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Method for preparing unsaturated and conjugated diolefin-nitrile copolymer

A technology of conjugated diene nitrile copolymer and conjugated diene, which is applied in the field of preparation of unsaturated conjugated diene nitrile copolymer, can solve the problems of long vulcanization time of rubber and achieve good processing performance and fast vulcanization speed Effect

Active Publication Date: 2011-04-20
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This does solve the problem of long rubber vulcanization time to a certain extent, but from the perspective of the long-term development of the rubber industry, it has certain limitations

Method used

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  • Method for preparing unsaturated and conjugated diolefin-nitrile copolymer
  • Method for preparing unsaturated and conjugated diolefin-nitrile copolymer
  • Method for preparing unsaturated and conjugated diolefin-nitrile copolymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] The polymerization reaction was carried out in a 30L autoclave. The addition amount of each monomer additive is calculated per 100 parts of total monomer weight (the same below). At the beginning of the polymerization reaction, add 300 parts of desalted water, 2.0 parts of sodium dodecylbenzenesulfonate soap, 0.005 parts of Diaobai block, 0.001 part of EDTA-Fe, 0.001 part of EDTA-4Na salt, and 30 parts of monomeric acrylonitrile and 0.2 parts of tertiary dodecyl mercaptan and 0.3 parts of 2-mercaptobenzothiazole into the polymerization kettle, after vacuuming, replace with nitrogen three times, then add 70 parts of monomer butadiene, 0.03 parts of oxygen scavenger sodium dithionite, When the temperature of the polymerization tank reached 12°C, 0.06 parts of dicumyl hydroperoxide as an initiator was added to start the polymerization reaction. When the polymerization conversion rate finally reaches 90%, add 0.2 part of terminator hydroxylamine sulfate, stir for half an h...

Embodiment 2

[0030]The polymerization reaction was carried out in a 30L autoclave. At the beginning of the polymerization reaction, add 300 parts of desalted water, 3.0 parts of sodium dodecylbenzenesulfonate soap, 0.005 parts of Diaobai block, 0.001 part of EDTA-Fe, 0.001 part of EDTA-4Na salt, 28 parts of monomer methyl Acrylonitrile, 0.4 parts of 1,1,3,3-tetramethyl-1-butanethiol and 0.2 parts of 2-mercaptobenzothiazole were added to the polymerization kettle, after vacuuming, replaced with nitrogen three times, and then added 72 parts Monomer butadiene, 0.03 parts of oxygen scavenger sodium dithionite, when the temperature of the polymerization kettle reaches 12°C, add 0.08 parts of initiator dicumyl hydroperoxide to start the polymerization reaction, and measure the temperature every 4 hours during the polymerization process. Once the dry matter, when the polymerization conversion rate reaches 30%, add 0.05 part of molecular weight regulator 1,1,3,3-tetramethyl-1-butanethiol and 0.15 ...

Embodiment 3

[0032] The polymerization reaction was carried out in a 30L autoclave. At the beginning of the polymerization reaction, 500 parts of desalted water, 3.0 parts of potassium oleate soap, 0.03 parts of triethanolamine, 32 parts of monomeric acrylonitrile, 0.4 parts of tertiary dodecyl mercaptan and 0.25 parts of tert-butyl-2-benzo Add thiazole sulfenamide into the polymerization kettle, after vacuuming, replace with nitrogen three times, then add 68 parts of monomer 1,3 pentadiene, 0.05 parts of oxygen scavenger sodium dithionite, when the temperature of the polymerization kettle reaches 30°C, Add 0.05 parts of initiator potassium persulfate solution to start the polymerization reaction. Measure the dry matter every 4 hours during the polymerization process. When the polymerization conversion rate reaches 55%, add 0.05 part of tert-dodecyl mercaptan and 0.2 part of tert-butyl-2-benzothiazole sulfenamide, Continue the reaction until the conversion rate finally reaches 90%, add 0....

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Abstract

The invention discloses a method for preparing unsaturated and conjugated diolefin-nitrile copolymer, which is characterized in that: a polymerization reaction is carried out in a pressure-resistant kettle with a mixer; total monomer weight is measured as 100 portions by weight; 100 portions to 800 portions of desalted water, 1.0 portion to 10 portions of emulsifier, 0 portion to 1 portion of activating agent, 15 portions to 45 portions of unsaturated nitrile monomers, molecular weight regulators, and 85 portions to 55 portions of conjugated diene monomers are added into the pressure-resistant kettle; after the reaction temperature is controlled to be 5 DEG C to 45 DEG C, 0.01 portion to 2 portions of triggering agent is added and the polymerization reaction starts; and when the conversion rate of the polymerization reaction reaches 88 percent to 92 percent, a termination agent is added and the unsaturated and conjugated diolefin-nitrile copolymer is obtained. The molecular weight regulators are compound regulators, wherein one of the molecular weight regulators is alkyl sulfhydrate with 4 to 16 carbon atoms and another molecular weight regulator is an organic substance with a thiazole structure. The Mooney viscosity of the unsaturated and conjugated diolefin-nitrile copolymer is 30 to 120 and the prepared unsaturated and conjugated diolefin-nitrile copolymer has excellent processing properties and high curing rate.

Description

technical field [0001] The invention relates to a preparation method of an unsaturated conjugated diene nitrile copolymer, in particular, the unsaturated conjugated diene nitrile copolymer has the characteristics of excellent mechanical properties and fast vulcanization speed. technical background [0002] In recent years, nitrile rubber has been widely used in injection molding, mainly because of its excellent oil resistance and heat resistance. Recently it has been used in a wide range of applications including insulating rubber, electrical, automotive, industrial molding and shoe soles. In order to make nitrile rubber easy for injection molding, it is necessary for nitrile rubber to have good fluidity and crosslinking effect, that is, to have a faster vulcanization speed at high temperature and shorter vulcanization time. In order to obtain a fast-vulcanizing nitrile rubber, many proposals have been proposed, including the introduction of a carboxyl and amine functional ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F220/44C08F236/12C08F4/28C08F4/04C08F2/38C08K5/47
Inventor 张志强于奎李锦山李晶周雷桂强钟启林
Owner PETROCHINA CO LTD