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Addition type multi-component copolymerized phenyl silicone rubber and preparation method thereof

A technology for copolymerizing phenyl and silicone rubber, which is applied in the field of addition-type multi-component copolymerized phenyl silicone rubber and its preparation, can solve the problems of long reaction time, cumbersome operation process, cumbersome process, etc., and achieve the optimization of product post-treatment process, The effect of high conversion rate of raw materials and short reaction time

Inactive Publication Date: 2020-11-24
NANJING ADHESION TECH CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Liu Lihua and others used hexaethylcyclotrisiloxane and methylphenylsiloxane to copolymerize dimethyl-diethyl-methylphenyl copolymerized silicone rubber. The multi-component copolymerized silicone rubber is non-crystalline rubber. It has excellent low temperature resistance; Cui Yan and others synthesized dimethyl-diethyl-methylphenyl-methylethyl multi-component copolymerized silicone rubber, using KOH as the catalyst, although the yield is high, but the reaction time is relatively short Long, while using phosphoric acid as a neutralizing agent, the process is more cumbersome; Chinese patents CN111518132A, CN104004191A and CN109400880A use methyl phenyl mixed rings, and tetramethyl ammonium hydroxide as a catalyst to prepare phenyl silicone rubber, all through thermal vacuum The method of devolatilization is used to remove small molecules, and at the same time, the catalyst is decomposed and invalidated by heating at normal pressure. Addition-type phenyl silicone rubber is prepared from raw materials such as base dialkoxysilane, which is also used to remove low-boiling substances and promote catalyst decomposition and deactivation through high-temperature and reduced-pressure methods; Chinese patent CN109762092A synthesized a low-temperature-resistant fluorosilicone rubber , choose tert-butyl hydroperoxide or potassium persulfate as catalyst, but its yield is low, the highest is 34%
At present, the research and application of phenyl silicone rubber is still mainly concentrated on phenyl silicone rubber mainly composed of diphenyl chain members or methyl phenyl chain members. less, but it is undoubtedly an important way to invent new materials

Method used

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  • Addition type multi-component copolymerized phenyl silicone rubber and preparation method thereof
  • Addition type multi-component copolymerized phenyl silicone rubber and preparation method thereof
  • Addition type multi-component copolymerized phenyl silicone rubber and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Take the following components respectively in parts by weight (grams):

[0032] (1) Preparation for synthesis

[0033] Take 1.5 times the amount of the initiator required before the reaction, put it into a beaker, place it in a vacuum drying oven at 0.1Mpa, dry it at 40°C for 2 hours, and put it in a desiccator for later use. Clean the glass equipment and place it in a blast drying oven Store at 100°C, and return to room temperature naturally after 0.5h for later use.

[0034] (2) Synthesis process

[0035] In step (1) reactor, add 16 parts of octamethylcyclotetrasiloxanes (D 4 ), 16 parts of methylphenylcyclotetrasiloxane (D 4 ph ) and 8 parts of methyltrifluoropropylcyclotrisiloxane (D 3 F ), and then heated up to 42 ° C, while pumping vacuum while blowing N 2 Or while stirring, in order to improve the dehydration efficiency, the duration is 1.5h. Then in N 2 The catalyst tetramethylammonium hydroxide is added under the atmosphere, and the dosage is 0.1 parts...

Embodiment 2-4

[0039] The experimental procedure is the same as that of Example 1, and the addition-type multi-component copolymerized phenyl silicone rubbers of Examples 2-4 with different mass ratios were synthesized according to the formula in Table 1.

[0040] Table 1

[0041]

[0042] Structure Characterization

[0043] (1) 1 H-NMR characterization

[0044] Carry out proton nuclear magnetic resonance spectrum analysis (as figure 1 ), to get the following structure:

[0045]

[0046] In the formula, m is the number of dimethylsiloxane chains, n is the number of methylphenylsiloxane chains, and p is the number of methyltrifluoropropylsiloxane chains. Si-C at δ=7.32-7.52 6 h 5 The integrated area of ​​the peak is denoted as a, Si-CH at δ=2.01-2.22 2 CH 2 CF 3 The integrated area of ​​the peak is denoted as b, Si-CH at δ = 0-0.5 3 The integrated area of ​​the peak is denoted as c. Obtain following formula according to methylphenyl trifluoropropyl structural formula:

[004...

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PUM

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Abstract

The invention discloses addition type multi-component copolymerized phenyl silicone rubber and a preparation method thereof. The silicone rubber is of a structure with a side chain containing phenyl and trifluoropropyl. The synthetic method comprises the following steps: sequentially introducing octamethylcyclotetrasiloxane, methylphenyl cyclotetrasiloxane and methyltrifluoropropyl cyclotrisiloxane into a reactor according to a certain mass ratio, adding a catalyst and an end-capping reagent, continuously stirring the obtained mixture, heating to obtain a product, and performing polymerizationreaction at normal pressure; and removing low molecular weight impurities and an initiator by taking isopropanol or ethanol as a precipitator. The method disclosed by the invention has the advantagesof simple operating process, low reaction cost, short reaction time, high conversion rate, capability of removing impurities and catalysts by utilizing a precipitation method and the like.

Description

technical field [0001] The invention belongs to the technical field of silicone rubber synthesis, and in particular relates to an addition-type multi-component copolymerized phenyl silicone rubber and a preparation method thereof. Background technique [0002] Silicone rubber material is an emerging strong GDP industry that has risen rapidly with the development of social economy, science and technology. It has high and low temperature resistance, radiation resistance, ultraviolet resistance, weather resistance, electrical insulation, flame retardancy, high gas permeability, and chemical inertness. , physiological inertness and good biocompatibility. In recent years, it has been widely used in aerospace, national defense, electrical and electronic, petroleum, chemical, machinery and other fields, and plays an increasingly important role in the optimization and upgrading of high technology and industrial structure. The typical representative is methyl phenyl silicone rubber,...

Claims

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Application Information

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IPC IPC(8): C08G77/24C08G77/06C08G77/34
CPCC08G77/06C08G77/24C08G77/34C08G77/80
Inventor 姬科举戴振东吴文涛赵春霞乔元华甘培赟
Owner NANJING ADHESION TECH CO LTD
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