CN104817699A - Vinyl silicone oil and preparation method thereof - Google Patents
Vinyl silicone oil and preparation method thereof Download PDFInfo
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- CN104817699A CN104817699A CN201510199209.XA CN201510199209A CN104817699A CN 104817699 A CN104817699 A CN 104817699A CN 201510199209 A CN201510199209 A CN 201510199209A CN 104817699 A CN104817699 A CN 104817699A
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- 229920002545 silicone oil Polymers 0.000 title claims abstract description 29
- 229920002554 vinyl polymer Polymers 0.000 title claims abstract description 25
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- -1 polysiloxane Polymers 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 9
- 238000007259 addition reaction Methods 0.000 claims abstract description 6
- 239000001257 hydrogen Substances 0.000 claims abstract description 6
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 6
- 230000000694 effects Effects 0.000 claims abstract description 5
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 5
- 230000003472 neutralizing effect Effects 0.000 claims abstract description 3
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 20
- 238000006243 chemical reaction Methods 0.000 claims description 13
- 239000003054 catalyst Substances 0.000 claims description 12
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 10
- BITPLIXHRASDQB-UHFFFAOYSA-N ethenyl-[ethenyl(dimethyl)silyl]oxy-dimethylsilane Chemical compound C=C[Si](C)(C)O[Si](C)(C)C=C BITPLIXHRASDQB-UHFFFAOYSA-N 0.000 claims description 10
- 229910052697 platinum Inorganic materials 0.000 claims description 10
- 238000012676 equilibrium polymerization Methods 0.000 claims description 9
- HMMGMWAXVFQUOA-UHFFFAOYSA-N octamethylcyclotetrasiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O1 HMMGMWAXVFQUOA-UHFFFAOYSA-N 0.000 claims description 9
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 claims description 8
- 230000002745 absorbent Effects 0.000 claims description 6
- 239000002250 absorbent Substances 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- PMSZNCMIJVNSPB-UHFFFAOYSA-N bis(ethenyl)silicon Chemical compound C=C[Si]C=C PMSZNCMIJVNSPB-UHFFFAOYSA-N 0.000 claims description 5
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 5
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 5
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- 238000007171 acid catalysis Methods 0.000 claims description 4
- 230000015572 biosynthetic process Effects 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 4
- 238000003786 synthesis reaction Methods 0.000 claims description 4
- 238000010521 absorption reaction Methods 0.000 claims description 3
- 239000006229 carbon black Substances 0.000 claims description 3
- 238000006386 neutralization reaction Methods 0.000 claims description 3
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 2
- 239000003377 acid catalyst Substances 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 229910000077 silane Inorganic materials 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- 125000002769 thiazolinyl group Chemical group 0.000 claims description 2
- 239000007788 liquid Substances 0.000 abstract description 8
- 229910052760 oxygen Inorganic materials 0.000 abstract description 4
- 238000004806 packaging method and process Methods 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 3
- 239000011203 carbon fibre reinforced carbon Substances 0.000 abstract description 3
- 239000001301 oxygen Substances 0.000 abstract description 3
- FSIJKGMIQTVTNP-UHFFFAOYSA-N bis(ethenyl)-methyl-trimethylsilyloxysilane Chemical compound C[Si](C)(C)O[Si](C)(C=C)C=C FSIJKGMIQTVTNP-UHFFFAOYSA-N 0.000 abstract description 2
- 239000004205 dimethyl polysiloxane Substances 0.000 abstract description 2
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 abstract description 2
- 125000002947 alkylene group Chemical group 0.000 abstract 2
- 125000004122 cyclic group Chemical group 0.000 abstract 2
- VMAWODUEPLAHOE-UHFFFAOYSA-N 2,4,6,8-tetrakis(ethenyl)-2,4,6,8-tetramethyl-1,3,5,7,2,4,6,8-tetraoxatetrasilocane Chemical compound C=C[Si]1(C)O[Si](C)(C=C)O[Si](C)(C=C)O[Si](C)(C=C)O1 VMAWODUEPLAHOE-UHFFFAOYSA-N 0.000 abstract 1
- 230000001133 acceleration Effects 0.000 abstract 1
- 238000001914 filtration Methods 0.000 abstract 1
- 239000000203 mixture Substances 0.000 abstract 1
- 239000000047 product Substances 0.000 description 22
- 238000001035 drying Methods 0.000 description 10
- 238000003756 stirring Methods 0.000 description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 9
- 239000000463 material Substances 0.000 description 9
- 239000000741 silica gel Substances 0.000 description 7
- 229910002027 silica gel Inorganic materials 0.000 description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 6
- 239000003921 oil Substances 0.000 description 6
- 230000035699 permeability Effects 0.000 description 6
- 239000006227 byproduct Substances 0.000 description 5
- 239000000470 constituent Substances 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 238000009413 insulation Methods 0.000 description 5
- 229910052710 silicon Inorganic materials 0.000 description 5
- 239000010703 silicon Substances 0.000 description 5
- 238000000967 suction filtration Methods 0.000 description 5
- 125000000217 alkyl group Chemical group 0.000 description 3
- 125000003118 aryl group Chemical group 0.000 description 3
- 239000004721 Polyphenylene oxide Substances 0.000 description 2
- 239000000460 chlorine Chemical group 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000005538 encapsulation Methods 0.000 description 2
- 150000002431 hydrogen Chemical group 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 229920000570 polyether Polymers 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical group [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- 229910002808 Si–O–Si Inorganic materials 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 125000003342 alkenyl group Chemical group 0.000 description 1
- 125000003545 alkoxy group Chemical group 0.000 description 1
- 125000001118 alkylidene group Chemical group 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 125000000962 organic group Chemical group 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 229920000548 poly(silane) polymer Polymers 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
Landscapes
- Silicon Polymers (AREA)
Abstract
The invention relates to a preparation method of a modified silicone oil, i.e., a vinyl silicone oil containing an alkylene structure; and specifically, the invention relates to preparation steps and a preparation method of the vinyl silicone oil containing the alkylene structure. The method comprises the following steps: preparing carbon-carbon bond and silicon-oxygen bond into cyclic prepolymer polysiloxane A1 and A2 through silicon-hydrogen addition reaction; then concurrently balancing with polydimethylsiloxane cyclic mixture, hexamethyldisiloxane, divinyl-tetramethyl-disiloxane, tetramethyl tetravinyl cyclotetrasiloxane, or the like; and then neutralizing, filtering, and extracting low-boiling-point substances, thereby obtaining a colorless transparent liquid. The vinyl silicone oil is especially applicable to the requirements of low moisture permeation and low oxygen permeation in the LED packaging industry, and is of a certain acceleration effect to splicing packaging brackets.
Description
Technical field
The present invention relates to a kind of modified silicon oil namely containing the preparation method of the vinyl silicone oil of alkylen structures, specifically, the present invention relates to the preparation process containing the vinyl silicone oil of alkylen structures and method.
Background technology
Silicone oil is kind important in silicoorganic compound, and keep the linear polysilane product of liquid state under typically referring to room temperature, structural formula is as follows:
in formula, R is alkyl, aryl; R ' is alkyl, aryl, hydrogen carbon functional group and polyether chain etc.; X is alkyl, aryl, alkenyl, hydrogen, hydroxyl, alkoxyl group, acetoxyl group, chlorine, carbon functional group and polyether chain etc.; N, m=0,1,2,3
Because silicon and carbon belong to periodic table of elements IVA race element together, therefore there is some similar chemical property.As silicon and carbon all have 4 not paired S electronics and P electronics, the element (as Fe, O, Cl etc.) that they can be higher with electronegativity and the lower group (as H-, CH3-, C6H5-etc.) of electronegativity combine, and reach covalency saturated.Siliciumatom can form covalent linkage with carbon atom, also can combine with organic group, generates many silicoorganic compound.But the cycle residing for both does not stop, thus there is many difference.As carbon and oxygen preferentially generate double bond, and silicon mainly forms singly-bound.When forming polymkeric substance, carbon take C-C-C as main chain.Silicon is then main take Si-O-Si as main chain.This chain is the basic chains forming polysiloxane.
Silicone oil is a veriety, and series is more, the organosilicon product that range of application is wider.There is excellent release, breathable moisture permeability.But for LED encapsulation material, then need to increase the cementability with base material, reduce its breathable moisture permeability.The siloxane main chain joint of silicone oil imbeds the alkylen structures of carbon carbochain, other excellent performance of silicone oil can be kept, also can improve cementability and breathable moisture permeability very well simultaneously.
In LED industry, the impact of packaged material on LED is most important.LED encapsulation material is progressively transformed into organosilicon material by original epoxy-like materials.In order to reach the requirements such as the resistance to ultraviolet of packaged material, heat-proof aging and low-stress, according to different purposes, packaged material is roughly divided into low folding silica gel with the large class of high folding silica gel two.Low folding silica gel has good transparency and mechanical property, and color inhibition has superiority than high folding packaging plastic, but also there is certain defect, due to its structure problem, makes breathable moisture permeability poorer than high folding packaging plastic.The present invention is directed to this problem, linear ethylene base silicone oil structure is adjusted, introduce alkylen structures, to improve its resistance to breathable moisture permeability.
Summary of the invention
For existing low folding silica gel with the difference between high folding silica gel, first object of the present invention discloses a kind of novel modified vinyl silicone oil, is the vinyl silicone oil containing alkylidene group.The present invention's second object refers to that in the silica link of conventional organosilicon silicone oil, add carbon-carbon bond makes a kind of synthetic method containing alkylidene group modified silicon oil.Gained silicone oil can meet the breathable moisture permeability of low folding silica gel, and also can meet the stress influence problem of high folding silica gel, be the reasonable Material selec-tion of LED glue industry.
In order to realize first above-mentioned object, present invention employs following technical scheme:
A kind of containing alkylen structures vinyl silicone oil, it is characterized in that, described silicone oil structure is one or both the mixing in following structural formula:
(5)
(6)
Above-mentioned n1, n2, n3 be respectively be more than or equal to 0 positive integer and can not be all 0, above-mentioned m1, m2 be respectively be more than or equal to 0 positive integer and can not to be all 0, q be more than or equal to 1 positive integer.
As preferably, described n1, n2, n3 are the positive integer of 1 ~ 100, and m1, m2 are respectively the positive integer of 1 ~ 100, and q is the positive integer of 1 ~ 100.
As preferably, described n1, n2, n3 are the positive integer of 2 ~ 50, and m1, m2 are respectively the positive integer of 2 ~ 50, and q is the positive integer of 2 ~ 50.
In order to realize second above-mentioned object, present invention employs following technical scheme:
Prepare the above-mentioned preparation method containing alkylen structures vinyl silicone oil, the method comprises the following steps:
1) preparation of polysiloxane A:
By hydrogen siloxane and the silane or the siloxanes that contain thiazolinyl, under platinum catalyst effect, addition reaction obtains following structural product:
a1
A2；
Above-mentioned n be more than or equal to 1 positive integer;
2) by above-mentioned steps 1) product, then with octamethylcyclotetrasiloxane and 1,1,3,3-tetramethyl--1,3-divinyl disiloxane, under acid catalysis, equilibrium polymerization; Removing low-volatile component, obtains the product of following structural formula (1) and (2):
（1）
（2）；
3) by the product of structure above (1) and/or (2), with octamethylcyclotetrasiloxane, t etram-ethyltetravinylcyclotetrasiloxane, hexamethyldisiloxane, under acid catalysis, equilibrium polymerization; Must containing the vinyl silicone oil of alkylen structures, removing low-volatile component, obtains the vinyl silicone oil product containing alkylen structures shown in structural formula (5) and/or (6).
As preferably, the raw material of described structured product A1, A2 is 1,1,3,3-tetramethyl--1,3-dihydro base sily oxide, divinyl silane, 1,1,3,3-tetramethyl--1,3-divinyl disiloxane, under platinum catalyst effect, carries out addition reaction and obtains.
As preferably, the catalyzer that described structured product A1, A2 synthesis adopts is platinum catalyst, and as preferably, platinum catalyst selects platinum-vinyl siloxane title complex or platinum-ol solution.
As preferably, the described temperature of reaction that described structured product A1, A2 synthesis adopts: 40 ~ 120 DEG C, described reaction times: 5 ~ 24 hours.
As preferably, described structured product A1, A2 building-up reactions terminates, removing catalyzer, the method for removing platinum catalyst, selects metal absorbent or absorption carbon black.
As preferably, described structural formula (3) and/or (4) are synthesized described acid catalyst and are selected trifluoromethayl sulfonic acid, the vitriol oil or hydrochloric acid; Described temperature of reaction 30 ~ 100 DEG C; 4 ~ 48 hours described reaction times; Reaction terminates, removing catalyzer.
As preferably, described except catalyst method, select neutralization to filter, sodium carbonate selected by neutralizing agent, sodium bicarbonate or hexamethyldisilazane.
Present method is, by addition reaction of silicon with hydrogen, carbon-carbon bond and siloxane bond are made ring prepolymer polysiloxane A1, A2, again under certain condition, with polydimethylsiloxane mixed methylcyclosiloxane, hexamethyldisiloxane, divinyl tetramethyl disiloxane, the common equilibrium such as t etram-ethyltetravinylcyclotetrasiloxane, again through neutralization, filter, extract low-boiling-point substance, obtain colourless transparent liquid.Product of the present invention is specially adapted to LED embedding industry, for the requirement of low moisture-inhibiting oxygen flow, and is bonded with certain promoter action to embedding support.
Embodiment
Below the fact of the present invention is illustrated, but embodiment is not limiting the scope of the invention.
Embodiment 1:
Divinyl silane 112g is added in the there-necked flask of 500ml drying, start heating, under 40 degree, add catalyzer 1.5ppm, drip tetramethyl-dihydro base sily oxide 134g after stirring 5min, drip 1 hour, control temperature of reaction at 40 ~ 60 degree, after being added dropwise to complete, 40 ~ 60 degree of insulations were down to room temperature after 7 hours, added metal absorbent, stirring at room temperature 5 hours, leaches stand-by by product A.Product A 135g, octamethylcyclotetrasiloxane 130g, tetramethyl divinyl disiloxane 0.41g, trifluoromethayl sulfonic acid 0.11g equilibrium polymerization 12 hours is added in the there-necked flask of 500ml drying.After balance, to add in hexamethyldisilazane 40g and after, suction filtration, removes low component and obtains colourless transparent liquid, be product.Record viscosity 8220mpas, vinyl mass percentage 0.09%, fugitive constituent (150 DEG C/2hr) 0.33%.
Embodiment 2:
Divinyl silane 112g is added in the there-necked flask of 500ml drying, start heating, under 45 degree, add catalyzer 1.5ppm, drip tetramethyl-dihydro base sily oxide 134g after stirring 5min, drip 1 hour, control temperature of reaction at 40 ~ 60 degree, after being added dropwise to complete, 40 ~ 60 degree of insulations were down to room temperature after 9 hours, added metal absorbent, stirring at room temperature 5 hours, leaches stand-by by product A.Product A 134g, octamethylcyclotetrasiloxane 121g, tetramethyl divinyl disiloxane 0.34g, trifluoromethayl sulfonic acid 0.1g equilibrium polymerization 12 hours is added in the there-necked flask of 500ml drying.After balance, to add in hexamethyldisilazane 40g and after, suction filtration, removes low component and obtains colourless transparent liquid, be product.Record viscosity 4160mpas, vinyl mass percentage 0.15%, fugitive constituent (150 DEG C/2hr) 0.61%.
Embodiment 3:
Tetramethyl divinyl disiloxane 186g is added in the there-necked flask of 500ml drying, start heating, under 40 degree, add catalyzer 1.5ppm, drip tetramethyl-dihydro base sily oxide 134g after stirring 5min, drip 1 hour, control temperature of reaction at 40 ~ 60 degree, after being added dropwise to complete, 40 ~ 60 degree of insulations were down to room temperature after 7 hours, added metal absorbent, stirring at room temperature 5 hours, leaches stand-by by product A.Product A 113g, octamethylcyclotetrasiloxane 87g, tetramethyl divinyl disiloxane 0.24g, vitriol oil 3.2g equilibrium polymerization 12 hours is added in the there-necked flask of 500ml drying.After balance, to add in sodium bicarbonate 4.8g and after, suction filtration, removes low component and obtains colourless transparent liquid, be product.Record viscosity 3533mpas, vinyl mass percentage 0.17%, fugitive constituent (150 DEG C/2hr) 0.25%.
Embodiment 4:
Tetramethyl divinyl disiloxane 186g is added in the there-necked flask of 500ml drying, start heating, under 40 degree, add catalyzer 1.5ppm, drip tetramethyl-dihydro base sily oxide 134g after stirring 5min, drip 1 hour, control temperature of reaction at 40 ~ 60 degree, after being added dropwise to complete, 40 ~ 60 degree of insulations were down to room temperature after 7 hours, added metal absorbent, stirring at room temperature 5 hours, leaches stand-by by product A.Product A 113g, octamethylcyclotetrasiloxane 87g, tetramethyl divinyl disiloxane 1.03g, t etram-ethyltetravinylcyclotetrasiloxane 3.23g, vitriol oil 3.3g equilibrium polymerization 8 hours is added in the there-necked flask of 500ml drying.After balance, to add in sodium bicarbonate 4.9g and after, suction filtration, removes low component and obtains colourless transparent liquid, be product.Record viscosity 5190mpas, vinyl mass percentage 0.64%, fugitive constituent (150 DEG C/2hr) 0.38%.
Embodiment 5:
Divinyl silane 112g is added in the there-necked flask of 500ml drying, start heating, under 40 degree, add catalyzer 1.5ppm, drip tetramethyl-dihydro base sily oxide 134g after stirring 5min, drip 1 hour, control temperature of reaction at 40 ~ 60 degree, after being added dropwise to complete, 40 ~ 60 degree of insulations were down to room temperature after 7 hours, added absorption carbon black, stirring at room temperature 5 hours, leaches stand-by by product A.Product A 150g, octamethylcyclotetrasiloxane 120g, t etram-ethyltetravinylcyclotetrasiloxane 3.08g, hexamethyldisiloxane 1.5g, vitriol oil 4.4g equilibrium polymerization 8 hours is added in the there-necked flask of 500ml drying.After balance, to add in sodium bicarbonate 6.6g and after, suction filtration, removes low component and obtains colourless transparent liquid, be product.Record viscosity 6050mpas, vinyl mass percentage 0.35%, fugitive constituent (150 DEG C/2hr) 0.42%.
Claims (10)
1. a vinyl silicone oil, is characterized in that, described silicone oil structure is one or both the mixing in following structural formula:
(5)
(6)
Above-mentioned n1, n2, n3 be respectively be more than or equal to 0 positive integer and can not be all 0, above-mentioned m1, m2 be respectively be more than or equal to 0 positive integer and can not to be all 0, q be more than or equal to 1 positive integer.
2. a kind of vinyl silicone oil according to claim 1, is characterized in that, n1, n2, n3 are the positive integer of 1 ~ 100, and m1, m2 are respectively the positive integer of 1 ~ 100, and q is the positive integer of 1 ~ 100.
3. a kind of vinyl silicone oil according to claim 1, is characterized in that, n1, n2, n3 are the positive integer of 2 ~ 50, and m1, m2 are respectively the positive integer of 2 ~ 50, and q is the positive integer of 2 ~ 50.
4. prepare a preparation method for a kind of vinyl silicone oil described in claim 1 ~ 3 any one claim, it is characterized in that the method comprises the following steps:
1) preparation of polysiloxane A:
By hydrogen siloxane and the silane or the siloxanes that contain thiazolinyl, under platinum catalyst effect, addition reaction obtains following structural product:
a1
A2；
Above-mentioned n be more than or equal to 1 positive integer;
2) by above-mentioned steps 1) product, then with octamethylcyclotetrasiloxane and 1,1,3,3-tetramethyl--1,3-divinyl disiloxane, under acid catalysis, equilibrium polymerization; Removing low-volatile component, obtains the product of following structural formula (1) and (2):
（1）
（2）；
3) by the product of structure above (1) and/or (2), with octamethylcyclotetrasiloxane, t etram-ethyltetravinylcyclotetrasiloxane, hexamethyldisiloxane, under acid catalysis, equilibrium polymerization; Must containing the vinyl silicone oil of alkylen structures, removing low-volatile component, obtains the vinyl silicone oil product containing alkylen structures shown in structural formula (5) and/or (6).
5. preparation method according to claim 4, is characterized in that, the raw material of structured product A1, A2 is 1,1,3,3-tetramethyl--1,3-dihydro base sily oxide, divinyl silane, 1,1,3,3-tetramethyl--1,3-divinyl disiloxane, under platinum catalyst effect, carry out addition reaction and obtain.
6. preparation method according to claim 5, is characterized in that, the catalyzer that structured product A1, A2 synthesis adopts is platinum catalyst, and as preferably, platinum catalyst selects platinum-vinyl siloxane title complex or platinum-ol solution.
7. preparation method according to claim 5, is characterized in that, the described temperature of reaction that structured product A1, A2 synthesis adopts: 40 ~ 120 DEG C, the described reaction times: 5 ~ 24 hours.
8. preparation method according to claim 5, is characterized in that, structured product A1, A2 building-up reactions terminates, removing catalyzer, the method for removing platinum catalyst, selects metal absorbent or absorption carbon black.
9. preparation method according to claim 5, is characterized in that, structural formula (5) and/or (6) are synthesized described acid catalyst and selected trifluoromethayl sulfonic acid, the vitriol oil or hydrochloric acid; Described temperature of reaction 30 ~ 100 DEG C; 4 ~ 48 hours described reaction times; Reaction terminates, removing catalyzer.
10. preparation method according to claim 9, is characterized in that, except catalyst method, select neutralization to filter, sodium carbonate selected by neutralizing agent, sodium bicarbonate or hexamethyldisilazane.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108102100A (en) * | 2017-12-27 | 2018-06-01 | 浙江福斯特新材料研究院有限公司 | A kind of production method and production system of low volatilization vinyl silicone oil |
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| US6080829A (en) * | 1998-06-24 | 2000-06-27 | Medtronic, Inc. | Silalkylenesiloxane copolymer materials and methods for their preparation |
| CN101955587A (en) * | 2009-07-17 | 2011-01-26 | 信越化学工业株式会社 | Organohydrogenpolysiloxane, making method, and addition-cure silicone composition |
| CN102596970A (en) * | 2009-11-03 | 2012-07-18 | 道康宁公司 | Process for the production of polysilalkylenesiloxanes |
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2015
- 2015-04-24 CN CN201510199209.XA patent/CN104817699A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5442083A (en) * | 1993-09-03 | 1995-08-15 | Dow Corning Toray Silicone Company, Ltd. | Method for the preparation of organosilicon polymer |
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| CN101955587A (en) * | 2009-07-17 | 2011-01-26 | 信越化学工业株式会社 | Organohydrogenpolysiloxane, making method, and addition-cure silicone composition |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108102100A (en) * | 2017-12-27 | 2018-06-01 | 浙江福斯特新材料研究院有限公司 | A kind of production method and production system of low volatilization vinyl silicone oil |
| CN108102100B (en) * | 2017-12-27 | 2020-11-10 | 浙江福斯特新材料研究院有限公司 | A kind of production method and production system of low-volatile vinyl silicone oil |
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