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Hydrogen-containing MQ silicon resin and preparation method thereof

A technology of MQ silicone resin and tetraethyl orthosilicate, which is applied in the field of hydrogen-containing MQ silicone resin and its preparation, can solve the problems of complex methods, long time, low temperature, etc., and achieve the advantages of easy-to-obtain raw materials, convenient operation and short time Effect

Inactive Publication Date: 2015-02-25
深圳市红叶杰科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] Obviously, the above method is complex, cumbersome, takes a long time, and the temperature is low, and it even needs to be operated at 0-20°C, which brings difficulties to industrial production.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Add 100g of MMH (hydrogen-containing double head), 180g of MM (hexamethyldisiloxane), 110g of water, 50g of methanol, and 70g of hydrochloric acid into a 3000mL flask, stir well, and put it at room temperature (water bath 15~35℃) Under strong stirring, drop 500g of tetraethyl orthosilicate into the flask within 5 minutes through a constant pressure funnel, react (hydrolysis, condensation) for 2.5 hours, and then add AR grade NaHCO 3 Neutralize until the pH is 7-8, add 500ml of toluene to extract for 0.5h, then move the solution into a separatory funnel to separate layers, discard the water layer, add the toluene layer (oil layer) into the flask, and heat up the pressure in a thermostatic jacket heater. The hydrogen content is 0.19%, and the liquid hydrogen-containing MQ silicone resin can be completely dissolved in toluene according to the ratio (mass ratio) of 1:1.

Embodiment 2

[0040] Add 80g of MMH (hydrogen-containing double head), 180g of MM (hexamethyldisiloxane), 110g of water, 50g of methanol, and 70g of hydrochloric acid into a 3000mL flask, stir well, and put it at room temperature (water bath 15~35℃) Under strong stirring, drop 500 g of tetraethyl orthosilicate into the flask within 3 minutes through a constant pressure funnel, react (hydrolyze, condense) for 2 to 3 hours, and then add AR grade NaHCO 3 Neutralize until the pH is 7-8, add 500ml of toluene to extract for 0.5h, then move the solution into a separatory funnel to separate layers, discard the water layer, add the toluene layer (oil layer) into the flask, and heat up the pressure in a thermostatic jacket heater. The hydrogen content is 0.16%, and the white powder hydrogen-containing MQ silicone resin can be completely dissolved in toluene according to the ratio (mass ratio) of 1:1.

Embodiment 3

[0042] Add 100g of MMH (hydrogen-containing double-capped head), 70g of MM (hexamethyldisiloxane), 120g of water, 50g of methanol, and 70g of hydrochloric acid into a 3000mL flask, stir well, and put it at room temperature (water bath 15~35℃) Under strong stirring, drop 500 g of tetraethyl orthosilicate into the flask within 3 minutes through a constant pressure funnel, react (hydrolyze, condense) for 2 to 3 hours, and then add AR grade NaHCO 3 Neutralize until the pH is 7-8, add 500ml of toluene to extract for 0.5h, then move the solution into a separatory funnel to separate layers, discard the water layer, add the toluene layer (oil layer) into the flask, and heat up the pressure in a thermostatic jacket heater. The hydrogen-containing MQ silicone resin with a hydrogen content of 0.18% and completely soluble in toluene at a ratio (mass ratio) of 1:1 is obtained.

[0043] Mix 0.5g of 0.13% low-hydrogen-containing silicone oil, 0.5g of hydrogen-containing MQ silicone resin and...

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Abstract

The invention provides a hydrogen-containing MQ silicon resin with a general formula of [(CH3)2HSiO1 / 2]a[(CH3)3SiO1 / 2]b[SiO2]c, wherein M / Q is 0.6-0.9. The invention also provides a preparation method of the hydrogen-containing MQ silicon resin, comprising the following steps: uniformly mixing and stirring a monofunctional monomer, a catalyst, water and a cosolvent, wherein the monofunctional monomer comprises tetramethyldisiloxane and hexamethyldisiloxane, and the catalyst is acid; adding tetraethoxysilane at room temperature in five minutes with vigorous stirring, and reacting for 1-3 hours; and then neutralizing with an alkali, extracting with an extracting agent for layering, and performing reduced pressure dehydration on an extract to obtain the hydrogen-containing MQ silicon resin. By adopting the preparation method disclosed by the invention, the hydrogen-containing MQ resin is prepared by using a tetraethoxysilane method, various powdery and fluidic MQ resins and an MQ resin with different H contents can be prepared by adjusting M / Q, and the hydrogen-containing MQ silicon resin is mainly used for crosslinking agents and reinforcing agents containing molding rubber, can achieve a satisfactory effect, and has the advantages of convenience in operation, readily available raw materials, easy control, short time and the like.

Description

technical field [0001] The invention belongs to the field of polymer materials, and in particular relates to a hydrogen-containing MQ silicone resin and a preparation method thereof. Background technique [0002] Silicone resins are thermosetting polyorganosiloxane systems (prepolymers) with a highly crosslinked structure. Its preparation method usually uses organic silicon as raw material, and through hydrolysis, condensation, and rearrangement, it can produce resins with active genes directly linked to silicon atoms, such as hydroxyl, hydrogen atom, alkoxy, vinyl, phenyl, etc. , for stable storage and convenient application, most products are sold as varnishes dissolved in inert organic solvents such as toluene or xylene. [0003] Silicone resin has excellent various properties, such as heat resistance, weather resistance, electrical insulation, chemical resistance, hydrophobicity, adhesiveness and flame retardancy, etc. In addition, other resins can also be obtained thr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/12C08G77/08
Inventor 李贵宾
Owner 深圳市红叶杰科技有限公司
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