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Method for preparing unsaturated and conjugated diolefin-nitrile copolymer

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

Active Publication Date: 2009-09-16
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 added amount of each monomer adjuvant is based on 100 parts of total monomer weight (the same below). At the beginning of the polymerization reaction, add 300 parts of desalinated water, 2.0 parts of sodium dodecylbenzene sulfonate soap, 0.005 parts of white block, 0.001 parts of EDTA-Fe, 0.001 parts of EDTA-4Na salt, and 30 parts of monomer acrylonitrile. Add 0.2 parts of t-dodecyl mercaptan and 0.3 parts of 2-mercaptobenzothiazole to the polymerization kettle. After vacuuming, replace with nitrogen three times, then add 70 parts of monomer butadiene and 0.03 parts of sodium dithionite as the deoxidizer, When the temperature of the polymerization kettle reaches 12°C, add 0.06 parts of initiator dicumyl peroxide 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 hour to cool down and discharge....

Embodiment 2

[0030]The polymerization reaction was carried out in a 30L autoclave. At the beginning of the polymerization reaction, add 300 parts of desalinated water, 3.0 parts of sodium dodecylbenzene sulfonate soap, 0.005 parts of white block, 0.001 parts of EDTA-Fe, 0.001 parts 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 vessel, after vacuuming, replaced with nitrogen three times, and then added 72 parts Monomer butadiene, 0.03 parts of oxygen scavenger sodium hydrosulfite, when the temperature of the polymerization kettle reaches 12 ℃, add 0.08 parts of initiator dicumyl peroxide, start the polymerization reaction, and measure every 4 hours during the polymerization process For the primary dry matter, when the polymerization conversion rate reaches 30%, add the molecular weight regulator 0.05 parts 1,1,3,3-tetramethyl-1-butanethiol and 0.15 parts 2-merca...

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 monomer acrylonitrile, 0.4 parts of t-dodecyl mercaptan and 0.25 parts of tert-butyl-2-benzo Thiazole sulfenamide was added to the polymerization vessel, after vacuuming, replaced with nitrogen three times, and then 68 parts of monomer 1,3 pentadiene and 0.05 parts of sodium dithionite were added. When the temperature of the polymerization vessel reached 30°C, Add 0.05 parts of the initiator potassium persulfate solution to start the polymerization reaction. During the polymerization process, the dry matter is measured every 4 hours. When the polymerization conversion rate reaches 55%, add the molecular weight regulator 0.05 parts t-dodecyl mercaptan and 0.2 parts t-butyl-2-benzothiazole sulfenamide. Continue the reaction until the final conversion rate rea...

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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 method for preparing 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 nitrile rubber has excellent oil resistance and heat resistance. Recently, its application range has become wider and wider, including insulating rubber, electrical, automotive, industrial casting and shoe soles. In order to facilitate injection molding of nitrile rubber, nitrile rubber is required to have good fluidity and cross-linking effect, that is, to have a faster vulcanization speed under high temperature and short vulcanization time. In order to prepare a fast-vulcanizing nitrile rubber, many suggestions have been proposed, including the introduction of a carboxyl and amine functio...

Claims

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Application Information

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Patent Type & Authority Applications(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
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