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Narrow molecular weight distribution butyl rubber synthesis method

A narrow molecular weight distribution, butyl rubber technology, used in the field of synthetic butyl rubber, can solve the problems of low rubber vulcanization performance and low number-average absolute molecular weight of butyl rubber.

Active Publication Date: 2016-07-06
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0016] The shortcomings of the above patents are that the vulcanization performance of the rubber is not high, and the number average absolute molecular weight of the obtained butyl rubber is relatively low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0062] Under the protection of high-purity nitrogen, first remove the moisture in the monomer to below 10ppm, and then remove the R 1 -Al-Cl 2 , R 2 -Al-Cl 1 Mix with vanadyl trichloride in a certain molar ratio (1:1:0.5), then add a small amount of water according to the total number of moles of the catalyst (m catalyst: m water = 2:3), and then add 5% (calculated as aluminum, mole ratio) N-dimethylnitrosamine and 5% (in terms of aluminum, molar ratio) benzo(b)pyrene, prepared as a mixed initiator, mixed and aged for 5 minutes to 400 hours to form a concentration of 0.08 The complex catalyst of M (calculated as aluminum) is ready for use. After cooling 300ml of isobutylene and isoprene monomer to -70°C, mix it with 500ml of solvent (containing 35% (v) ethyl chloride), and then add 60ml The complex catalyst (concentration: 0.08M) aged for 30 minutes was reacted for 30 minutes, and 60ml of methanol was added to precipitate butyl rubber. Wash with 2% (m) NaOH aqueous solutio...

Embodiment 2

[0064] Under the protection of high-purity nitrogen, first remove the moisture in the monomer to below 10ppm, and then remove the R 1 -Al-Cl 2 , R 2 -Al-Cl 1 Mix according to a certain ratio (1:1), then add a small amount of water according to the total number of moles of the catalyst (m catalyst: m water = 2:3), mix well and age for 5 minutes to 400 hours to make a concentration of 0.08M ( The complex catalyst (calculated as aluminum) is ready for use. After 300ml of isobutylene and isoprene monomers are lowered to -60°C, they are evenly mixed with 500ml of solvent (containing 35% (v) of methyl chloride), and then added to 60ml for aging for 30 Minute complex catalyst (concentration is 0.08M), after reacting for 60 minutes, add 60ml methanol to terminate the reaction. Wash with 2% NaOH aqueous solution until alkaline, and then wash with distilled water until neutral. After drying in a vacuum oven at 60°C for 8 hours, the absolute molecular weight of butyl rubber was detec...

Embodiment 3

[0066] Under the protection of high-purity nitrogen, first remove the moisture in the monomer to below 10ppm, and then remove the R 1 -Al-Cl 2 , R 2 -Al-Cl 1 Mix with vanadyl trichloride in a certain molar ratio (2:1:0.2), then add a small amount of water according to the total number of moles of the catalyst (m catalyst: m water = 4:1), and then add 5% (calculated as aluminum, mole ratio) N-dimethylnitrosamine and 5% (in terms of aluminum, molar ratio) benzo(b)pyrene, prepared as a mixed initiator, mixed and aged for 5 minutes to 400 hours to form a concentration of 0.08 The complex catalyst of M (calculated as aluminum) is ready for use. After cooling 300ml of isobutylene and isoprene monomer to -80°C, mix it with 500ml of solvent (containing 40% (v) of methyl chloride), and then add 65ml of The complex catalyst (concentration is 0.08M) was melted for 15 minutes, and after 40 minutes of reaction, 60ml of methanol was added to precipitate butyl rubber. Wash with 2% (m) Na...

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Abstract

The invention belongs to the technical field of rubber synthesis, and is a method for synthesizing butyl rubber with a narrow molecular weight distribution. The solvent used in the method is a solvent formed by mixing halogenated alkanes and saturated alkanes with carbon four to ten carbons, wherein the volume ratio of the content of halogenated alkanes is 1 %~55%; the composition of the main catalyst used is R-Al-Cl 2 :R 2 -Al-Cl 1 : vanadyl trihalide, add a certain proportion of water in the catalyzer; Add benzopyrene and / or nitrosamine compound again in the prepared main catalyst, form co-initiator; Main initiator is R-Al-Cl 2 and R 2 -Al-Cl 1 . The advantages of the present invention: the catalytic system is a homogeneous system, which is convenient for feeding; by adding a small amount of water, a stable complex initiation system is formed; the method can solve the problem that the molecular weight of butyl rubber decreases with the increase of temperature, and the obtained butyl The number average absolute molecular weight of the rubber is 2,000 to 550,000, and the molecular weight distribution is between 1.1 and 2.0.

Description

technical field [0001] The invention relates to a new technology for synthesizing butyl rubber, in particular to a method for synthesizing butyl rubber with isobutylene and isoprene as monomers by a solution method, and controlling the molecular weight and distribution by changing the composition and proportion of the catalyst . Background technique [0002] Butyl rubber is a product obtained by cationic copolymerization of isobutylene (94.5% to 98.5%) and a small amount of isoprene (4.5% to 1.5%). Due to its structural characteristics, it has excellent air tightness, such as About 9 times higher for air. Butyl rubber has been put into production since 1943 and is still an irreplaceable rubber for synthetic tire inner tubes or using it as the inner sealing coating of the outer tire, so that the inner and outer tires are combined into one tubeless tire. It has excellent heat aging resistance, ozone resistance and chemical stability. In addition, it also has unique damping p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F210/12C08F4/685C08F2/06
Inventor 潘广勤王福善张耀亨刘秀兰焦宏宇胡开放刘志琴王兴刚彭仁苹王春磊徐海燕何春武冠英徐惠俭李彤霞崔嘉敏张新
Owner PETROCHINA CO LTD
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