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Preparation method of high-temperature-resistant anti-cracking MDQ silicon resin

A non-cracking, silicone resin technology, applied in the field of silicone resin synthesis, can solve the problems of high temperature cracking viscosity of film

Inactive Publication Date: 2017-05-24
YANTAI DARBOND TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Aiming at the deficiency of the existing MQ silicone resin, the present invention provides a synthesis method of MDQ silicone resin which can greatly improve the high-temperature cracking problem of the film and reduce the viscosity of the resin

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Add 1.77g of concentrated hydrochloric acid, 15.13g of vinyl double caps, 67.70g of hexamethyldisiloxane MM, 60.11g of dimethyldiethoxysilane, 15.10g of ethanol and 3.00g of water into the four-necked bottle React for 1 hour at a rotation speed of 300 rpm and 25°C. After the reaction is completed, add 57.40 g of water and 208.33 g of tetraethyl orthosilicate dropwise at room temperature at the same time, and control the temperature in the system between 30°C. After the addition, react at 70°C for 2 hours, then distill the ethanol in the system at 80°C, then add 172.10g of toluene and an appropriate amount of NaOH to adjust the pH of the system to 9, react at 90°C for 1 hour, then raise the temperature to 120°C to evaporate the system The remaining ethanol and water in the system are finally cooled down, neutralized with acid, and washed with water until the pH of the system is 6-7; the toluene in the system is removed by rotary evaporation at 120°C to obtain methyl vinyl...

Embodiment 2

[0025] Add 1.17g of concentrated hydrochloric acid, 15.13g of vinyl double head, 67.70g of hexamethyldisiloxane MM, 60.11g of dimethyldimethoxysilane, 15.10g of methanol and 3.00g of water into the four-necked flask React for 1 hour at a rotation speed of 300 rpm and 25°C. After the reaction is completed, add 56.00g of water and 152.22g of methyl orthosilicate dropwise at room temperature at the same time, control the temperature in the system at 35°C, and complete the dropwise addition Then react at 70°C for 2 hours, then distill out the methanol in the system at 70°C, then add 163.61g of toluene and an appropriate amount of KOH to adjust the pH of the system to 9, react at 90°C for 1 hour, then raise the temperature to 120°C to evaporate the remaining methanol and water, and finally lower the temperature, add acid to neutralize, and wash with water until the pH of the system = 6-7; at 120 ° C, the toluene in the system is removed by rotary evaporation to obtain methyl vinyl M...

Embodiment 3

[0027] Add 1.50g of concentrated hydrochloric acid, 15.13g of vinyl double caps, 67.70g of hexamethyldisiloxane MM, 60.11g of dimethyldimethoxysilane, 15.10g of isopropanol and 3.00g of Water was reacted for 1 hour at a rotation speed of 300 rpm and 25°C. After the reaction was completed, 69.00 g of water and 152.22 g of isopropyl orthosilicate were added dropwise at room temperature at the same time, and the temperature in the system was controlled at 40°C. After the addition, react at 70°C for 2 hours, then distill off the isopropanol in the system at 90°C, then add 163.61g of toluene and an appropriate amount of Na 2 CO 3 Adjust the pH of the system to 9, react at 90°C for 1 hour, then raise the temperature to 120°C to evaporate the remaining isopropanol and water in the system, and finally lower the temperature, add acid to neutralize, and wash with water until the system pH=6-7; 120 The toluene in the system was removed by rotary evaporation at °C to obtain the methyl vi...

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PUM

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Abstract

The invention relates to a preparation method of high-temperature-resistant anti-cracking MDQ silicon resin. The method comprises the following steps of adding acid, divinyl tetramethyl disiloxane, hexamethyldisiloxane and dimethyl dialkoxy silane, alcohol and 2 to 5g of water into a four-opening bottle; performing stirring; heating the materials to 25 DEG C; performing reaction for 1 to 2 hours; after the reaction is completed, dripping the rest total amount of water and silicate ester at the same time at the room temperature; controlling the temperature in a system to be between 30 and 40 DEG C; after the dripping completion, performing reaction for 1 to 2 hours at 70 DEG C; then, distilling out alcohol in the system; then, adding methylbenzene and alkali with the same mass as the theoretical synthesis resin to regulate the system pH to be 9 to 10; performing reaction for 1 hour at 90 DEG C; then, raising the temperature to distill out the rest alcohol and water; finally, lowering the temperature; performing neutralization by acid; performing water washing until the system pH is 6 to 7; performing rotary evaporateion at 120 DEG C to remove methylbenzene so as to obtain the silicon resin. The DMQ silicon resin prepared by the method provided by the invention is mainly used for reinforcing agents of encapsulation glue, organic silicon additives and organic silicon mold plastics.

Description

technical field [0001] The invention relates to a preparation method of high-temperature resistant non-cracking methyl vinyl MDQ silicone resin, belonging to the technical field of silicone resin synthesis. Background technique [0002] Silicone resin, as an earlier product among silicone materials, has excellent dielectric constant, stable performance, excellent oxidation resistance, chemical resistance, electrical insulation, radiation resistance and weather resistance. Therefore, silicone resin can be used in electrical insulating varnishes, coatings, molding compounds, laminated materials, demoulding machines, etc., and has a wide range of uses in aerospace, electronic devices, construction, machinery, etc. [0003] In the existing technology, there are few reports about MDQ silicone resin, only the synthesis method of methyl vinyl MQ silicone resin. MQ resin has high rigidity, which easily leads to high-temperature cracking of the film in the formulation, obvious reinf...

Claims

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Application Information

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IPC IPC(8): C08G77/20
CPCC08G77/20
Inventor 秦余磊陈维
Owner YANTAI DARBOND TECH
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