Ethyl-acetate-grafted isobutene-isoprene-alkylstyrene polymer and preparation method thereof

A technology of alkyl styrene and ethyl acetate, applied in the production of bulk chemicals, etc., can solve the problems such as the limitation of polymerization reaction control, and achieve the effects of good rigidity, narrow molecular weight distribution and stable processing performance

Inactive Publication Date: 2017-07-07
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

[0030] (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 -50°C, add 15g of crown ether and 5g of isobutylaluminum dichloride (i-BuAlCl 2 ) complexed with crown ether, and shaken for complexation for 8min; in another flask, 5g main initiator tert-butyl chloride (t-BuCl) was added; then the i-BuAlCl complexed with crown ether 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 -50°C, add 500g of methyl chloride as a solvent, and then add 200g Isobutylene, 1g isoprene and step (1) gained o-toluene styrene ionic liquid solution, then add 1 / 2 step (2) gained initiator, react 30min, add 1g ethyl acetate, add remaining initiator, After reacting for 30 minutes, 3 g of methan...

Embodiment 2

[0034] (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 7g of crown ether and 7g of i-BuAlCl to a flask 2 Complex with crown ether, shake well for 5min; add 7g 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 15 minutes; (3) Under normal pressure, replace the polymerization kettle with nitrogen three times, then cool down to -50°C, add 1000g of methyl chloride as a solvent, and then add 400g Isobutylene, 2g isoprene and step (1) gained m-methylstyrene ionic liquid solution, then add 3 / 4 step (2) gained initiator, react 3h, add 2g ethyl acetate, add remaining initiator, After reacting for 1 hour, 3 g of methanol was added as a terminator, and the terminated solution...

Embodiment 3

[0038] (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 -70°C, add 30g of crown ether to a flask, add 10g of i-BuAlCl 2 Complex with crown ether, shake well for 4min; add 8g 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 20 minutes; (3) Under normal pressure, replace the polymerization kettle with nitrogen three times, then cool down to -100°C, add 1000g of methyl chloride as a solvent, and then add 400g Isobutylene, 1g isoprene and step (1) gained p-methylstyrene ionic liquid solution, then add 1 / 4 of the initiator of step (2) gained, react 2h, add 1g ethyl acetate, add remaining initiator , React for 2h, add 2g of methanol as a terminator, and the terminated solution is f...

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Abstract

The invention provides an ethyl-acetate-grafted isobutene-isoprene-alkylstyrene polymer and a preparation method thereof. The preparation method includes the steps of subjecting a polymerization kettle to nitrogen displacement for three times at the normal pressure, cooling to -50-100 DEG C, adding chloromethane as a solvent and an isobutene-isoprene-alkylstyrene ionic liquid solution sequentially, adding 1 / 4-3 / 4 part by mass of initiator to react for 30 minutes to 3 hours, adding ethyl acetate and residual initiator to react for 30 minutes to 3 hours, adding a terminator for termination reaction, and performing flashing, filtration and drying on a terminated solution so as to obtain a finished product. The molecular weight of the polymer is 50,000-150,000, molecular weight distribution ranges from 1.5 to 2.5, the molar content of alkylstyrene in the polymer is more than 3%, the molar content of an ester group is between 0.02% and 0.05%, and the tensile strength of vulcanized rubber is not less than 15 MPa.

Description

technical field [0001] The invention relates to a polymer of isobutylene, isoprene and alkylstyrene grafted with ethyl acetate and a preparation method thereof, in particular to a solution method for preparing polymers of isobutylene, isoprene and alkylstyrene Methods. 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...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F210/12C08F212/12C08F236/10C08F297/00C08F2/42C08F8/14
CPCC08F8/14C08F210/12C08F297/00C08F212/12C08F236/10C08F2500/03C08F2/42Y02P20/54
Inventor 魏绪玲魏玉丽燕鹏华付含琦杨珊珊丛日新李晶赵玉中赵洪国龚光碧胡海华梁滔郑聚成陈建刚武爱军蔡文婧伍一波郭文莉李树新
Owner PETROCHINA CO LTD
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