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Process for production of butyl rubber

A hydrocarbon-based and aryl-based technology, applied in the field of polymer preparation, can solve problems such as inactivity and inability to obtain polymers

Inactive Publication Date: 2005-08-17
LANXESS LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In fact, ZnCl 2 With or without haloalkane activators (such as Me 3 In the case of CCl or MeCOCl) and in the use of pure isobutene or isobutene / chloromethane mixtures it has been shown to be inactive, no polymers can be obtained

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] 97ml of isobutene was condensed in a 250ml 3-neck reaction flask fitted with a magnetic tracker and cooled to -78°C with a dry ice / acetone bath. Me in 3ml of isoprene and dichloromethane (2ml) 3 CCl solution (18.5 mg, 0.2 mmol) was added to the reaction vessel and then equilibrated at -78°C.

[0048] Zn(C 6 f 5 ) 2 • Toluene (98 mg, 0.2 mmol) was dissolved in 2 ml of dichloromethane and transferred via injection into the rapidly stirred (1000 rpm) mixture.

[0049] After 30 minutes, methanol (10 mL) was added to quench the reaction. The polymer was precipitated with 200 ml methanol, filtered and dried at 50°C to constant weight. The yield was 4.5g, M n =581000 and M w = 1306000, the isoprene content is 2.7-mol% and the gel content is 1.5%.

Embodiment 2

[0051] 95ml of dry isobutene was condensed in a 250ml 3 neck reaction flask fitted with a magnetic tracker and cooled to -78°C with a dry ice / acetone bath. Me in 5ml of isoprene and dichloromethane (2ml) 3 CCl solution (27.8 mg, 0.3 mmol) was added to the reaction vessel. The compound was stirred rapidly at -78°C, and 148 mg (0.3 mmol) of Zn(C 6 f 5 ) 2 • Toluene. After 30 minutes methanol (10ml) was added to quench the reaction. The polymer was precipitated with 200 ml of methanol and dried at 50°C to constant weight.

[0052] The yield of the copolymer was 3.8 g, M n = 226000 and M w =661000, the isoprene content is 4.7 mol-% and the gel content is 1.0%.

Embodiment 3

[0054] The procedure of Example 2 was repeated except that 93 ml of isobutene and 7 ml of isoprene were used. The yield of the copolymer was 4.0 g, M n = 302000 and M w =782000, the isoprene content is 6.4 mol-% and the gel content is 3.8%.

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PUM

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Abstract

The present invention relates to a process for the preparation of polymers comprising repeat units derived from at least one isoolefin monomer, optionally repeat units derived from at least one multiene monomer and optionally other copolymerizable monomers, The process is carried out in the presence of a zinc compound and optionally an organic halide activator.

Description

technical field [0001] The present invention relates to a process for the preparation of polymers comprising repeat units derived from at least one isoolefin monomer, optionally repeat units derived from at least one multiene monomer and optionally other copolymerizable monomers , which is carried out in the presence of a zinc compound. Background technique [0002] Butyl rubber is considered to be a copolymer of an isoolefin and one or more (preferably conjugated) multiolefins as comonomers. Commercial butyl rubber contains mostly isoolefins and a small amount of conjugated polyolefins. The isoolefin is preferably isobutene. [0003] Butyl rubber or butyl polymers are usually prepared by the slurry method, which uses methyl chloride as a carrier and Friedel-Crafts catalyst as part of the polymerization initiator. The temperature of the polymerization reaction is generally between about -90°C and -100°C. See US Patent No. 2,356,128 and Ullmanns Encyclopedia of Industrial...

Claims

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Application Information

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IPC IPC(8): C08F10/10C08F2/04C08F4/50C08F10/00C08F36/04C08F110/10C08F210/10C08F210/12C08F236/08C08L11/00
CPCC08F210/12C08F10/00C08F4/50C08F4/00C08F236/08C08F2500/03
Inventor M·博赫曼S·加拉特
Owner LANXESS LTD