Cationic polymerization system and preparation method of high-unsaturation-degree isoolefin copolymer

A cationic polymerization and isoolefin technology, which is applied in the field of cationic polymerization system and high unsaturation isoolefin copolymer preparation, can solve the problems of toxic safety of organic nitrating reagents, poisonous and explosive nitromethane, and achieve unsaturated Increased efficiency, efficient utilization, and reduced energy consumption

Active Publication Date: 2016-06-08
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The organic nitration reagents used in the above-mentioned patented technologies are toxic and poor in safety, such as nitromethane is toxic, flammable, explosive, etc.
CN1526745B and CN101775092A disclose a kind of adopting AlCl 3 Co-initiation systems and continuous processes for the production of polymers at conversions from 50% to 95% in the presence of at least one polyene crosslinker divinylbenzene reagent, the gel content of the polymer product being less than 15% by weight, The degree of unsaturation is greater than 4.1mol%. This method is carried out in the absence of transition metal compounds and organic nitro compounds, but the polyene crosslinking agent divinylbenzene is expensive, and the presence of difunctional groups can easily lead to gel formation. form

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Under the protection of -40℃ and high-purity nitrogen, CH 2 Cl 2 As the reaction medium, the H 2 O, HCl and AlCl 3 Pre-react for 1 hour, then add butyl chloroacetate, mix well and let stand for 2 hours to obtain a homogeneous solution.

[0023] Under the protection of high-purity nitrogen at -102°C, add 20 mL of a mixed solution containing isobutene (IB), isoprene (IP) and tetrafluoroethane ([IB]=5.0mol / L, IP Feeding amount accounts for 3.0mol% of monomer total amount), then adds above-mentioned homogeneous solution and initiates monomer to carry out polymerization reaction, wherein AlCl 3 The molar ratio to the total amount of monomers is 1.1×10 -3 , H 2 The molar ratio of O to the total amount of monomers is 2.4×10 -5 , the molar ratio of HCl to the total amount of monomers is 2.2×10 -5 , the molar ratio of butyl chloroacetate to monomer (IB+IP) is 1.8×10 -3 . After 0.5 hours of polymerization reaction, 5 mL of ethanol solution containing 1 wt % antioxidant 1...

Embodiment 2

[0025] Under the protection of -50℃ and high-purity nitrogen, CH 2 Cl 2 As the reaction medium, the H 2 O, HCl and AlCl 3 Pre-react for 0.5 hour, then add tert-butyl chloroacetate and isopropyl chloroacetate, mix well and leave for 4 hours to prepare a homogeneous solution.

[0026] The polymerization method is the same as in Example 1, except that the solvent is dichloromethane, [IB] is 3.9mol / L, the IP charging amount is 7.5mol%, AlCl 3 The molar ratio to the total amount of monomers is 6.2×10 -3 , H 2 The molar ratio of O to the total amount of monomers is 6.2×10 -5 , the molar ratio of HCl to the total amount of monomers is 1.0×10 -5 , the molar ratio of tert-butyl chloroacetate to the total amount of monomers is 2.0×10 -3 , the molar ratio of isopropyl chloroacetate to the total amount of monomers is 2.0×10 -4 . The polymerization reaction was terminated after 1 hour, and the termination and aftertreatment methods were the same as in Example 1. The yield of isob...

Embodiment 3

[0028] Under the protection of -90℃ and high-purity nitrogen, CH 2 Cl 2 As the reaction medium, the H 2 O, HCl and AlCl 3 Pre-reacted for 1 hour, then added butyl chloroacetate, mixed evenly and left for 168 hours to obtain a homogeneous solution.

[0029] The polymerization method is the same as in Example 1, [IB] is 3.0mol / L, and the IP charging amount accounts for 2.5mol% of the total amount of monomers, and the AlCl 3 The molar ratio to the total amount of monomers is 1.3×10 -3 , H 2 The molar ratio of O to the total amount of monomers is 6.0×10-5 , the molar ratio of butyl chloroacetate to the total amount of monomers is 1.4×10 -3 . The polymerization reaction was terminated after 2 hours, and the termination and aftertreatment methods were the same as in Example 1. The yield of isobutylene and isoprene copolymer is 28%, M w 3.2×10 5 g / mol, M w / M n It was 2.7, the isoprene content was 2.6%, and the gel content was undetectable.

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Abstract

The invention relates to a cationic polymerization system and a preparation method of a high-unsaturation-degree isoolefin copolymer. The polymerization system and a polymerization method can improve the feeding amount of multiolefin copolymerization monomers in the system, high-molecular-weight, high-unsaturation-degree (high multiolefin content) and substantially gel-free copolymer product can be obtained, the monomer conversion rate is relatively high, the reaction efficiency of a catalyst and the copolymerization monomers is high, the catalyst cost is low, and industrial application value is achieved.

Description

technical field [0001] The present invention relates to a cationic polymerization system and a method for preparing a high unsaturation isoolefin copolymer, more specifically, a cationic polymerization of an isoolefin monomer under the action of a composite catalyst to prepare a high unsaturation isoolefin copolymer Methods. Background technique [0002] Isoolefin copolymers containing unsaturated structural units are usually copolymerized from isoolefins and other olefin monomers, and the degree of unsaturation refers to the content of unsaturated structural units (such as conjugated dienes) in the copolymer. For example, the industrial product butyl rubber is an important synthetic rubber, which is a copolymer of isobutylene (IB) and a small amount of isoprene (IP). The degree of unsaturation refers to the content of isoprene in the copolymer, usually at 2.5 mol% (mole fraction) or less. Butyl rubber has excellent air tightness and tension / compression shock absorption, a...

Claims

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Application Information

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IPC IPC(8): C08F210/10C08F236/00C08F210/14C08F210/12C08F236/08
Inventor 吴一弦孟晓燕刘文红
Owner CHINA PETROLEUM & CHEM CORP
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