partial size≤5 μm, 150g ten is added
Methyl cyclopentasiloxane is stirred mixing, and silicone elastomer gels are generated when being vigorously stirred, and flies viscosity with rich strangle
Measure its viscosity is about 650000mm2/s。
Embodiment 5
The present embodiment provides a kind of silicone elastomer gels, the difference from embodiment 1 is that, d component are as follows: CH2=
CHCH2O(C2H4O)12H。
Embodiment 6
The present embodiment provides a kind of silicone elastomer gels, the difference from embodiment 1 is that, d component are as follows: CH2=
CHCH2O(C3H6O)12H。
Embodiment 7
The present embodiment provides a kind of silicone elastomer gels, the difference from embodiment 1 is that, b component is by 2.5g b1 group
Divide 17 diene of 1,16- and 0.5g b2 component laurylene composition (molar ratio 1:0.3).
Embodiment 8
The present embodiment provides a kind of silicone elastomer gels, the difference from embodiment 1 is that, the dosage of d component is 15g
(a component Si-H and d component double bond molar ratio=3:1).
Embodiment 9
The present embodiment provides a kind of silicone elastomer gels, the difference from embodiment 1 is that, the dosage of d component is 3g
(a component Si-H and d component double bond molar ratio=15:1).
Comparative example 1
The present embodiment provides a kind of silicone elastomer gels, the difference from embodiment 1 is that, the dosage of b component is 9g,
The dosage of c component is 250g (double bond molar ratio=0.5:1 in Si-H and b component and c component in a component).
Comparative example 2
The present embodiment provides a kind of silicone elastomer gels, the difference from embodiment 1 is that, the dosage of b component is 1g,
The dosage of c component is 50g (double bond molar ratio=4:1 in Si-H and b component and c component in a component).
Comparative example 3
The present embodiment provides a kind of silicone elastomer gels, the difference from embodiment 1 is that, the dosage of b component is
The dosage of 1.2g, c component is 230g.(b component double bond and c component double bond molar ratio=1:4)
Comparative example 4
The difference from embodiment 1 is that not adding b component, the dosage of c component is 300g (double bond total amount is constant).
Comparative example 5
The difference from embodiment 1 is that not adding c component, the dosage of b component is 6.3g (double bond total amount is constant).
Comparative example 6
The difference from embodiment 1 is that not adding d component.
With 20 testers to the oleophylic of above-described embodiment 1-12 and comparative example 1-3 silicone elastomer gels provided
Lipid, organic-philic silicone oil, hydrophily, skin sense, spreadability and the transparency are evaluated, and evaluation result is divided into 1 to 10 grades,
10 be it is best, statistical result is as shown in table 1 below:
Table 1
As can be seen from Table 1, machine silicone elastomer gel provided by the invention has good oleophylic lipid, organic-philic silicone oil
Property, hydrophily, skin sense, spreadability and the transparency.
Wherein, the content of d component unsaturated polyether is more in embodiment 8, leads to the transparency of silicone elastomer gels
It is relatively low, and its smell is heavier, is unfavorable for applying；The content of d component unsaturated polyether is less in embodiment 9, leads to organosilicon bullet
The hydrophily of elastomeric gel is relatively low.
The double bond content of b component and c component is excessive in comparative example 1, causes the degree of cross linking of silicone elastomer gels too low,
Skin sense is poor, is unsatisfactory for application demand；The double bond content of b component and c component is very few in comparative example 2, leads to elastomer silicone
The degree of cross linking of gel is excessively high, and skin sense and spreadability are poor.
B constituent content in comparative example 3 and comparative example 4 is very few, and c constituent content is excessive, leads to silicone elastomer gels
Oleophylic lipid and hydrophily decline；B component is only added in comparative example 5, does not add c component, causes elastomer silicone solidifying
The oleophylic lipid of glue, skin sense, spreadability and the transparency are poor.
D component unsaturated polyether is not added in comparative example 6, causes the hydrophily of silicone elastomer gels too low, is discontented with
Sufficient application demand.
The Applicant declares that the foregoing is merely a specific embodiment of the invention, but protection scope of the present invention not office
It is limited to this, it should be clear to those skilled in the art, any to belong to those skilled in the art and take off in the present invention
In the technical scope of dew, any changes or substitutions that can be easily thought of, and all of which fall within the scope of protection and disclosure of the present invention.
Claims (10)
1. a kind of elastomer silicone, which is characterized in that the raw material for preparing of the elastomer silicone includes:
A component: intramolecular contains the organic hydrogen polysiloxanes of at least three Si-H unit；
B component: intramolecular be averaged unsaturated group number be greater than 1 unsaturated fatty hydrocarbons class；
C component: intramolecular contains the polysiloxanes of at least two unsaturated fatty hydrocarbons bases；
D component: unsaturated polyether；
E component: hydrosilylation catalysts；
Si-H unit and the b component in a component and the molar ratio of the unsaturated group in c component are 0.7-3:1；Institute
The molar ratio for stating b component and the unsaturated group in the c component is 0.5-1.5:1；Si-H unit and institute in a component
The molar ratio for stating the unsaturated group in d component is 1-20:1.
2. elastomer silicone according to claim 1, which is characterized in that the structural formula of the organic hydrogen polysiloxanes is
R3SiO(R1R2SiO)y(R1HSiO)zSiR3；
Wherein, R1、R2It is each independently phenyl or the alkyl containing 1-20 carbon atom, R is hydrogen atom, phenyl or contains 1-
The alkyl of 20 carbon atoms, y are the integer of 0-400, and z is the integer of 3-200；
Preferably, y is the integer of 90-300, and z is the integer of 15-150；
Preferably, it is 0.05-0.9% that the H in the Si-H unit, which accounts for the weight percent of a component,.
3. elastomer silicone according to claim 1 or 2, which is characterized in that the b group is divided into b1 component or b1
The mixture of component and b2 component, the b1 group are divided into the aliphatic hydrocarbon that intramolecular contains at least two unsaturated groups, institute
It states b2 group and is divided into the mixture that intramolecular contains the aliphatic hydrocarbon of a unsaturated group；
Preferably, the b1 group is selected from intramolecular and contains in the alkadienes, diyne or yne compounds of 6-20 carbon atom
One kind or at least two combination；
Preferably, the b1 group is selected from 1,7- octadiene, 1,9- decadinene, 1,11-, 12 diene, 1,13-, 14 diene, 1,
One of 20 diene of 19- or 1,5- hexadiine or at least two combination；
Preferably, the b2 group is selected from the monoolefine or single alkynes that intramolecular contains 10-18 carbon atom；
Preferably, the molar ratio of the b2 component and b1 component is less than 0.3:1.
4. elastomer silicone according to claim 1-3, which is characterized in that the c group, which is selected from, to be had such as
One of polymer of following formula I or Formula II structure or at least two combination:
Wherein, R3For monovalence unsaturated fatty hydrocarbons base, u is the integer of 10-400, and v is the integer of 2-20；
Preferably, R3Selected from CH2=CH-, CH2=CHCH2-、CH2=C (CH3)CH2Or one of CH ≡ C-；
Preferably, the integer that u is 10-300 in Formulas I and Formula II；
Preferably, the Si-H unit in a component and the molar ratio of the unsaturated group in the b component and c component are
0.9-2:1。
5. elastomer silicone according to claim 1-4, which is characterized in that the d group, which is selected from, to be had such as
One of polymer of Formula Il I structure or at least two combination:
Wherein, R4For unsaturated fatty hydrocarbons base, R5Selected from hydroxyl, allyloxy, the alkoxy containing 1-20 carbon atom or contain
There is one of the ester group of 1-20 carbon atom, n, m are the integer more than or equal to 0 and n+m=4~50；
Preferably, R4For allyl；
Preferably, n+m=8~20；
Preferably, the molar ratio of ethylene glycol unit and propylene glycol units is 0.8-14:1, further preferably 2- in the d component
9:1；
Preferably, the type of unsaturated polyether is no more than 3 kinds in the d component, and any one unsaturated polyether is in the d group
Molar content in point is not less than 5%；
Preferably, the Si-H unit in a component and the molar ratio of the unsaturated group in the d component are 5-10:1；
Preferably, the e group is selected from the complex compound of chloroplatinic acid, platinum black or chloroplatinic acid and unsaturated organosilicon；
Preferably, the pt atom in the e component accounts for the mass fraction of a component, b component, c component and d component gross mass
For 1-1000ppm.
6. a kind of preparation method of elastomer silicone as described in any one in claim 1-5, which is characterized in that the preparation
Method are as follows:
A component, b component, c component, d component and e component are mixed, temperature reaction obtains the elastomer silicone.
7. preparation method according to claim 6, which is characterized in that the mixed method are as follows: first by a component, b group
Point, c component and d component mix at normal temperature, then heat to 35-60 DEG C, e component be added and is mixed；
Preferably, the temperature of the reaction is 70-90 DEG C, time 0.5-1.5h；
Preferably, it also proceeds as follows after the completion of reaction: reaction product is dried into 8-12h at 90-105 DEG C.
8. a kind of silicone elastomer gels, which is characterized in that the silicone elastomer gels include carrier fluid and dispersion
Silicone elastomer particles in the carrier fluid；
The silicone elastomer particles are dispersed by the described in any item elastomer silicones of claim 1-5 are clipped.
9. silicone elastomer gels according to claim 8, which is characterized in that the grain of the silicone elastomer particles
Diameter≤5 μm；
Preferably, it is 1-50mm that the carrier fluid, which is selected from alcohols, hydro carbons, esters, fatty oil or viscosity,2The low viscosity silicone of/s
One of or at least two combination；
Preferably, the alcohols is selected from the combination of one of ethyl alcohol, cyclohexanol, propylene glycol or glycerine or at least two；
Preferably, the hydro carbons is selected from the combination of one of Permethyl 99A, isohexadecane or mineral oil or at least two；
Preferably, the fatty oil is selected from one of corn oil, soya-bean oil, olive oil, coconut oil or shea butter or at least two
Combination；
Preferably, the low viscosity silicone is selected from linear alkyl siloxanes and/or cyclic alkyl siloxane；
Preferably, the linear alkyl siloxanes is selected from hexamethyldisiloxane, octamethyltrisiloxane, decamethyl tetrasiloxane
Seven one of Methyl Octyl trisiloxanes or at least two combination；
Preferably, the cyclic alkyl siloxane is selected from trimethyl cyclotrisiloxane, octamethylcy-clotetrasiloxane, decamethyl ring penta
One of six siloxanes of siloxanes or ten diformazan basic rings or at least two combination.
10. a kind of purposes of silicone elastomer gels as claimed in claim 8 or 9, which is characterized in that the organosilicon bullet
Elastomeric gel is used for care product or cosmetics.
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