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Preparation of methylvinylsilane resin

A technology of methyl vinyl silane and tetramethyl divinyl disiloxane, which is applied in the field of preparation of methyl vinyl silane resin, can solve the problems of low strength, difficult control of molecular weight, poor light transmittance, etc. The synthesis reaction process is simple, the product is widely used, and the production cost is low.

Inactive Publication Date: 2017-06-16
烟台鑫海耐磨胶业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the main methods of producing methyl vinyl MQ silicone resin are sodium silicate method and silicate method. Both methods have their own advantages and disadvantages. Control, the molecule contains a large number of unreacted Si-OH and Si-OR (R is Me, Et, etc.) groups, which are immiscible with the components of the LED packaging material, turbid, low vinyl content, etc.
The silicone encapsulant reinforced with the resin produced in this way has poor light transmittance, low strength, and great problems in storage life

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0007] Add 42g ethyl orthosilicate, 8g toluene, 9g hexamethyldisiloxane, 3g tetramethyldivinyldisiloxane, 15g absolute ethanol in a three-necked flask equipped with stirrer, thermometer, and condenser , 1.4g concentrated hydrochloric acid (wt%=36%); add 15g water dropwise at a rate of 1d / s in an ice-water bath, stir for 5min after dripping, heat up to 35°C for initial reaction for 30min; raise the temperature of the system to 78°C React for 4h, stop the reaction, add 1.43gNaHCO 3 , and heated to 125 ° C to distill water and ethanol. After steaming, reflux reaction at this temperature for 4 hours, then add 0.3 g of hexamethyldisiloxane to react at this temperature for 1 hour, and wash until PH=7. Filter to obtain a colorless and transparent filtrate, transfer the filtrate to a pear-shaped flask, and distill off low boiling substances such as xylene under reduced pressure to obtain methylvinylsilane resin.

Embodiment 2

[0009] Add 43g ethyl orthosilicate, 8g toluene, 9g hexamethyldisiloxane, 3g tetramethyldivinyldisiloxane, 20g absolute ethanol in a three-necked flask equipped with stirrer, thermometer, and condenser , 1.4g concentrated hydrochloric acid (wt%=36%); add 15g water dropwise at a rate of 1d / s in an ice-water bath, stir for 5min after dripping, heat up to 35°C for initial reaction for 40min; raise the temperature of the system to 78°C React for 4h, stop the reaction, add 1.43gNaHCO 3 , and heated to 125 ° C to distill water and ethanol. After steaming, reflux reaction at this temperature for 4 hours, then add 0.3 g of hexamethyldisiloxane to react at this temperature for 1 hour, and wash until PH=7. Filter to obtain a colorless and transparent filtrate, transfer the filtrate to a pear-shaped flask, and distill off low boiling substances such as xylene under reduced pressure to obtain methylvinylsilane resin.

Embodiment 3

[0011] Add 41g ethyl orthosilicate, 8g toluene, 9g hexamethyldisiloxane, 3g tetramethyldivinyldisiloxane, 10g absolute ethanol in a three-necked flask equipped with a stirrer, a thermometer, and a condenser , 1.4g concentrated hydrochloric acid (wt%=36%); add 15g water dropwise at a rate of 1d / s in an ice-water bath, stir for 5min after dripping, heat up to 35°C for initial reaction for 25min; raise the system temperature to 78°C React for 4h, stop the reaction, add 1.43gNaHCO 3 , and heated to 125 ° C to distill water and ethanol. After steaming, reflux reaction at this temperature for 4 hours, then add 0.3 g of hexamethyldisiloxane to react at this temperature for 1 hour, and wash until PH=7. Filter to obtain a colorless and transparent filtrate, transfer the filtrate to a pear-shaped flask, and distill off low boiling substances such as xylene under reduced pressure to obtain methylvinylsilane resin.

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Abstract

The invention relates to preparation of methylvinylsilane resin. The methylvinylsilane resin is prepared through the following steps: adding 41 to 43 g of ethyl orthosilicate, 8 g of toluene, 9 g of hexamethyldisiloxane, 3 g of tetramethyldivinyldisiloxane, 10 to 20 g of absolute ethyl alcohol and 1.4 g of concentrated hydrochloric acid (wherein wt% is 36%) into a three-neck flask equipped with a stirrer, a thermometer and a condenser tube; adding 15 g of water in an ice water bath drop by drop at a rate of 1 d / s, carrying out stirring for 5 min after addition, and then carrying out heating to 35 DEG C for a preliminary reaction for 25 to 40 min; allowing the temperature of a system to rise to 78 DEG C, carrying out a reaction for 4 h, then terminating the reaction, adding 1.43 g of NaHCO3 and carrying out heating to 125 DEG C to evaporate water and ethanol; after evaporation, carrying out a reflux reaction at 125 DEG C for 4 h, then adding 0.3 g of hexamethyldisiloxane, carrying out a reaction at 125 DEG C for 1 h, and then carrying out washing until a pH value is 7; and carrying out filtering so as to obtain a colorless transparent filtrate, transferring the filtrate to a pyriform flask, and carrying out pressure-reduced distillation to remove low-boiling-point substances like xylene so as to obtain the methylvinylsilane resin.

Description

technical field [0001] The invention relates to the preparation of a methyl vinyl silane resin, which belongs to the field of synthetic chemistry. Background technique [0002] Silicone LED packaging adhesive has excellent heat resistance, UV resistance, radiation resistance, high refractive index, high transparency and good mechanical properties, etc., and is very suitable for packaging LEDs, especially high-power LEDs. At present, the many characteristics of organic silicon LED packaging materials make them put forward higher requirements for their own reinforcing fillers. As a reinforcing filler for liquid silicone rubber used in high-power LED packaging materials—methyl vinyl MQ silicone resin is becoming more and more important. At present, the main methods of producing methyl vinyl MQ silicone resin are sodium silicate method and silicate method. Both methods have their own advantages and disadvantages. Control, the molecule contains a large number of unreacted Si-OH...

Claims

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Application Information

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IPC IPC(8): C08G77/20
CPCC08G77/20
Inventor 阎珊珊
Owner 烟台鑫海耐磨胶业有限公司
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