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A kind of carbon nanotube modified isobutylene and alkylstyrene polymer and preparation method thereof

A carbon nanotube modification, alkyl styrene technology, applied in the field of isobutylene and alkyl styrene polymers and their preparation, can solve the problems of polymerization reaction control limitations, achieve stable reaction, improve mechanical properties, and be widely used Effect

Active Publication Date: 2020-10-13
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

CN1253141A of Bayer Company proposes a method for preparing a butyl rubber polymer with a molecular weight of at least 400,000, so that the C4~C14 polyolefin monomer is in the temperature range of about -100°C~+50°C, in the aliphatic diluent and Contacting is carried out first in the presence of a catalyst mixture containing a major amount of dialkylaluminum halide, with the disadvantage of limited control of the polymerization reaction

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] (1) Dissolve 10g o-methylstyrene monomer in 10g ionic liquid 1-butyl-3-methylimidazole bis(trifluoromethanesulfonyl)imide salt; (2) Preparation of initiator complex : In an anhydrous and oxygen-free glove box, at a temperature of -40°C, add 4g of crown ether and 1g of isobutylaluminum dichloride (i-BuAlCl 2 ) complexed with crown ether, and shaken for 8 minutes; in another flask, 1g of main initiator tert-butyl chloride (t-BuCl) was added; then the i-BuAlCl complexed with crown ether was 2 Add the co-initiator to the main initiator, shake well and age for 10 minutes; (3) Under normal pressure, replace the polymerization kettle with nitrogen three times, then cool down to -30°C, add 500g of solvent methyl chloride, and the dispersed 5g of carbon Hexane 100ml of nanotube amount, add 200g isobutylene, step (1) gained o-methylstyrene ionic liquid solution again, add hexahydropyridine 1g, then add step (2) gained initiator in 3 times, react 3h, add 3g of methanol was termin...

Embodiment 2

[0036] (1) Dissolve 10g m-methylstyrene monomer in 10g ionic liquid 1-butyl-3-methylimidazole bis(trifluoromethanesulfonyl)imide salt; (2) Preparation of initiator complex : In an anhydrous and oxygen-free glove box, at a temperature of -60°C, add 25g of crown ether to a flask, add 5g of i-BuAlCl 2 Complex with crown ether, shake well for 5min; add 5g main initiator tert-butyl chloride (t-BuCl) to another flask; then i-BuAlCl complexed with crown ether 2 Add the co-initiator to the main initiator, shake well and age for 20 minutes; (3) Under normal pressure, replace the polymerization kettle with nitrogen three times, then cool down to -100°C, add 500g of solvent methyl chloride, dispersed carbon-containing The amount of nanotubes is 20g of hexane 200ml, then add 400g isobutylene, step (1) m-methylstyrene ionic liquid solution, add hexahydropyridine 5g, then add step (2) initiator in 3 times, react for 3h, add The terminator is 3g methanol, and the terminated solution is flas...

Embodiment 3

[0040] (1) Dissolve 20g p-methylstyrene monomer in 10g ionic liquid 1-butyl-3-methylimidazole bis(trifluoromethanesulfonyl)imide salt; (2) Preparation of initiator complex : In an anhydrous and oxygen-free glove box, at a temperature of -80°C, add 7.5g crown ether and 2.5g i-BuAlCl to a flask 2 Complex with crown ether, shake well for 4min; add 5g main initiator tert-butyl chloride (t-BuCl) to another flask; then i-BuAlCl complexed with crown ether 2 Add the co-initiator into the main initiator, shake well and age for 8 minutes; (3) Under normal pressure, replace the polymerization kettle with nitrogen three times, then cool down to -60°C, add 1000g of solvent methyl chloride, dispersed carbon-containing The amount of nanotubes is 20g of hexane 200ml, then add 400g isobutylene, step (1) p-methylstyrene ionic liquid solution, add hexahydropyridine 5g, then add step (2) initiator in 4 times, react for 3h, add The terminator is 3g methanol, and the terminated solution is flashed...

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Abstract

The invention provides a carbon nano tube modified isobutene and alkyl styrene polymer and a preparation method thereof. An initiator is added in several times, stability and controllability in reaction are realized, a polymerization reaction temperature range is wide, and reaction at a temperature ranging from -30 DEG C to -100 DEG C is available; due to addition of carbon nanotubes in the polymer, mechanical properties of the polymer are improved, and wide application in the field of polymer modification is realized; due to addition of piperidine which is a nucleophilic agent in a polymer synthesis process, the polymer is narrower in molecular weight distribution and excellent in processability. The polymer is a brand-new material, excellent in abrasion resistance and ageing resistance, polymer molecular weight reaches 50,000-150,000, molecular weight distribution is 1.5-3.0, the molar content of alkyl styrene in the polymer is larger than 3%, vulcanized rubber tensile strength is larger than or equal to 16.5MPa, abrasion strength I is smaller than or equal to 0.135cm<3>, and an ageing coefficient K is larger than or equal to 0.56.

Description

technical field [0001] The invention relates to an isobutylene and alkylstyrene polymer modified by carbon nanotubes and a preparation method thereof, in particular to a method for preparing isobutylene and alkylstyrene polymer by using a solution method. Background technique [0002] Butyl rubber (IIR) is synthesized by cationic polymerization of isobutylene and isoprene under the action of a catalyst. Its air tightness is 8 times better than that of natural rubber. It is mainly used in the production of automobile tire inner tubes, curing bladders and water tires; it is the world's largest The fourth largest type of synthetic rubber. As people pay more and more attention to the quality, safety and service temperature of automobile tires, many properties of butyl rubber (including heat resistance, oxygen, ozone aging and compression deformation resistance) need to be greatly improved. Therefore, it is of great significance to develop new types of rubber with high performan...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F210/10C08F212/12C08K5/3415C08K7/24
CPCC08F210/10C08K5/3415C08K7/24C08K2201/011C08F212/12
Inventor 魏绪玲付含琦杨珊珊燕鹏华龚光碧赵玉中张华强李晶胡海华梁滔郑聚成陈建刚
Owner PETROCHINA CO LTD
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