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Method for preparing resin from phenyl alkoxy silane high-boiling residue

A technology of phenylalkoxysilane and high boiler, which is applied in the field of preparing resin from phenylalkoxysilane high boiler, can solve the problems of poor mechanical properties of vulcanizate, difficult to control, complicated and tedious preparation process, etc. Inexpensive, inexpensive and flexible

Inactive Publication Date: 2020-04-24
湖北新四海化工股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Unreinforced vulcanizate has poor physical and mechanical properties and cannot meet the requirements, so reinforcing fillers must be added to reinforce the packaging material, but the addition of fillers can easily have a negative impact on the refractive index and light transmittance of the packaging material , which puts forward higher requirements for the selection of reinforcing fillers
[0003] Phenyl silicone resin has excellent electrical insulation, hydrophobicity, weather resistance, high temperature and low temperature resistance, radiation resistance and physiological inertness. However, most of the existing phenyl silicone resins have the following problems in the preparation process: preparation A large amount of acid wastewater is produced in the process; the preparation process is complex and cumbersome, and it is not easy to control

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Embodiment 1, a kind of method for preparing resin from phenylalkoxysilane high boiler comprises the following steps:

[0017] Press the phenylalkoxysilane high boiler, chlorosilane monomer, and part of the solvent into the dripping kettle by the feed pump for standby; part of the solvent, water, and alcohol are mixed into the reaction kettle, and the materials in the dropping kettle are added dropwise In the reaction kettle, control the reaction temperature at 15-55°C, and the dropwise addition time is 3-8h; after the dropwise addition, stir for 1-3h to separate the acidic water layer, and wash the silicone resin prepolymer 3-6 times to medium After deactivation, filter, evaporate the solvent, add a catalyst to polymerize, and add a solvent to cool down to obtain the finished phenyl silicone resin.

[0018] Among them, phenylalkoxysilane high boilers include high boilers produced by the production of phenyltrimethoxysilane and phenyltriethoxysilane;

[0019] Wherein, ...

Embodiment 2

[0023] Embodiment 2, a method for preparing resin from phenylalkoxysilane high boilers, comprising the following steps: 212 parts of phenylalkoxysilane high boilers, 45 parts of methyltrichlorosilane, 67 parts of dimethyl Dichlorosilane and 430 parts of xylene are pressed into the dripping kettle by the feed pump for subsequent use; 210 parts of toluene, 561 parts of water, and 242 parts of ethanol are allocated in the reactor, and the material in the dripping kettle is added dropwise in the reactor. Control the reaction temperature at 25-35°C, and the dropwise addition time is about 4 hours; after the dropwise addition, stir for 2 hours to separate the lower layer of acidic water, wash the upper layer of silicone resin prepolymer with water for 6 times until neutral, filter, and evaporate the solvent at low temperature Add 0.006 parts of manganese naphthenate, polymerize under reduced pressure at 140°C, add a solvent and cool down to get the finished phenyl silicone resin, the...

Embodiment 3

[0024] Embodiment 3, a method for preparing resin from phenylalkoxysilane high boilers, comprising the following steps: 183 parts of phenylalkoxysilane high boilers, 29 parts of methyltrichlorosilane, 76 parts of dimethyl Dichlorosilane, 51 parts of diphenyldichlorosilane, and 418 parts of xylene are pressed into the dripping kettle by the feed pump for standby; 324 parts of toluene, 411 parts of water, and 256 parts of methanol are allocated in the reaction kettle, and the dripping kettle Add the material in the reaction kettle dropwise, control the reaction temperature at 20-30°C, and drop the time for about 5 hours; after the drop is completed, stir for 2 hours to separate the lower layer of acid water, and wash the upper layer of silicone resin prepolymer with water for 5 times to After neutralization, filter, evaporate the solvent at low temperature, add 0.01 part of butyl titanate and polymerize under reduced pressure at 150°C, add solvent and cool down to get the finishe...

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PUM

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Abstract

The invention discloses a method for preparing resin from a phenyl alkoxy silane high-boiling residue. The method comprises the following steps: step (1) pressing the phenyl alkoxy silane high-boilingresidue, a chlorosilane monomer and part of a solvent into a dropwise adding kettle by a feeding pump for later use; and step (2) adding part of the solvent, water and alcohol into a reaction kettle,dropwise adding the material in the dropwise adding kettle into the reaction kettle, and controlling the reaction temperature to be 15-55 DEG C and the dropwise adding time to be 3-8 h; stirring for1-3 h after dropwise adding is finished, standing to separate out an acid water layer, washing the silicon resin prepolymer with water for 3-6 times until the silicon resin prepolymer is neutral, filtering, evaporating a solvent, adding a catalyst for polymerization, adding the solvent, and cooling to obtain the finished product phenyl silicon resin. The product produced by the method is low in cost and high in yield; the prepared silicon resin has good heat resistance, flexibility and insulation moisture resistance, and is suitable for electric insulation paint, high-temperature-resistant paint, coil impregnating varnish and the like.

Description

technical field [0001] The invention relates to the technical field of composite materials, in particular to a method for preparing resin from phenylalkoxysilane high boilers. Background technique [0002] Silicone materials have high refractive index, good light transmittance, good thermal stability, strong UV resistance, small internal stress, low moisture absorption, etc., and their performance is significantly better than epoxy resin, making them ideal for power LED packaging materials. Domestically, the R&D and production of power LED packaging materials are relatively backward, and most of the demand for power LED packaging materials in the domestic market depends on imports. Silicon packaging materials are the main materials and have an absolute advantage in the domestic high-end packaging market. In addition to high refractive index, light transmittance and ultraviolet radiation resistance, power LED packaging materials also require materials to have certain basic m...

Claims

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Application Information

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IPC IPC(8): C08G77/06C08G77/08C09D183/04C09D5/25
CPCC08G77/06C08G77/08C09D5/00C09D183/04
Inventor 邵玲龚家全杨帆杨开柱
Owner 湖北新四海化工股份有限公司
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