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Preparation method of in-situ hybrid reinforced butadiene-acrylonitrile-isoprene copolymer

A technology of isoprene and butadiene, which is applied in the field of synthetic rubber preparation, can solve the problems of complicated use of microcrystalline cellulose, and achieve the effects of good wet skid resistance, good processing performance and high tensile stress.

Active Publication Date: 2011-08-31
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This document applies modified microcrystalline cellulose in the processing process, and does not involve the modification and reinforcement of rubber in the polymerization process, which complicates the use of microcrystalline cellulose

Method used

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  • Preparation method of in-situ hybrid reinforced butadiene-acrylonitrile-isoprene copolymer
  • Preparation method of in-situ hybrid reinforced butadiene-acrylonitrile-isoprene copolymer
  • Preparation method of in-situ hybrid reinforced butadiene-acrylonitrile-isoprene copolymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Add 200 parts of water, 5 parts of fatty acid sodium, and 28 parts of isoprene into a 10L polymerization kettle, and pass nitrogen gas to test the pressure. After confirming that there is no leakage in the polymerization kettle, replace it with nitrogen several times, and then add 36 parts of butadiene and 36 parts of 1 part of acrylonitrile (I / B / A: 28 / 36 / 36), drop 1 part of compound reinforcing agent (the mass ratio of vinyltetraethoxysilane and microcrystalline cellulose is 4:6), start the polymerization kettle Stir for 10 minutes, and pour cold water into the polymerization kettle to cool down. When the temperature of the polymerization kettle drops to 10°C, add 0.3 parts of initiator persulfate and 0.5 parts of tertiary dodecyl mercaptan, and react at 20°C for 12 hours. The conversion rate was controlled at 75%, and 0.1 part of terminator diethylhydroxylamine was added. The rubber is condensed after being degassed, and the product of the present invention is obtaine...

Embodiment 2

[0039] The formulation and conditions of the polymerization system are the same as those in Example 1, except that the monomer ratio of isoprene, butadiene and acrylonitrile and the amount of molecular weight regulator mercaptan are different. The monomer ratio of this embodiment is 25 parts of isoprene, 50 parts of butadiene and 25 parts of acrylonitrile (I / B / A: 25 / 50 / 25), the molecular weight regulator tert-dodecyl mercaptan consumption is 0.38 part, and 0.6 part of compound reinforcing agent is added dropwise (vinyl four The mass ratio of ethoxysilane to microcrystalline cellulose is 4:6). The structure and properties of the samples were tested by classical methods. 1 H-NMR detection analysis showed that no acrylonitrile homopolymer block (block polyacrylonitrile) existed. The experimental results are shown in Table 2.

Embodiment 3

[0045] The formulation and conditions of the polymerization system are the same as those in Example 1, except that the ratio of isoprene, butadiene, and acrylonitrile monomers and the amount of molecular weight regulator mercaptan are different. The monomer ratio of this embodiment is 22 parts of isoprene, 52 parts of butadiene and 26 parts of acrylonitrile (I / B / A: 22 / 52 / 26), the molecular weight regulator tert-dodecyl mercaptan consumption is 0.30 part, and 1 part of compound reinforcing agent is added dropwise (vinyl four The mass ratio of ethoxysilane to microcrystalline cellulose is 5:5). The structure and properties of the samples were tested by classical methods. 1 H-NMR detection analysis showed that no acrylonitrile homopolymer block (block polyacrylonitrile) existed. The experimental results are shown in Table 3.

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Abstract

The invention provides an emulsion polymerization method for hybridizing and reinforcing a butadiene-acrylonitrile-isoprene copolymer in situ by using vinyl tetraethoxysilane and microcrystalline cellulose as a compounded reinforcing agent. The number average molecular weight of the prepared copolymer is 5*10<4> to 40*10<4>; the isoprene content is 10 to 60 percent; the butadiene content is 10 to 80 percent; the acrylonitrile content is 15 to 55 percent; and in the copolymer, the 1,4-polyisoprene content is 60 to 95 percent, the 3,4-polyisoprene content is 5 to 30 percent, the 1,4-polybutadiene content is 60 to 90 percent and the 1,2-polybutadiene content is 10 to 40 percent. The copolymer has the characteristics of excellent mechanical property and simpleness in process, meets the high-performance requirement of nitrile rubber and enlarges the application range.

Description

technical field [0001] The invention relates to a method for preparing synthetic rubber, in particular to a method for preparing a compound reinforcing agent in-situ hybrid reinforced butadiene-acrylonitrile-isoprene copolymer. Background technique [0002] When the acrylonitrile content of nitrile rubber increases, its oil resistance increases, wear resistance improves, heat aging resistance becomes better, modulus stress, tensile strength and hardness increase, but resilience decreases, cold resistance and The low temperature resistance and air permeability are reduced, which limits the application fields of nitrile rubber. [0003] CN03805768.9 relates to a wear-resistant elastomer composition, a terpolymer of derived units and p-bromomethylstyrene derived units, at least one filler suitable for wear-resistant articles comprising 5-10 phr C 4 -C 7 Isoolefin derived units. CN200410066552.9 relates to the preparation of polyisoprene copolymer emulsion and its green glov...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F236/12C08F236/06C08F236/08C08F2/44
Inventor 梁滔魏绪玲艾纯金钟启林曹凤霞郑聚成龚光碧桂强丛日新郑红兵朱晶翟云芳
Owner PETROCHINA CO LTD
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