Unlock instant, AI-driven research and patent intelligence for your innovation.

Preparation method of toughened high temperature resistant silicone resin

A technology of high temperature resistance and silicone resin, applied in the field of preparation of toughened and high temperature resistant silicone resin, can solve the problems of low impact resistance, intense reaction process, poor toughness, etc., and achieve the effect of high impact resistance

Active Publication Date: 2016-08-03
SHANGHAI RESIN FACTORY
View PDF2 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Since chlorosilane is generally used as a monomer for hydrolysis and condensation to make silicone resin, the reaction process is intense and complicated. In large-scale production, the process is complicated, the product quality is unstable, and the efficiency is low. A large amount of acid-containing wastewater will be generated during the reaction process. Wastewater treatment costs are extremely high; and toxic aromatic solvents are often used in the production process, which seriously pollutes the environment during production and use, which is not conducive to environmental protection
[0005] However, the high-temperature-resistant silicone resin prepared by the current method has the advantages of high hardness, wear resistance, and good insulation performance, but its toughness is not good enough. As a coating insulation material, it will sometimes crack under high and low temperature alternating conditions. Low strength limits its application

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Add 97 parts by mass of methyltriethoxysiloxane and 3 parts by mass of dimethyldiethoxysiloxane into the reactor, heat up to 50°C under stirring, then add 24 parts by mass of water dropwise With the mixture of 0.04 parts by mass of hydrochloric acid, the temperature is maintained at about 50°C during the dropwise addition, and the dropwise addition time is 27 minutes;

[0031] After the dropwise addition, 20 parts by mass of the toughening agent 208 hydroxy silicone oil was added, after stirring evenly, the temperature was raised to about 83°C, and condensed and refluxed for 3.5 hours.

[0032] After the reflux is completed, the pressure is reduced to -0.03MPa, and the by-products of the reaction are slowly released until no by-products are released from the reaction system.

[0033] Heat up to 100°C for polycondensation and keep for 35 minutes;

[0034] Add 0.07 parts by mass of neutralizing agent hexamethyldisilazane to neutralize;

[0035] Add ethanol to adjust the...

Embodiment 2

[0038] Add 90 parts by mass of methyltriethoxysiloxane and 10 parts by mass of dimethyldiethoxysiloxane into the reactor, raise the temperature to 80°C under stirring, and then add dropwise 36 The mixture of water and 0.12 parts by mass of catalyst acetic acid is added dropwise for 45 minutes, and the temperature is maintained at about 80°C during the dropwise addition;

[0039] After the dropwise addition, add 5 parts by mass of toughening agent 208 hydroxy silicone oil, stir evenly, heat up to about 83°C, condense and reflux for 5.5 hours;

[0040] Reduce the pressure to -0.04MPa to slowly release the by-products until no by-products are released from the reaction system. Afterwards, the temperature was raised to 120° C. for polycondensation under reduced pressure and maintained for 25 minutes;

[0041] Add 0.15 parts by mass of neutralizing agent 1,3-dibutyl-1,1,3,3-tetramethylsilazane for neutralization;

[0042] Add ethanol to adjust the solid content of the resin to 58...

Embodiment 3

[0044] Add 95 parts by mass of methyltriethoxysiloxane and 5 parts by mass of dimethyldiethoxysiloxane into the reactor, raise the temperature to 70°C under stirring, and add 30 The mixture of parts by mass of water and 0.10 parts by mass of catalyst formic acid is added dropwise for 35 minutes, and the temperature is maintained at about 70° C. during the dropwise addition.

[0045] After the dropwise addition, 15 parts by mass of the toughening agent 208 hydroxy silicone oil was added, the temperature was raised to about 83° C. after stirring evenly, and condensed and refluxed for 4.5 hours. After the reflux is completed, the pressure is reduced to -0.05MPa, so that the by-products of the reaction are slowly released until no by-products are released from the reaction system;

[0046] Under reduced pressure, the temperature was raised to 110°C for polycondensation and maintained for 32 minutes;

[0047] Add 0.12 parts by mass of neutralizing agent hexamethylcyclotrisilazane ...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
impact strengthaaaaaaaaaa
gel timeaaaaaaaaaa
impact strengthaaaaaaaaaa
Login to View More

Abstract

The invention discloses a preparation method of toughened high temperature resistance silicone resin. The preparation method comprises the steps that the mixture of water and an acid catalyst is added into a siloxane monomer, and then hydrolysis is carried out; a toughening agent is added, and then condensation reflux reaction is carried out, wherein the toughening agent is 208 hydroxy silicone oil; a reaction by-product is removed through decompression until no by-product is removed from the reaction system; heating and polycondensation are carried out; a neutralizer is added for neutralization, wherein the neutralizer is one or more of hexamethyl disilazane, 1, 3-dibutyl-1, 1, 3, 3-tetramethyldisilazane and hexamethyl cyclotrisilazane; and ethanol is added to adjust the solid content of the resin weight, so as to acquire the toughened high temperature resistance silicone resin. According to the invention, chlorosilane and arene are not used in production; environmental production is realized; and the resin has a high impact resistance performance, and can be used as the base material of a high temperature resistance material, an electric insulating paint, a heat resistance coating, a weather resistance coating and the like.

Description

technical field [0001] The invention relates to a preparation method of silicone resin, more specifically to a preparation method of toughened high temperature resistant silicone resin. Background technique [0002] Silicone resin is an important part of silicone products. It is a cross-linked semi-inorganic polymer with silicon-oxygen-silicon as the main chain and organic groups connected to silicon atoms. Silicone resin is different from silicone oil and silicone rubber. It is a kind of highly branched polysiloxane system, which can be further solidified into an insoluble and infusible solid by heating. Silicone resin has the characteristics of both organic resin and inorganic material. It has excellent heat resistance, weather resistance, electrical insulation, water repellency and chemical resistance, and also has good processability and curing performance. It is a special polymer material that is different from general organic resins, and it is widely used in many indu...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/44C09D183/10
Inventor 吴蓁陈少彪何辛马东阳孙揭阳朱爱琴
Owner SHANGHAI RESIN FACTORY