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Claw-type polyvinyl silicone oil and preparation method thereof

A technology of polyvinyl silicone oil and hexavinyldisiloxane, which is applied in the field of claw-type polyvinyl silicone oil and its preparation, can solve the problems of difficult removal, scene applications with limited insulation performance requirements, and high residual potassium ions. , to achieve the effect of reducing adhesion, improving material utilization efficiency and good appearance transparency

Active Publication Date: 2021-11-09
HUBEI XINGRUI SILICON MATERIAL CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main chain of the product obtained here is polysiloxane, the terminal is a methyl group or a single vinyl group, and the residual potassium ion is high and difficult to remove, which limits its application in scenarios where insulation performance is required

Method used

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  • Claw-type polyvinyl silicone oil and preparation method thereof
  • Claw-type polyvinyl silicone oil and preparation method thereof
  • Claw-type polyvinyl silicone oil and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] 100kg of dimethylsiloxane cyclic body (DMC) is filtered through a first-stage bag filter and a first-stage membrane filter, then enters a glass fiber reinforced plastic dehydration kettle, heats up to 70°C, vacuumizes at a pressure of 100Pa, and dehydrates for 4 hours to obtain a purity of 99.9995%. , DMC-1 with a water content of 15ppm, spare.

[0028] 10kg of hexavinyldisiloxane (HVDS) was filtered by a primary bag filter and a primary membrane filter respectively, and then entered into a packed tower equipped with molecular sieves for 18 hours to obtain HVDS with a purity of 99.92% and a water content of 12 ppm- 1, spare.

[0029] Catalyst: polystyrene cation exchange resin loaded with acid sites, acid site concentration 5.1 mmol / g, effective particle size 0.50-1.00 mm, uniformity coefficient ≤ 0.50, water content ≤ 0.15%.

[0030] Add 1950g of DMC-1 and 50g of HVDS-1 into the FRP stirred tank, raise the temperature to 70±2°C, and stir at a low speed for 1h to obtai...

Embodiment 2

[0032] Except that the residence time in the fluidized bed was controlled for about 4 hours, other processes and steps were the same as in Example 1 to obtain crude polymer C2 and finished product D2 respectively. Crude polymer C2 has a viscosity of 185cP and a conversion rate of 89.1%. Finished product D2, in the molecular formula, m=140-190, n=0, colorless and transparent appearance, 0.80% volatile matter, viscosity 304cP, relative value of silanol 1.028.

Embodiment 3

[0034] Except that the constant temperature in the stirred tank was 40±2°C and the constant temperature in the fluidized bed was 35±2°C, other processes and steps were the same as in Example 1 to obtain crude polymer C3 and finished product D3 respectively. Crude polymer C3 has a viscosity of 125cP and a conversion rate of 84.1%. The finished product D3 has a molecular formula of m=800-135, n=0, colorless and transparent appearance, a volatile content of 0.78%, a viscosity of 190cP, and a relative value of silanol of 1.020.

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Abstract

The invention relates to claw-type polyvinyl silicone oil and a preparation method thereof. The preparation method comprises the following steps that raw materials such as dimethyl siloxane cyclics, methylvinyl siloxane cyclics and hexavinyl disiloxane are subjected to water removal and impurity removal pretreatment, the pretreated materials are added into a stirring kettle in proportion at a constant temperature T of 30-70 DEG C, the pretreated materials are pumped into a fluidized bed through a conveying pump to undergo a reaction at a low temperature to obtain a crude polymer, the crude polymer enters a low-temperature removal system with a pressure of smaller than 50 Pa and a temperature of 100-150 DEG C, and light components are removed so as to obtain the claw-type polyvinyl silicone oil which is free of peculiar smell, good in appearance transparency and low in silicon hydroxyl value. According to the claw-type polyvinyl silicone oil prepared by adopting a low-temperature solid catalyst, the use efficiency of hexavinyl disiloxane is improved, cost is reduced, metal ions are not additionally introduced, the variety of vinyl silicone oil is enriched, and application performance indexes such as a linear expansion coefficient and a size change rate of materials such as silica gel can be greatly enhanced.

Description

technical field [0001] The invention relates to a claw-type polyvinyl silicone oil and a preparation method thereof. Background technique [0002] Vinyl silicone oil is the main raw material of addition-type silicone rubber, a reinforcing agent for high-temperature rubber, and a modifier for other materials such as polyurethane and acrylate, and has a wide range of applications. Polyvinyl silicone oil, generally a kind of polysiloxane with siloxane chain as the main chain, side chain or terminal containing vinyl groups and high vinyl content, mainly to increase crosslinking density and hardness , tear strength and other properties. [0003] Chinese patent document CN105482121A (application number: CN201511008606.0) discloses a method for synthesizing polyvinyl silicone oil, including: a mixture of dimethylcyclosiloxane DMC and tetramethyldivinyldisiloxane in alkaline A polymerization reaction occurs under the action of a catalyst. After the reaction is over, the temperatur...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/20C08G77/06C08G77/08
CPCC08G77/20C08G77/06C08G77/08
Inventor 李书兵徐小刚孙刚王龙文李磊段贤桂
Owner HUBEI XINGRUI SILICON MATERIAL CO LTD