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Method for preparing phenyl vinyl silicon resin by non-hydrolyzing method

A phenyl vinyl silicon, non-hydrolysis technology, applied in the field of new organic silicon materials, non-hydrolysis preparation of phenyl vinyl silicone resin, to achieve the effect of high molecular weight, clean and environmentally friendly synthesis process, regular chemical structure

Inactive Publication Date: 2014-02-12
INST OF APPLIED CHEM JIANGXI ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] The synthesis of traditional silicone resins is generally made from a mixture of various organosilanes, which are prepared through hydrolysis, polycondensation, neutralization and other reactions in a mixed solvent. The reaction process A large amount of acid water and toxic volatile gases are produced in the process. This synthesis process is not conducive to the sustainable development of the organic silicon industry and has caused great harm to the environment.
Silicone resins synthesized by traditional chlorosilane or alkoxysilane hydrolysis methods tend to generate linear, cyclic or cross-linked polysiloxanes with different degrees of polymerization during polycondensation due to the different degrees of hydrolysis of organosilicon monomers. The existence of the structure directly leads to the instability of the physical and chemical properties of the synthesized silicone resin

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Add 15.4 parts of methylphenyldihydroxysilane, 14.8 parts of vinyltrimethoxysilane and 0.11 parts of barium hydroxide monohydrate into a three-neck flask, stir and heat up to 80°C under nitrogen protection, dehydrate under reduced pressure for 1 hour, and then heat up to 90°C After the equilibrium reaction for 3 hours, continue to raise the temperature to 150°C to remove the low molecular weight and obtain the phenylvinyl silicone resin.

Embodiment 2

[0023] Add 15.8 parts of phenyltrihydroxysilane, 13.2 parts of methylvinyldimethoxysilane and 0.12 parts of barium hydroxide monohydrate into a three-necked flask, stir and heat up to 85°C under nitrogen protection, dehydrate under reduced pressure for 1 hour, and then heat up to Carry out the polymerization reaction at 95°C, and continue to heat up to 150°C after the equilibrium reaction for 3.5 hours to remove low-molecular substances by vacuuming to obtain the phenyl vinyl silicone resin.

Embodiment 3

[0025] Add 21.6 parts of diphenyldihydroxysilane, 14.8 parts of vinyltrimethoxysilane and 0.15 parts of barium hydroxide monohydrate into a three-necked flask, stir and heat up to 85°C under nitrogen protection, dehydrate under reduced pressure for 1 hour, and then heat up to 95°C Carry out the polymerization reaction, and after the equilibrium reaction for 3.5 hours, continue to heat up to 150°C and vacuumize to remove the low-molecular substances to obtain the phenyl vinyl silicone resin.

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Abstract

The invention discloses a method for preparing phenyl vinyl silicon resin by a non-hydrolyzing method. The method adopts the non-hydrolyzing method to conduct condensation polymerization on a certain amount of hydroxyl-terminated organosilane and vinyl-terminated organosilane in an environment without water and solvent under the catalysis of a metal hydroxide or a metal organic salt hydroxide to prepare the phenyl vinyl silicon resin. The specific steps are as follows: the hydroxyl-terminated organosilane, the vinyl-terminated organosilane and the metal hydroxide or the metal organic salt hydroxide are stirred and heated up to be at 75-85 DEG C under the nitrogen protection in a flask until the three are homogeneous and transparent, subjected to pressure reduction to dehydrate, are heated up to be at 90-95 DEG C for polymerization, continuously heated up be at 150 DEG C after being in a balanced reaction for 3 hours, and vacuumized to remove low-molecular substances to obtain the phenyl vinyl silicon resin. The preparation method is simple; the synthetic technique is clean and environmentally-friendly; poisonous three-waste byproducts are avoided. The preparation method is suitable for LED packaging materials.

Description

technical field [0001] The invention relates to a method for preparing phenylvinyl silicone resin by a non-hydrolysis method, which belongs to the research field of new organic silicon materials. Background technique [0002] The synthesis of traditional silicone resins is generally made from a mixture of various organosilanes through hydrolysis, polycondensation, neutralization and other reactions in a mixed solvent. A large amount of acid water and toxic volatile gases are produced during the reaction process. The synthesis process It is not conducive to the sustainable development of the organic silicon industry, and has also caused great harm to the environment. Silicone resins synthesized by traditional chlorosilane or alkoxysilane hydrolysis methods tend to generate linear, cyclic or crosslinked polysiloxanes with different degrees of polymerization during polycondensation due to the different degrees of hydrolysis of organosilicon monomers. The existence of the str...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/20C08G77/08
Inventor 董晓娜陈衍华谌开红游胜勇张鹏
Owner INST OF APPLIED CHEM JIANGXI ACAD OF SCI