CN106810700A - One kind contains phenyl end capped methyl ethylene（Tetraphenyl）Phenyl modified silica gel and preparation method thereof - Google Patents

One kind contains phenyl end capped methyl ethylene（Tetraphenyl）Phenyl modified silica gel and preparation method thereof Download PDF

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Publication number
CN106810700A
CN106810700A CN201611224963.5A CN201611224963A CN106810700A CN 106810700 A CN106810700 A CN 106810700A CN 201611224963 A CN201611224963 A CN 201611224963A CN 106810700 A CN106810700 A CN 106810700A
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phenyl
tetraphenyl
end capped
silica gel
capped methyl
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葛铁军
张煜欣
肖尚雄
张瑾
赵越
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Shenyang University of Chemical Technology
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    • 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
    • C08G77/04—Polysiloxanes
    • C08G77/38—Polysiloxanes modified by chemical after-treatment
    • C08G77/382—Polysiloxanes modified by chemical after-treatment containing atoms other than carbon, hydrogen, oxygen or silicon
    • C08G77/385—Polysiloxanes modified by chemical after-treatment containing atoms other than carbon, hydrogen, oxygen or silicon containing halogens
    • 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
    • C08G77/04—Polysiloxanes
    • C08G77/38—Polysiloxanes modified by chemical after-treatment

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  • Chemical & Material Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Developing Agents For Electrophotography (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

One kind contains phenyl end capped methyl ethylene（Tetraphenyl）Phenyl modified silica gel and preparation method thereof, is related to a kind of modified silica-gel and preparation method thereof, the phenyl end capped, methyl, vinyl,（Tetraphenyl）Phenyl block copolymer, by introducing phenyl end capped methyl ethylene（Tetraphenyl）While phenyl makes silica gel keep excellent electrical insulating property, heat resistance, phenyl end capped methyl ethylene is contained by introducing（Tetraphenyl）Phenyl not only makes the modified silica-gel have excellent gloss retention, electrical insulating property, heat resistance, also has the advantages that high surface hardness, bending resistance, and curing rate is fast, resistance to tear-resistant, not efflorescence.The block copolymer structure is controllable, is greatly expanded containing phenyl end capped methyl ethylene（Tetraphenyl）The performance and range of application of phenyl modified silica gel.

Description

One kind contains phenyl end capped methyl ethylene（Tetraphenyl）Phenyl modified silica gel and its preparation Method
Technical field
It is more particularly to a kind of to contain phenyl end capped methyl ethylene the present invention relates to a kind of modified silica-gel and preparation method thereof （Tetraphenyl）Phenyl modified silica gel and preparation method thereof.
Background technology
Silicon rubber refers to that molecular backbone is-Si-O- inorganic structures, and side chain is a class elastomer of organic group.Silicon rubber Glue belongs to half inorganic saturation, heterochain, non-polar elastomer.Silicon rubber has excellent heat resistance, cold resistance, dielectricity, resistance to The performance such as ozone and resistance to atmospheric aging, the performance that silicon rubber is protruded is broad temperature in use, can be -60 DEG C (or lower temperatures) Long-term use to+250 DEG C (or temperature higher).
High temperature resistant silica gel is a kind of common performance silica gel product of silica gel product, and common silica gel high temperature resistant degree is 200~300 Between degree Celsius, but under given conditions, there is requirement very high to the resistance to elevated temperatures of silica gel.In the prior art, produce Common high temperature resistant silicon colloidality can meet requirement.
The application for a patent for invention of Publication No. 103642240A, discloses a kind of conductive silicon rubber.Including following component：Silicon Rubber, white carbon, calcium carbonate, acetylene carbon black, structure inhibitor, liquid silastic, vulcanizing agent, alundum (Al2O3), containing vinyl Silane coupler, methyl-silicone oil, zinc stearate.Silicon rubber of the present invention has the excellent of high thermal conductivity, heat resistance and low compressibility Point, its thermal conductivity factor is more than 3, because it has good thermal conductivity, therefore can bear bigger conductive current.
A kind of application for a patent for invention of Publication No. 102532914A, composition of raw materials of high-temperature-resisting silicon rubber, is related to organic Polymeric silicon Material Field, the quality parts ratio of each raw material is in formula：185 parts of methyl vinyl silicone rubber, gas-phase silica 50 parts, 6 parts, No. 67 parts of oil of hydroxy silicon oil, 5 parts of phenyl silicone oil, 0.6 part of containing hydrogen silicone oil, 0.5 part of releasing agent, the heat-resisting addition of nanometer Agent is the 1~1.5% of gross mass.High-temperature-resisting silicon rubber obtained by the present invention, adds a nanometer heat-resisting additive, can be resistance to Less than 400 degree of high temperature, can meet the high temperature resistant requirement to silicon rubber under specific condition.
The content of the invention
Contain phenyl end capped methyl ethylene it is an object of the invention to provide one kind（Tetraphenyl）Phenyl modified silica gel and its Preparation method, the present invention is by introducing phenyl end capped methyl ethylene（Tetraphenyl）Phenyl makes silica gel keep excellent electric insulation Property, heat resistance while, by introduce contain phenyl end capped methyl ethylene（Tetraphenyl）It is excellent that phenyl not only has modified silica-gel Good gloss retention, electrical insulating property, heat resistance, also has the advantages that high surface hardness, bending resistance, and curing rate is fast, resistance to Tear-resistant, not efflorescence.
The purpose of the present invention is achieved through the following technical solutions：
One kind contains phenyl end capped methyl ethylene（Tetraphenyl）Phenyl modified silica gel, the silica gel structure is as follows：
。
Described phenyl end capped methyl ethylene（Tetraphenyl）Phenyl modified silica gel, the phenyl end capped methyl ethylene silicon Oil is 1 with the mass ratio of tetraphenylcyclopentadienone:0.4~2.
One kind contains phenyl end capped methyl ethylene（Tetraphenyl）Phenyl modified silica gel preparation method, methods described includes as follows Step：
（1）Agitator, condenser pipe, thermometer are installed in 500ml three neck round bottom flask.And connect vacuum filtration machine；By three Mouth flask is placed in oil bath pan；230g octamethylcy-clotetrasiloxanes and 60g tetramethyl tetravinyls are added in there-necked flask Cyclotetrasiloxane, is warming up to 90 degree, and under N2 protections, magnetic agitation is evacuated to -0.08MPa, is dehydrated one hour；Add the benzene of 8g tetra- Base divinyl disiloxane and 6g TMAHs, are warming up to 110 DEG C, react three hours；System is warming up to again 160 DEG C, 1h is reacted, decompose catalyst, remove low-boiling-point substance under reduced pressure, obtain the i.e. phenyl end capped methyl ethylene silicon of product liquid Oil；
（2）Agitator, reflux condensing tube device and thermometer are connected in three neck round bottom flask, and install oil bath pan；To three Phenyl end capped methyl vinyl silicon oil, tetraphenylcyclopentadienone, α-chloronaphthalene are added in mouth round-bottomed flask；Oil bath pot temperature is set It is set to 220 DEG C.Heating stirring backflow a few hours in N2 atmosphere；The widely different purple for flowing to tetraphenylcyclopentadienone of heating is decorporated, cold But, after layering, upper strata is product；
。
The phenyl end capped methyl ethylene（Tetraphenyl）Phenyl modified silica gel preparation method, in step (1), prestox Cyclotetrasiloxane is 4 with the mass ratio of t etram-ethyltetravinylcyclotetrasiloxane:1~19:1.
The phenyl end capped methyl ethylene（Tetraphenyl）Phenyl modified silica gel preparation method, it is described in step (1) Acidic catalyst is the concentrated sulfuric acid of mass fraction 98%, and consumption is the 0.0005%~0.5% of reactant gross mass.
Described phenyl end capped methyl ethylene（Tetraphenyl）Phenyl modified silica gel preparation method, in step (1), four benzene Base divinyl disiloxane is 1 with the mass ratio of TMAH:1.5~1:3.
Described phenyl end capped methyl ethylene（Tetraphenyl）Phenyl modified silica gel preparation method, it is described in step (2) Phenyl end capped methyl vinyl silicon oil:Tetraphenylcyclopentadienone:The mol ratio of α-chloronaphthalene is 2.1:1:1.
Advantages of the present invention is with effect：
The present invention provides a kind of containing phenyl end capped methyl ethylene（Tetraphenyl）Prepared by phenyl modified silica gel, the phenyl end capped, first Base, vinyl,（Tetraphenyl）Phenyl block copolymer, by introducing phenyl end capped methyl ethylene（Tetraphenyl）Phenyl makes silica gel While keeping excellent electrical insulating property, heat resistance, phenyl end capped methyl ethylene is contained by introducing（Tetraphenyl）Phenyl is not only Make modified silica-gel that there is excellent gloss retention, electrical insulating property, heat resistance, also there is high surface hardness, bending resistance, and And curing rate is fast, resistance to tear-resistant, not efflorescence.The block copolymer structure is controllable, is greatly expanded containing phenyl end capped methyl Vinyl（Tetraphenyl）The performance and range of application of phenyl modified silica gel.
The present invention provides a kind of with heat-resisting phenyl end capped methyl ethylene（Tetraphenyl）It is prepared by phenyl modified silica gel.Solution The low shortcoming of traditional silastic material heat resistance of having determined.New synthesis（Tetraphenyl）Phenyl vinyl silastic material due to（Four Phenyl）The characteristics of phenyl vinyl has steric effect, homeostasis, overcomes general silicon rubber and is held labile lacking by high temperature Point.Synthesis（Tetraphenyl）Phenyl vinyl silastic material is a chemical addition reaction, and Diels-Alder is anti-for reaction mechanism thing Should.Single step reaction is convenient and swift, and low cost, accessory substance is few.This synthesis technique is reasonable, it is easy to industrialized production.
Specific embodiment
With reference to embodiment, the present invention is described in detail.
The synthesis of phenyl end capped methyl vinyl silicon oil
The first step：Agitator, condenser pipe, thermometer are installed in 500ml three neck round bottom flask.And connect vacuum filtration machine. There-necked flask is placed in oil bath pan.
Second step：230g octamethylcy-clotetrasiloxanes and the silicon of 60g tetramethyl tetravinyls ring four are added in there-necked flask Oxygen alkane, is warming up to 90 degree, N2Under protection, magnetic agitation is evacuated to -0.08MPa, is dehydrated one hour.
3rd step：8g tetraphenyls divinyl disiloxane and 6g TMAHs are added, 110 DEG C is warming up to, instead Answer three hours.
4th step：System is warming up to 160 DEG C again, 1h is reacted, catalyst is decomposed, low-boiling-point substance is removed under reduced pressure, liquid is obtained Body product is phenyl end capped methyl vinyl silicon oil.
The synthesis of tetraphenyl phenyl vinyl silicone oil
The first step：Agitator, reflux condensing tube device and thermometer are connected in three neck round bottom flask, and install oil bath pan.
Second step：To addition multi-vinyl silicone oil, tetraphenylcyclopentadienone, α-chloronaphthalene in three neck round bottom flask.By oil Bath temperature is set as 220 DEG C.
3rd step：N2Heating stirring backflow a few hours in atmosphere.
4th step：The widely different purple for flowing to tetraphenylcyclopentadienone of heating is decorporated, and is cooled down, and after layering, upper strata is product, under Layer is solvent.
Embodiment 1
（1）Agitator, condenser pipe, thermometer are installed in 500ml three neck round bottom flask.And connect vacuum filtration machine.By three Mouth flask is placed in oil bath pan.230g octamethylcy-clotetrasiloxanes and 60g tetramethyl tetravinyls are added in there-necked flask Cyclotetrasiloxane, is warming up to 90 degree, N2Under protection, magnetic agitation is evacuated to -0.08MPa, is dehydrated one hour.Add the benzene of 8g tetra- Base divinyl disiloxane and 6g TMAHs, are warming up to 110 DEG C, react three hours.System is warming up to again 160 DEG C, 1h is reacted, decompose catalyst, remove low-boiling-point substance under reduced pressure, obtain product liquid i.e. multi-vinyl silicone oil.Mixing, stirring It is uniform stand-by.
（2）By multi-vinyl silicone oil, tetraphenylcyclopentadienone, in mass ratio 5.03：1 adds the reactor containing 70ml In, in 200 DEG C of temperature in N2Heating stirring flows back 7.5 hours in atmosphere, that is, obtain（Tetraphenyl）Phenyl vinyl silicon rubber is helped Agent.Take（Tetraphenyl）2 parts of phenyl vinyl silicon rubber auxiliary agent, 100 parts of 107 silicon rubber, 20 parts of modified white carbon black, TiO25 parts, 4 parts of containing hydrogen silicone oil, 0.4 part of dibutyl tin dilaurate, mix, stir it is stand-by.
（3）The silicon rubber that will be prepared, is bonded between cementing print selection stainless steel.Adhesive surface is entered before bonding Row pretreatment, with surface degreasing machinery blast.Experiment uses the simple degreasing in metal surface, with emery cloth burnished metal surface Afterwards, with solvent degreasing once.Adhering method is docked using single spreading, and bonding batten meets GB GB7124.86 standards.System 6 parts, active phase test, mechanical property test, hot air aging, viscosity test are carried out respectively.
Embodiment 2
（1）Agitator, condenser pipe, thermometer are installed in 500ml three neck round bottom flask.And connect vacuum filtration machine.By three Mouth flask is placed in oil bath pan.230g octamethylcy-clotetrasiloxanes and 60g tetramethyl tetravinyls are added in there-necked flask Cyclotetrasiloxane, is warming up to 90 degree, N2Under protection, magnetic agitation is evacuated to -0.08MPa, is dehydrated one hour.Add the benzene of 8g tetra- Base divinyl disiloxane and 6g TMAHs, are warming up to 110 DEG C, react three hours.System is warming up to again 160 DEG C, 1h is reacted, decompose catalyst, remove low-boiling-point substance under reduced pressure, obtain product liquid i.e. multi-vinyl silicone oil.Mixing, stirring It is uniform stand-by.
（2）By multi-vinyl silicone oil, tetraphenylcyclopentadienone, in mass ratio 3.34：1 adds the reactor containing 70ml In, in 200 DEG C of temperature in N2Heating stirring flows back 7.5 hours in atmosphere, that is, obtain（Tetraphenyl）Phenyl vinyl silicon rubber is helped Agent.Take（Tetraphenyl）4 parts of phenyl vinyl silicon rubber auxiliary agent, 100 parts of 107 silicon rubber, 20 parts of modified white carbon black, TiO25 parts, 4 parts of containing hydrogen silicone oil, 0.4 part of dibutyl tin dilaurate, mix, stir it is stand-by..
（3）With the step of embodiment 1 the 3rd.
Embodiment 3
（1）Agitator, condenser pipe, thermometer are installed in 500ml three neck round bottom flask.And connect vacuum filtration machine.By three Mouth flask is placed in oil bath pan.230g octamethylcy-clotetrasiloxanes and 60g tetramethyl tetravinyls are added in there-necked flask Cyclotetrasiloxane, is warming up to 90 degree, N2Under protection, magnetic agitation is evacuated to -0.08MPa, is dehydrated one hour.Add the benzene of 8g tetra- Base divinyl disiloxane and 6g TMAHs, are warming up to 110 DEG C, react three hours.System is warming up to again 160 DEG C, 1h is reacted, decompose catalyst, remove low-boiling-point substance under reduced pressure, obtain product liquid i.e. multi-vinyl silicone oil.Mixing, stirring It is uniform stand-by.
（2）By multi-vinyl silicone oil, tetraphenylcyclopentadienone, in mass ratio 2.35：1 adds the reactor containing 70ml In, in 200 DEG C of temperature in N2Heating stirring flows back 7.5 hours in atmosphere, that is, obtain（Tetraphenyl）Phenyl vinyl silicon rubber is helped Agent.Take（Tetraphenyl）6 parts of phenyl vinyl silicon rubber auxiliary agent, 100 parts of 107 silicon rubber, 20 parts of modified white carbon black, TiO25 parts, 4 parts of containing hydrogen silicone oil, 0.4 part of dibutyl tin dilaurate, mix, stir it is stand-by.
（3）With the step of embodiment 1 the 3rd.
Embodiment 4
（1）Agitator, condenser pipe, thermometer are installed in 500ml three neck round bottom flask.And connect vacuum filtration machine.By three Mouth flask is placed in oil bath pan.230g octamethylcy-clotetrasiloxanes and 60g tetramethyl tetravinyls are added in there-necked flask Cyclotetrasiloxane, is warming up to 90 degree, N2Under protection, magnetic agitation is evacuated to -0.08MPa, is dehydrated one hour.Add the benzene of 8g tetra- Base divinyl disiloxane and 6g TMAHs, are warming up to 110 DEG C, react three hours.System is warming up to again 160 DEG C, 1h is reacted, decompose catalyst, remove low-boiling-point substance under reduced pressure, obtain product liquid i.e. multi-vinyl silicone oil.Mixing, stirring It is uniform stand-by.
（2）By multi-vinyl silicone oil, tetraphenylcyclopentadienone, in mass ratio 5.03：1 adds the reactor containing 70ml In, in 200 DEG C of temperature in N2Heating stirring flows back 7.5 hours in atmosphere, that is, obtain（Tetraphenyl）Phenyl vinyl silicon rubber is helped Agent.Take（Tetraphenyl）6 parts of phenyl vinyl silicon rubber auxiliary agent, 100 parts of 107 silicon rubber, 20 parts of modified white carbon black, TiO25 parts, 4 parts of containing hydrogen silicone oil, 0.4 part of dibutyl tin dilaurate, mix, stir it is stand-by..
（3）With the step of embodiment 1 the 3rd.
Embodiment 5
（1）Agitator, condenser pipe, thermometer are installed in 500ml three neck round bottom flask.And connect vacuum filtration machine.By three Mouth flask is placed in oil bath pan.230g octamethylcy-clotetrasiloxanes and 60g tetramethyl tetravinyls are added in there-necked flask Cyclotetrasiloxane, is warming up to 90 degree, N2Under protection, magnetic agitation is evacuated to -0.08MPa, is dehydrated one hour.Add the benzene of 8g tetra- Base divinyl disiloxane and 6g TMAHs, are warming up to 110 DEG C, react three hours.System is warming up to again 160 DEG C, 1h is reacted, decompose catalyst, remove low-boiling-point substance under reduced pressure, obtain product liquid i.e. multi-vinyl silicone oil.Mixing, stirring It is uniform stand-by.
（2）By multi-vinyl silicone oil, tetraphenylcyclopentadienone, in mass ratio 5.03：1 adds the reactor containing 70ml In, in 200 DEG C of temperature in N2Heating stirring flows back 7.5 hours in atmosphere, that is, obtain（Tetraphenyl）Phenyl vinyl silicon rubber is helped Agent.Take（Tetraphenyl）12 parts of phenyl vinyl silicon rubber auxiliary agent, 100 parts of 107 silicon rubber, 20 parts of modified white carbon black, TiO25 parts, 4 parts of containing hydrogen silicone oil, 0.4 part of dibutyl tin dilaurate, mix, stir it is stand-by..
（3）With the step of embodiment 1 the 3rd.
Embodiment 6
（1）Agitator, condenser pipe, thermometer are installed in 500ml three neck round bottom flask.And connect vacuum filtration machine.By three Mouth flask is placed in oil bath pan.230g octamethylcy-clotetrasiloxanes and 60g tetramethyl tetravinyls are added in there-necked flask Cyclotetrasiloxane, is warming up to 90 degree, N2Under protection, magnetic agitation is evacuated to -0.08MPa, is dehydrated one hour.Add the benzene of 8g tetra- Base divinyl disiloxane and 6g TMAHs, are warming up to 110 DEG C, react three hours.System is warming up to again 160 DEG C, 1h is reacted, decompose catalyst, remove low-boiling-point substance under reduced pressure, obtain product liquid i.e. multi-vinyl silicone oil.Mixing, stirring It is uniform stand-by.
（2）By multi-vinyl silicone oil, tetraphenylcyclopentadienone, in mass ratio 5.03：1 adds the reactor containing 70ml In, in 200 DEG C of temperature in N2Heating stirring flows back 7.5 hours in atmosphere, that is, obtain（Tetraphenyl）Phenyl vinyl silicon rubber is helped Agent.Take（Tetraphenyl）24 parts of phenyl vinyl silicon rubber auxiliary agent, 100 parts of 107 silicon rubber, 20 parts of modified white carbon black, TiO25 parts, 4 parts of containing hydrogen silicone oil, 0.4 part of dibutyl tin dilaurate, mix, stir it is stand-by..
（3）With the step of embodiment 1 the 3rd.
Comparative example
Prepared by the embodiment of the present invention 1 to 6（Tetraphenyl）Phenyl vinyl silicon rubber is as follows with the performance comparison of silicon rubber Table：
Table 1
As seen from the above table, it is of the invention（Tetraphenyl）The heat resistance of phenyl vinyl silicon rubber is greatly improved, product Combination property is improved.This be due to（Tetraphenyl）Phenyl vinyl imparts its stability, space steric effect（Tetraphenyl） Phenyl vinyl silicon rubber, and cause the lifting of its heat resistance.Middle change is auxiliary agent in embodiment 1 to 6（Tetraphenyl）Benzene The mass ratio of base vinyl, from result, mass ratio 5.03：Effect is best when 1.

Claims (7)

1. it is a kind of to contain phenyl end capped methyl ethylene（Tetraphenyl）Phenyl modified silica gel, it is characterised in that the silica gel structure is such as Under：
。
2. phenyl end capped methyl ethylene according to claim 1（Tetraphenyl）Phenyl modified silica gel, it is characterised in that institute It is 1 that phenyl end capped methyl vinyl silicon oil is stated with the mass ratio of tetraphenylcyclopentadienone:0.4~2.
3. it is a kind of to contain phenyl end capped methyl ethylene（Tetraphenyl）Phenyl modified silica gel preparation method, it is characterised in that the side Method comprises the following steps：
（1）Agitator, condenser pipe, thermometer are installed in 500ml three neck round bottom flask, and connect vacuum filtration machine；By three Mouth flask is placed in oil bath pan；230g octamethylcy-clotetrasiloxanes and 60g tetramethyl tetravinyls are added in there-necked flask Cyclotetrasiloxane, is warming up to 90 degree, and under N2 protections, magnetic agitation is evacuated to -0.08MPa, is dehydrated one hour；Add the benzene of 8g tetra- Base divinyl disiloxane and 6g TMAHs, are warming up to 110 DEG C, react three hours；System is warming up to again 160 DEG C, 1h is reacted, decompose catalyst, remove low-boiling-point substance under reduced pressure, obtain the i.e. phenyl end capped methyl ethylene silicon of product liquid Oil；
（2）Agitator, reflux condensing tube device and thermometer are connected in three neck round bottom flask, and install oil bath pan；To three Phenyl end capped methyl vinyl silicon oil, tetraphenylcyclopentadienone, α-chloronaphthalene are added in mouth round-bottomed flask；Oil bath pot temperature is set It is set to 220 DEG C, heating stirring backflow a few hours in N2 atmosphere；The widely different purple for flowing to tetraphenylcyclopentadienone of heating is decorporated, cold But, after layering, upper strata is product；
。
4. phenyl end capped methyl ethylene according to claim 3（Tetraphenyl）Phenyl modified silica gel preparation method, its feature It is that in step (1), octamethylcy-clotetrasiloxane is 4 with the mass ratio of t etram-ethyltetravinylcyclotetrasiloxane:1~ 19:1。
5. phenyl end capped methyl ethylene according to claim 3（Tetraphenyl）Phenyl modified silica gel preparation method, its feature It is that in step (1), described acidic catalyst is the concentrated sulfuric acid of mass fraction 98%, and consumption is reactant gross mass 0.0005%~0.5%.
6. phenyl end capped methyl ethylene according to claim 3（Tetraphenyl）Phenyl modified silica gel preparation method, it is special Levy and be, in step (1), tetraphenyl divinyl disiloxane is 1 with the mass ratio of TMAH:1.5~ 1:3。
7. phenyl end capped methyl ethylene according to claim 3（Tetraphenyl）Phenyl modified silica gel preparation method, it is special Levy and be, in step (2), described phenyl end capped methyl vinyl silicon oil:Tetraphenylcyclopentadienone:α-chloronaphthalene mole Than being 2.1:1:1.
CN201611224963.5A 2016-12-27 2016-12-27 One kind contains phenyl end capped methyl ethylene（Tetraphenyl）Phenyl modified silica gel and preparation method thereof Withdrawn CN106810700A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109749451A (en) * 2018-12-10 2019-05-14 沈阳化工大学 A kind of silicon rubber of Sakyamuni, the founder of Buddhism's molecule base POSS heat resistance accessory preparation
CN109749083A (en) * 2018-12-10 2019-05-14 沈阳化工大学 Eight (trimethoxy silica ethyl) poss silicone rubber crosslinking agent
CN109880523A (en) * 2019-03-18 2019-06-14 苏州世华新材料科技股份有限公司 Low transfer silicone release agent of a kind of high temperature resistant and preparation method thereof
CN111349241A (en) * 2020-04-30 2020-06-30 新纳奇材料科技江苏有限公司 Preparation method of vinyl phenyl silicone oil with high phenyl content

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Publication number Priority date Publication date Assignee Title
CN101704954A (en) * 2009-04-30 2010-05-12 山东大学 Tetraphenyl phenyl graft polysiloxane, preparation method thereof and application thereof
CN102432887A (en) * 2011-08-12 2012-05-02 浙江精业生化有限公司 Preparation method of polyester-modified silica gel
CN104672459A (en) * 2015-02-05 2015-06-03 上海应用技术学院 Vinyl phenyl silicon resin with side chain containing epoxy group and preparation method of vinyl phenyl silicon resin
CN105238067A (en) * 2015-11-09 2016-01-13 沈阳化工大学 High-temperature resistance silicone rubber coloring master batch and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101704954A (en) * 2009-04-30 2010-05-12 山东大学 Tetraphenyl phenyl graft polysiloxane, preparation method thereof and application thereof
CN102432887A (en) * 2011-08-12 2012-05-02 浙江精业生化有限公司 Preparation method of polyester-modified silica gel
CN104672459A (en) * 2015-02-05 2015-06-03 上海应用技术学院 Vinyl phenyl silicon resin with side chain containing epoxy group and preparation method of vinyl phenyl silicon resin
CN105238067A (en) * 2015-11-09 2016-01-13 沈阳化工大学 High-temperature resistance silicone rubber coloring master batch and preparation method thereof

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109749451A (en) * 2018-12-10 2019-05-14 沈阳化工大学 A kind of silicon rubber of Sakyamuni, the founder of Buddhism's molecule base POSS heat resistance accessory preparation
CN109749083A (en) * 2018-12-10 2019-05-14 沈阳化工大学 Eight (trimethoxy silica ethyl) poss silicone rubber crosslinking agent
CN109880523A (en) * 2019-03-18 2019-06-14 苏州世华新材料科技股份有限公司 Low transfer silicone release agent of a kind of high temperature resistant and preparation method thereof
CN111349241A (en) * 2020-04-30 2020-06-30 新纳奇材料科技江苏有限公司 Preparation method of vinyl phenyl silicone oil with high phenyl content

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Application publication date: 20170609