Preparation method for MDTQ type methyl phenyl vinyl silicone resin

A technology of methyl phenyl vinyl and MQ silicone resin, which is applied in the field of preparation of MDTQ type methyl phenyl vinyl silicone resin, can solve the problems of poor product stability, weak reinforcement contribution, low dosage, etc. Solubility problem, good resilience, good compatibility

Active Publication Date: 2014-11-19
江西新嘉懿新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

CN101475689B discloses the method for preparing MDT type methylphenylvinyl silicone resin with vinyl end-blocking agent, methylphenyldimethoxysilane and phenyltrimethoxysilane under the catalysis of trifluorosulfonic acid cation exchange resin , The refractive index of the product is 1.53 to 1.54. This method filters out the trifluorosulfonic acid cation exchange resin immediately after the hydrolysis is completed and then degrades, which is not conducive to the further condensation of the residual hydroxyl and alkoxy groups in the delowering process, and the product stability is poor; CN103819678A discloses with hexamethyldisiloxane, diphenylsilanediol, diphenyldimethoxysilane and methyltrimethoxysilane, vinyltrimethoxysilane under the catalysis of tetramethylammonium hydroxide , toluene as a solvent, the method for preparing MDT-type methylphenyl vinyl silicone resin, the product has a refractive index of 1.50 to 1.57, this method has poor stability, and the product is solid, which is difficult to pack and use
[0009] Although tetraethyl orthosilicate is also added in the above-mentioned patents, its dosage is extremely low, less than 1% of the feeding amount, and its contribution to reinforcement is weak, and it is all synthesized in one step by "one-pot method". Form an MQ-type structure with a reinforcing effect and an M / Q value of 0.6~0.9

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] To the flask was added 68.6 g tetramethyldivinyldisiloxane, 102 g hexamethyldisiloxane, 396 g phenyltrimethoxysilane, 182 g methylphenyldimethoxysilane and 600 g methylcyclohexyl alkane, stir well. 30 g of p-toluenesulfonic acid was added as a catalyst, and then 1000 g of deionized water was added dropwise for hydrolysis. After the dropwise addition was completed, the temperature was raised to 70° C. for constant temperature aging for 3 hours, then cooled to room temperature, liquid separation was carried out, and 1162 g of the organic layer was taken and weighed. Transfer to a clean beaker, which is the hydroxyl-containing MDT type methylphenylvinyl silicone resin prepolymer solution (component A).

[0027]Add 1000g of deionized water and 50g of p-toluenesulfonic acid to another flask, stir evenly, and then slowly add 674g of ethyl orthosilicate dropwise for hydrolysis. After the dropwise addition, 500g of methylcyclohexane and 236g of hexamethyldisiloxane were added...

Embodiment 2

[0030] To the flask was added 174 g tetramethyldivinyldisiloxane, 10.65 g hexamethyldisiloxane, 396 g phenyltrimethoxysilane, 182 g methylphenyldimethoxysilane and 600 g methylcyclohexyl alkane, stir well. 30 g of p-toluenesulfonic acid was added as a catalyst, and then 1000 g of deionized water was added dropwise for hydrolysis. After the dropwise addition was completed, the temperature was raised to 70° C. for constant temperature aging for 3 hours, then cooled to room temperature, liquid separation was carried out, and 1175 g of the organic layer was taken and weighed. Transfer to a clean beaker, which is the hydroxyl-containing MDT type methylphenylvinyl silicone resin prepolymer solution (component A).

[0031] Add 1000g of deionized water and 50g of p-toluenesulfonic acid to another flask, stir evenly, and then slowly add 591g of ethyl orthosilicate dropwise for hydrolysis. After the dropwise addition, 500g of methylcyclohexane and 161g of hexamethyldisiloxane were add...

Embodiment 3

[0034] The preparation method of the hydroxyl-containing MDT type methyl phenyl vinyl resin prepolymer solution (component A) is the same as in Example 2.

[0035] Add 1000g of deionized water and 50g of p-toluenesulfonic acid to another flask, stir evenly, then slowly add 740g of ethyl orthosilicate dropwise for hydrolysis. After the dropwise addition, 500g of methylcyclohexane and 260g of hexamethyldisiloxane were added, and the temperature was raised to 70°C for constant temperature aging for 3 hours, then cooled to room temperature, separated, and the organic layer was taken to weigh 967g. Transfer to a clean beaker, which is the hydroxyl-containing MQ silicone resin prepolymer solution (component B).

[0036] Mix the above-mentioned component A and component B according to the mass ratio of 1.2:1, stir evenly, then add 1gKOH, heat up to reflux, and distill the water produced by the condensation with a water separator at the same time, stir and react for 3 hours, stop heat...

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Abstract

A preparation method for MDTQ type methyl phenyl vinyl silicone resin is characterized by comprising the following steps: mixing MDT type methyl phenyl vinyl silicone resin prepolymer solution containing a hydroxyl with MQ type silicone resin prepolymer solution containing a hydroxyl, heating and reflowing, so as to distil off water generated from condensation; stirring for reaction, stopping heating, and cooling to the room temperature; then washing until the mixture is neutral, drying, decoloring, and separating out a solvent and a low-molecular-weight compound under the vacuum condition, so as to obtain the colorless and transparent MDTQ type methyl phenyl vinyl silicone resin reinforced by the MQ silicon resin. The methyl phenyl vinyl silicone resin provided by the invention is high in light transmittance, clear and transparent, has excellent intermiscibility with phenyl vinyl silicone oil and phenyl hydrogen-contained silicon resin, can be used for preparing phenyl silicone rubber, has excellent reinforcing effect, and enables the silicone rubber to be excellent in resilience, tearing resistant, hot-cold impact resistant, heatproof, radiation resistant and ageing resistant.

Description

technical field [0001] The invention relates to a method for preparing methylphenylvinyl silicone resin, in particular to a method for preparing MDTQ type methylphenylvinyl silicone resin reinforced with MQ silicone resin. Background technique [0002] The methyl phenyl vinyl silicone resin described in the present invention is the basic raw material for the preparation of addition-type phenyl silicone rubber. Reinforcing fillers must be added to the formula of the silicone rubber, otherwise the silicone rubber will not have mechanical properties and strength after vulcanization and cannot be used. Commonly used reinforcing fillers are white carbon black, carbon black, calcium carbonate, MQ silicone resin, etc. MQ silicone resin is composed of monofunctional chain link M (M represents hexamethyldisiloxane) and tetrafunctional chain link Q (Q represents SiO 2 ) is an organosiloxane product with a relatively special structure, and only when the M / Q value is 0.6~0.9 can it hav...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/44C08G77/20C08G77/16C08G77/08
Inventor 朱淮军戴子林涂伟萍
Owner 江西新嘉懿新材料有限公司
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