CN104892943A - High-refraction-index phenyl vinyl silicone oil and preparation method thereof - Google Patents
High-refraction-index phenyl vinyl silicone oil and preparation method thereof Download PDFInfo
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- CN104892943A CN104892943A CN201510315144.0A CN201510315144A CN104892943A CN 104892943 A CN104892943 A CN 104892943A CN 201510315144 A CN201510315144 A CN 201510315144A CN 104892943 A CN104892943 A CN 104892943A
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Abstract
The invention discloses high-refraction-index phenyl vinyl silicone oil and a preparation method thereof. The preparation method comprises the following steps: performing dehydration pretreatment to raw materials, including methyl phenyl cyclosiloxane and dimethyl cyclosiloxane, adding a defined amount of end-capping agent, stirring uniformly, and adding an alkaline catalyst; in a nitrogen atmosphere, heating for polymerization reaction, and cooling to room temperature after the reaction is over; adding excessive acidic neutralizing agent, stirring for full neutralization, and washing with deionized water to a neutral degree; performing stratification by standing, collecting a product layer, and removing low molecules in vacuum to obtain the phenyl vinyl silicone oil. The process is simple, is easy to control and generates no waste gas. The product has high reactivity without peculiar smell, resists radiation and high and low temperature, has high storage stability, can be widely applied to the field of silicone rubber, is particularly suitable for LED organic silicon encapsulating material, and can effectively improve the luminous efficiency and reduce the energy consumption.
Description
Technical field
The present invention relates to a kind of silicone oil, be specifically related to phenyl-vinyl silicon oil of a kind of high refractive index and preparation method thereof.
Technical background
In organosilicon product, silicone oil of a great variety, wherein phenyl silicone oil is one of its principal item.Phenyl silicone oil possesses insulativity, ozone resistants, hydrophobic protection against the tide, high-low temperature resistant and radioresistance, is widely used in the fields such as electronics, machinery and cosmetics of everyday use.In additional organosilicon material, the refractive index of phenyl-vinyl silicon oil is high, is conducive to the output of light, thus becomes the base polymer of LED encapsulation material first-selection.
Traditional phenyl silicone oil is connected with two methyl for repeating unit same Siliciumatom to be connected with on two phenyl and same Siliciumatom.With solid-state octaphenylcyclotetrasiloxane and liquid octamethylcyclotetrasiloxane for monomer prepares phenyl-vinyl silicon oil, because the compatibility of two kinds of monomers is poor, copolymerization is difficult to uniform alternating copolymerization.The product prepared of this method in view of the refractive index of segment different in molecular chain different, the phenyl-vinyl silicon oil transparency thus obtained is poor.
At present, the structure mainly dimethyl diphenyl silicone oil of phenyl silicone oil, be raw material by methyl dioxane TMOS, phenylbenzene dialkoxy silicane, diphenyl dichlorosilane, dialkyl dialkoxy silicane and hydroxy-end capped low polymerization degree dimethyldiphenylsiloxane etc., through hydrolysis, condensation, neutralization, by steps such as deionized water washings.The skill of the preparation of this type of phenyl silicone oil is loaded down with trivial details, cost is high and efficiency is low.China Patent Publication No. is the preparation method that CN102432883A describes a kind of phenyl-vinyl silicon oil, by being raw material with vinyl epoxy base silane, methyl epoxy radicals silicone hydride after phenyl alkoxysilane hydrolysis, by polyreaction, organic solvent extraction, be washed to the step acquisition phenyl-vinyl silicon oils such as neutral decompression is de-low.This method employs organic solvent toluene, is unfavorable for environmental protection, does not have acid neutralization, is only difficult to remove basic catalyst by washing, causes product stock stability to reduce.In addition, the product of phenyl-vinyl silicon oil that CN1569925A uses amines catalyst to obtain, but due to catalyst decomposition products part residual in the product, product can be made to have amine taste.
Summary of the invention
The object of the invention is for the deficiencies in the prior art, phenyl-vinyl silicon oil of a kind of high refractive index and preparation method thereof is provided.
The object of the invention is to be achieved through the following technical solutions: a kind of phenyl-vinyl silicon oil of high refractive index, described phenyl-vinyl silicon oil is made up of the end-capping reagent of the monomer of 100 weight parts, 0.5-5 weight part, catalyzer and neutralizing agent, wherein the quality of catalyzer be monomer and end-capping reagent total mass 0.005% ~ 0.01%, neutralizing agent quality is 0.005% ~ 0.02% of monomer and end-capping reagent total mass; Described monomer is made up of the methyl phenyl ring siloxane of 70-100 weight part, the dimethicone of 0-30 weight part.
Further, methyl phenyl ring siloxane is one or more mixtures formed according to any proportioning in aminomethyl phenyl cyclotrisiloxane, aminomethyl phenyl cyclotetrasiloxane, aminomethyl phenyl D5.
Further, dimethicone is the multiple mixture formed according to any proportioning in hexamethyl cyclotrisiloxane, octamethylcyclotetrasiloxane, decamethylcyclopentaandoxane, ten diformazan basic ring six siloxanes.
Further, end-capping reagent is divinyl tetramethyl disiloxane.
Further, catalyzer is the one in potassium hydroxide powder, sodium hydroxide powder.
Further, neutralizing agent is CH
3cOOH, H
3pO
4in one.
A kind of preparation method of phenyl-vinyl silicon oil of high refractive index, comprise the following steps: (1) is by the monomer of 100 weight parts, the i.e. methyl phenyl ring siloxane of 70-100 weight part and the dimethicone of 0-30 weight part, after mixing, at 50-60 DEG C, vacuum tightness is under the condition of ﹣ 0.090-﹣ 0.100MPa, dehydration 0.5-2h; Add the end-capping reagent of 0.5-5 weight part, after stirring, add catalyzer again; Reaction system is replaced into nitrogen atmosphere, is then warming up to 130-150 DEG C, polyreaction for some time, after unchanged to viscosity, stop heating, is cooled to room temperature; (2) add neutralizing agent, after stirring at room temperature 0.5-1h, by the deionized water washing of the product after stirring reaction, leave standstill, obtain silicon layer; (3) to silicon layer after 50 DEG C of silicone oil vacuum hydro-extraction, be warming up to 190-210 DEG C, decompression is de-to be low to moderate and to flow out without cut, the phenyl-vinyl silicon oil of acquisition high refractive index.
Beneficial effect of the present invention is: phenyl-vinyl silicon oil of the present invention is made up of end-capping reagent, catalyzer, neutralizing agent, methyl phenyl ring siloxane, dimethicone.Owing to selecting dimethicone, methyl phenyl ring siloxane to be monomer, be conducive to phenyl being uniformly distributed in silicone molecule chain; Select potassium hydroxide, sodium hydroxide to be catalyzer, use sour catalyst neutralisation, do not have catalyst residue, make product stock good stability and free from extraneous odour, Heat stability is good; Catalyst levels is little, and use Determining Micro Acid neutralization, the salt of generation is few, is convenient to washing and effectively reduces potassium ion, sodium ions content in silicone oil; Decompression dehydration after washing, temperature programming, guarantees that water and low-boiling-point substance remove completely.In a word, due to from the selection of raw material and the strict controls of step such as monomer, catalyzer, neutralizing agents, adopt present method to obtain phenyl-vinyl silicon oil, phenyl is uniformly distributed that product storage stability is good, refractive index is high and transmittance is high.This method is simple to operate, be easy to control.
Embodiment
Below in conjunction with embodiment, the invention will be further described:
Embodiment 1
Be equipped with in the reactor of whipping appts, condenser system and thermometer at one and add 70.0g methyl phenyl ring siloxane and 30.0 parts of dimethicone mixtures, 50 DEG C, under vacuum tightness is ﹣ 0.095MPa, constant temperature dehydration 1h; Add 2g divinyl tetramethyl disiloxane, after stirring, then add the KOH of 0.005g, system is replaced into nitrogen atmosphere, is warmed up to 130 DEG C, and after reacting about 8h, viscosity no longer changes; Be cooled to room temperature.By massfraction be 1% phosphoric acid solution be added drop-wise in cooling fluid, wherein containing the H of 0.005g
3pO
4, after stirring at room temperature 0.5h, the product obtained by stirring reaction is placed in separating funnel, washes away the inorganic salt in product with deionized water, has washed rear leaving standstill, has obtained silicone oil.By the silicone oil of acquisition after 50 DEG C of silicone oil vacuum hydro-extraction, then be warming up to 190 DEG C, decompression takes off to be low to moderate and flows out without obvious cut.
Test data: refractive index is 1.509, transmittance is 98.9% (500nm), and viscosity is 1300mPa.s, and potassium content is 9ppm.
Embodiment 2
Be equipped with in the reactor of whipping appts, condenser system and thermometer at one and add 75.0g methyl phenyl ring siloxane and 25.0g dimethicone mixture, 50 DEG C, under vacuum tightness is ﹣ 0.010MPa, constant temperature dehydration 1h; Add 2g divinyl tetramethyl disiloxane, after stirring, then add the KOH of 0.006g, system is replaced into nitrogen atmosphere, is warmed up to 130 DEG C, and after reacting about 7h, viscosity no longer changes; Be cooled to room temperature.Phosphoric acid solution is added drop-wise in cooling fluid, the H wherein containing 0.006g
3pO
4, after stirring at room temperature 0.5h, the product obtained by stirring reaction is placed in separating funnel, washes away the inorganic salt in product with deionized water, has washed rear leaving standstill, has obtained silicone oil.By the silicone oil of acquisition after 50 DEG C of silicone oil vacuum hydro-extraction, then be warming up to 200 DEG C, decompression takes off to be low to moderate and flows out without obvious cut.
Test data: refractive index is 1.513, transmittance is 98.5% (500nm), and viscosity is 1450mPa.s, and potassium content is 11ppm.
Embodiment 3
Be equipped with in the reactor of whipping appts, condenser system and thermometer at one and add 80.0g methyl phenyl ring siloxane and 20.0g dimethicone mixture, 60 DEG C, under vacuum tightness is ﹣ 0.090MPa, constant temperature dehydration 1h; Add 0.5g divinyl tetramethyl disiloxane, after stirring, then add the KOH of 0.01g, system is replaced into nitrogen atmosphere, is warmed up to 150 DEG C, and after reacting about 4h, viscosity no longer changes; Be cooled to room temperature.Acetum (1wt%) is added drop-wise in cooling fluid, the CH wherein containing 0.02g
3cOOH, after stirring at room temperature 0.5h, the product obtained by stirring reaction is placed in separating funnel, washes away the inorganic salt in product with deionized water, has washed rear leaving standstill, has obtained silicone oil.By the silicone oil of acquisition 50 DEG C of silicone oil vacuum hydro-extraction for some time, then be warming up to 200 DEG C, decompression takes off to be low to moderate and flows out without obvious cut.
Test data: refractive index is 1.519, transmittance is 98.8% (500nm), and viscosity is 6600mPa.s, and potassium content is 16ppm.
Embodiment 4
Be equipped with in the reactor of whipping appts, condenser system and thermometer at one and add 85.0g methyl phenyl ring siloxane and 15.0g dimethicone mixture, 50 DEG C, under vacuum tightness is ﹣ 0.090MPa, constant temperature dehydration 2h; Add 3g divinyl tetramethyl disiloxane, after stirring, then add the KOH of 0.008g, system is replaced into nitrogen atmosphere, is warmed up to 150 DEG C, and after reacting about 5h, viscosity no longer changes; Be cooled to room temperature.Acetum is added drop-wise in cooling fluid, the CH wherein containing 0.015g
3cOOH, after stirring at room temperature 0.5h, the product obtained by stirring reaction is placed in separating funnel, washes away the inorganic salt in product with deionized water, has washed rear leaving standstill, has obtained silicone oil.By the silicone oil of acquisition 50 DEG C of silicone oil vacuum hydro-extraction for some time, then be warming up to 200 DEG C, decompression takes off to be low to moderate and flows out without obvious cut.
Test data: refractive index is 1.527, transmittance is 98.2% (500nm), and viscosity is 850mPa.s, and potassium content is 13ppm.
Embodiment 5
Be equipped with in the reactor of whipping appts, condenser system and thermometer at one and add 85.0g methyl phenyl ring siloxane and 15.0g dimethicone mixture, 55 DEG C, under vacuum tightness is ﹣ 0.095MPa, constant temperature dehydration 1h; Add 1.5g divinyl tetramethyl disiloxane, after stirring, then add the NaOH of 0.01g, system is replaced into nitrogen atmosphere, is warmed up to 140 DEG C, and after reacting about 6h, viscosity no longer changes; Be cooled to room temperature.Phosphoric acid solution is added drop-wise in cooling fluid, the H wherein containing 0.012g
3pO
4, after stirring at room temperature 0.5h, the product obtained by stirring reaction is placed in separating funnel, washes away the inorganic salt in product with deionized water, has washed rear leaving standstill, has obtained silicone oil.By the silicone oil of acquisition 50 DEG C of silicone oil vacuum hydro-extraction for some time, then be warming up to 200 DEG C, decompression takes off to be low to moderate and flows out without obvious cut.
Test data: refractive index is 1.527, transmittance is 98.0% (500nm), and viscosity is 1650mPa.s, and sodium ions content is 13ppm.
Embodiment 6
Be equipped with in the reactor of whipping appts, condenser system and thermometer at one and add 90.0g methyl phenyl ring siloxane and 10.0g dimethicone mixture, 60 DEG C, under vacuum tightness is ﹣ 0.090MPa, constant temperature dehydration 1h; Add 2g divinyl tetramethyl disiloxane, after stirring, then add the KOH of 0.008g, system is replaced into nitrogen atmosphere, is warmed up to 150 DEG C, and after reacting about 5h, viscosity no longer changes; Be cooled to room temperature.Phosphoric acid solution is added drop-wise in cooling fluid, the H wherein containing 0.01g
3pO
4, after stirring at room temperature 0.5h, the product obtained by stirring reaction is placed in separating funnel, washes away the inorganic salt in product with deionized water, has washed rear leaving standstill, has obtained silicone oil.By the silicone oil of acquisition 50 DEG C of silicone oil vacuum hydro-extraction for some time, then be warming up to 210 DEG C, decompression takes off to be low to moderate and flows out without obvious cut.
Test data: refractive index is 1.537, transmittance is 97.8% (500nm), and viscosity is 2000mPa.s, and sodium ions content is 10ppm.
Embodiment 7
Be equipped with in the reactor of whipping appts, condenser system and thermometer at one and add 90.0g methyl phenyl ring siloxane and 10.0g dimethicone mixture, 60 DEG C, under vacuum tightness is ﹣ 0.010MPa, constant temperature dehydration 0.5h; Add 5g divinyl tetramethyl disiloxane, after stirring, then add the NaOH of 0.0075g, system is replaced into nitrogen atmosphere, is warmed up to 140 DEG C, and after reacting about 7h, viscosity no longer changes; Be cooled to room temperature.Phosphoric acid solution is added drop-wise in cooling fluid, the H wherein containing 0.01g
3pO
4, after stirring at room temperature 1h, the product obtained by stirring reaction is placed in separating funnel, washes away the inorganic salt in product with deionized water, has washed rear leaving standstill, has obtained silicone oil.By the silicone oil of acquisition 50 DEG C of silicone oil vacuum hydro-extraction for some time, then be warming up to 210 DEG C, decompression takes off to be low to moderate and flows out without obvious cut.
Test data: refractive index is 1.536, transmittance is 96.8% (500nm), and viscosity is 10500mPa.s sodium ions content is 10ppm.
Embodiment 8
Be equipped with in the reactor of whipping appts, condenser system and thermometer at one and add 95.0g methyl phenyl ring siloxane and 5.0g dimethicone mixture, 60 DEG C, under vacuum tightness is ﹣ 0.095MPa, constant temperature dehydration 1h; Add 2g divinyl tetramethyl disiloxane, after stirring, then add the KOH of 0.005g, system is replaced into nitrogen atmosphere, is warmed up to 140 DEG C, and after reacting about 8h, viscosity no longer changes; Be cooled to room temperature., acetum is added drop-wise in cooling fluid, the CH wherein containing 0.01g
3cOOH, after stirring at room temperature 1h, the product obtained by stirring reaction is placed in separating funnel, washes away the inorganic salt in product with deionized water, has washed rear leaving standstill, has obtained silicone oil.By the silicone oil of acquisition 50 DEG C of silicone oil vacuum hydro-extraction for some time, then be warming up to 200 DEG C, decompression takes off to be low to moderate and flows out without obvious cut.
Test data: refractive index is 1.543, transmittance is 97.2% (500nm), and viscosity is 2100mPa.s, and potassium content is 8ppm.
Embodiment 9
Be equipped with in the reactor of whipping appts, condenser system and thermometer at one and add 100.0g methyl phenyl ring siloxane, 60 DEG C, under vacuum tightness is ﹣ 0.010MPa, constant temperature dehydration 0.5h; Add 5g divinyl tetramethyl disiloxane, after stirring, then add the NaOH of 0.0075g, system is replaced into nitrogen atmosphere, is warmed up to 140 DEG C, and after reacting about 7h, viscosity no longer changes; Be cooled to room temperature.Phosphoric acid solution is added drop-wise in cooling fluid, the H wherein containing 0.01g
3pO
4, after stirring at room temperature 1h, the product obtained by stirring reaction is placed in separating funnel, washes away the inorganic salt in product with deionized water, has washed rear leaving standstill, has obtained silicone oil.By the silicone oil of acquisition 50 DEG C of silicone oil vacuum hydro-extraction for some time, then be warming up to 210 DEG C, decompression takes off to be low to moderate and flows out without obvious cut.
Test data: refractive index is 1.548, transmittance is 95.8% (500nm), and viscosity is 650mPa.s, and sodium ions content is 9ppm.
The Data Summary of embodiment, carries out test analysis from refractive index, transmittance and viscosity to the product obtained, and find that the raw material ratio of monomer determines the refractive index of product, and refractive index is all higher than 1.5%; Product, in visible-range, all possesses high transmission rate; The viscosity of product can reach and control hundreds of to up to ten thousand.
Claims (7)
1. the phenyl-vinyl silicon oil of a high refractive index, it is characterized in that: described phenyl-vinyl silicon oil is made up of the end-capping reagent of the monomer of 100 weight parts, 0.5-5 weight part, catalyzer and neutralizing agent, wherein the quality of catalyzer be monomer and end-capping reagent total mass about 0.005% ~ 0.01%, neutralizing agent quality is about 0.005% ~ 0.02% of monomer and end-capping reagent total mass; Described monomer is generally made up of the methyl phenyl ring siloxane of 70-100 weight part, the dimethicone of 0-30 weight part.
2. the phenyl-vinyl silicon oil of a kind of high refractive index according to claims 1, is characterized in that: methyl phenyl ring siloxane is one or more mixtures formed according to any proportioning in aminomethyl phenyl cyclotrisiloxane, aminomethyl phenyl cyclotetrasiloxane, aminomethyl phenyl D5.
3. the phenyl-vinyl silicon oil of a kind of high refractive index according to claims 1, is characterized in that: dimethicone is the multiple mixture formed according to any proportioning in hexamethyl cyclotrisiloxane, octamethylcyclotetrasiloxane, decamethylcyclopentaandoxane, ten diformazan basic ring six siloxanes.
4. the phenyl-vinyl silicon oil of a kind of high refractive index according to claims 1, is characterized in that: end-capping reagent is divinyl tetramethyl disiloxane.
5. the phenyl-vinyl silicon oil of a kind of high refractive index according to claims 1, is characterized in that: catalyzer is the one in potassium hydroxide powder, sodium hydroxide powder.
6. the phenyl-vinyl silicon oil of a kind of high refractive index according to claims 1, is characterized in that: neutralizing agent is CH
3cOOH, H
3pO
4in one.
7. the preparation method of the phenyl-vinyl silicon oil of the high refractive index described in claims 1, it is characterized in that, comprise the following steps: (1) is by the monomer of 100 weight parts, the i.e. methyl phenyl ring siloxane of 70-100 weight part and the dimethicone of 0-30 weight part, after mixing, at 50-60 DEG C, vacuum tightness is under the condition of ﹣ 0.090-﹣ 0.100MPa, dehydration 0.5-2h; Add the end-capping reagent of 0.5-5 weight part, after stirring, add catalyzer again; Reaction system is replaced into nitrogen atmosphere, is then warming up to 130-150 DEG C, polyreaction for some time, after unchanged to viscosity, stop heating, is cooled to room temperature; (2) add neutralizing agent, after stirring at room temperature 0.5-1h, by the deionized water washing of the product after stirring reaction, leave standstill, obtain silicon layer; (3) to silicon layer after 50 DEG C of silicone oil vacuum hydro-extraction, be warming up to 190-210 DEG C, decompression is de-to be low to moderate and to flow out without cut, the phenyl-vinyl silicon oil of acquisition high refractive index.
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| CN105754104A (en) * | 2016-05-18 | 2016-07-13 | 上海化工研究院 | Preparation method of methyl phenyl vinyl silicone oil with controllable refractive index |
| CN109957327A (en) * | 2017-12-26 | 2019-07-02 | 中国科学院长春应用化学研究所 | A kind of method that long-acting hydrophobic self-cleaning surface can be constructed in multiple material substrate |
| CN110229337A (en) * | 2019-07-11 | 2019-09-13 | 枣阳市华威硅氟材料有限公司 | The production method of phenyl methyl silicone oil |
| CN110591098A (en) * | 2019-10-09 | 2019-12-20 | 浙江新安化工集团股份有限公司 | Methyl phenyl vinyl silicone oil and preparation method and application thereof |
| CN111560119A (en) * | 2020-07-09 | 2020-08-21 | 威海新元化工有限公司 | Preparation method of dimethyl diphenyl polysiloxane |
| CN112940260A (en) * | 2021-03-01 | 2021-06-11 | 陈亚荣 | Production method of low-viscosity high-refractive index benzyl silicone oil |
| CN113321810A (en) * | 2021-06-01 | 2021-08-31 | 万华化学集团股份有限公司 | Q-type high-refraction phenyl vinyl silicone oil, and synthesis method and application thereof |
| CN115028839A (en) * | 2022-07-11 | 2022-09-09 | 桂林宝龙达新材料有限公司 | Preparation method of methyl phenoxy silicone oil |
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| CN105754104A (en) * | 2016-05-18 | 2016-07-13 | 上海化工研究院 | Preparation method of methyl phenyl vinyl silicone oil with controllable refractive index |
| CN109957327A (en) * | 2017-12-26 | 2019-07-02 | 中国科学院长春应用化学研究所 | A kind of method that long-acting hydrophobic self-cleaning surface can be constructed in multiple material substrate |
| CN109957327B (en) * | 2017-12-26 | 2021-08-24 | 中国科学院长春应用化学研究所 | Method for constructing long-acting hydrophobic self-cleaning surface on various material substrates |
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| CN110591098A (en) * | 2019-10-09 | 2019-12-20 | 浙江新安化工集团股份有限公司 | Methyl phenyl vinyl silicone oil and preparation method and application thereof |
| CN111560119A (en) * | 2020-07-09 | 2020-08-21 | 威海新元化工有限公司 | Preparation method of dimethyl diphenyl polysiloxane |
| CN112940260A (en) * | 2021-03-01 | 2021-06-11 | 陈亚荣 | Production method of low-viscosity high-refractive index benzyl silicone oil |
| CN113321810A (en) * | 2021-06-01 | 2021-08-31 | 万华化学集团股份有限公司 | Q-type high-refraction phenyl vinyl silicone oil, and synthesis method and application thereof |
| CN115028839A (en) * | 2022-07-11 | 2022-09-09 | 桂林宝龙达新材料有限公司 | Preparation method of methyl phenoxy silicone oil |
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Address after: 311300 Ling'an Province, Hangzhou City, Jin Jin Bao street, North Street Applicant after: Hangzhou Forster applied materials Limited by Share Ltd Address before: 311300 Ling'an Province, Hangzhou City, Jin Jin Bao street, North Street Applicant before: Hangzhou First PV Material Co., Ltd. |
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Application publication date: 20150909 |
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| RJ01 | Rejection of invention patent application after publication |