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A kind of synthetic method of methyl vinyl mq silicone resin

A technology of MQ silicone resin and methyl vinyl, applied in the field of methyl vinyl MQ silicone resin synthesis, it can solve the problems of low strength, low vinyl content, immiscibility, etc., and achieve high light transmittance, high hardness, high The effect of tensile strength

Inactive Publication Date: 2015-09-02
YANTAI DARBOND TECH
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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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  • A kind of synthetic method of methyl vinyl mq silicone resin
  • A kind of synthetic method of methyl vinyl mq silicone resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] In a three-necked flask equipped with a stirrer, a thermometer and a condenser, add 41.75g ​​of ethyl orthosilicate, 8.00g of xylene, 10.48g of hexamethyldisiloxane, and 3.5g of tetramethyldivinyldisiloxane. , 2.51g of absolute ethanol, 1.42g of concentrated hydrochloric acid (wt%=36%), and add 15.15g of water dropwise at a rate of 1d / s in an ice-water bath, stir for 5min after dripping, heat up to 35℃, and initially react for 25min . The temperature of the system was raised to 78°C, and the reaction was refluxed for 4h. Stop stirring and add 1.45g NaHCO 3 Turn on stirring and heat up to 125°C to distill out water and ethanol. After steaming, reflux and react at this temperature for 4h, then add 0.2g of hexamethyldisilazane and stir for 1h at 125°C. Turn off the heating and stirring system. The liquid in the bottle is transferred to a separatory funnel and washed with distilled water until PH=7. A colorless and transparent filtrate was obtained by filtration, and the f...

Embodiment 2

[0027] Add 41.75g ​​of ethyl orthosilicate, 8.10g of xylene, 9.07g of hexamethyldisiloxane, and 3.09g of tetramethyldivinyldisiloxane into a three-necked flask equipped with a stirrer, thermometer and condenser. , 2.65g absolute ethanol, 1.40g concentrated hydrochloric acid (wt%=36%). And add 15.20g of water dropwise at a rate of 1d / s in an ice water bath, and stir for 5min after the drop. The temperature was raised to 35°C for a preliminary reaction for 25 minutes. The temperature of the system was raised to 78°C for 4h. Stop the reaction and add 1.43g NaHCO 3 , And heat up to 125 ℃ to steam out water and ethanol. After the evaporation, the reaction was refluxed at this temperature for 4h, then 0.3g of hexamethyldisiloxane was added and reacted at this temperature for 1h, and washed until the PH=7. A colorless and transparent filtrate was obtained by filtration, and the filtrate was transferred to a pear-shaped flask, and low-boiling substances such as xylene were distilled...

Embodiment 3

[0029] Add 39.45g ethyl orthosilicate, 8.25g xylene, 10.36g hexamethyldisiloxane, and 3.53g tetramethyldivinyldisiloxane into a three-necked flask equipped with a stirrer, thermometer and condenser. , 2.40g absolute ethanol, 1.43g concentrated hydrochloric acid (wt%=36%). 14.32g of water was added dropwise in an ice water bath at a rate of 1d / s, and stirred for 5 minutes after the dropping. The temperature was raised to 35°C for a preliminary reaction for 25 minutes. The temperature of the system was increased to 78°C for 4.5 hours. Stop the reaction and add 1.40gNaHCO 3 The temperature is increased to 125°C to distill out water and ethanol. After the evaporation, the reaction was refluxed and stirred at this temperature for 4 hours, and then 0.2g of hexamethyldisiloxane was added to react at this temperature for 1 hour, and washed until PH=7. A colorless and transparent filtrate was obtained by filtration. The filtrate was transferred to a pear-shaped flask, and low-boiling...

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PUM

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Abstract

The invention relates to a synthetic method of methyl vinyl MQ silicon resin. The methyl vinyl MQ silicon resin prepared by the synthetic method disclosed by the invention is white solid powder, and clear and transparent while being mutually mixed with vinyl silicon oil in an LED (Light-Emitting Diode) encapsulating material, does not contain Si-OH and Si-OR (R is Me, Et, and the like), and can be mixed with each component of the LED encapsulating material without turbidity. Vinyl content is 3wt%-5wt%, M / Q is equal to 0.6-0.9, and therefore, the methyl vinyl MQ silicon resin is very suitable for being used as an LED encapsulating reinforcing agent and capable of satisfying requirements of high light transmittance, high tensile strength and high hardness of the LED encapsulating material.

Description

Technical field [0001] The invention relates to a method for synthesizing methyl vinyl MQ silicone resin. Background technique [0002] With the development of the global low-carbon economy, LED has become one of the most promising high-tech industries in the world in recent years due to its technical advantages such as energy saving, environmental protection, longevity, and controllability. As a new generation of lighting and display devices The light source represents that LED will replace traditional light sources on a large scale in the next few years. The solution of power LED packaging technology and the preparation of packaging materials is one of the key technologies for LED industrialization. Therefore, the production of LED packaging materials with high light transmittance and high intensity has attracted more and more attention. [0003] Silicone LED encapsulant has excellent heat resistance, UV resistance, radiation resistance, refractive index, high transparency, and ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/20C08G77/08C08L83/07
Inventor 陈维张燕王建斌陈田安
Owner YANTAI DARBOND TECH
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