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Technology for directly producing halogenated butyl rubber using butyl glue prepared by solution method

A technology of halogenated butyl rubber and butyl rubber, which is applied in the field of direct production of halogenated butyl rubber from butyl glue solution by solution method, which can solve the problems of inability to prepare uniform and stable halogenated butyl rubber, processing difficulties, and degradation of butyl rubber, etc. problems, to avoid solvent switching, improve co-vulcanization, and increase reactivity

Inactive Publication Date: 2012-10-03
BEIJING INSTITUTE OF PETROCHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method easily degrades butyl rubber during processing and mixing, which brings difficulties in the processing process, and cannot prepare uniform and stable halogenated butyl rubber.
[0009] The production methods of butyl rubber mainly include slurry method and solution method. The preparation of butyl rubber and halogenated butyl rubber by slurry method technology is monopolized by EXXON Company of the United States and Lanxess Company of Germany. The preparation of butyl rubber by solution method technology in Russia Taoli Developed by Yadi Synthetic Rubber Company, there is no report on the direct preparation of halogenated butyl rubber by solution method technology

Method used

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  • Technology for directly producing halogenated butyl rubber using butyl glue prepared by solution method
  • Technology for directly producing halogenated butyl rubber using butyl glue prepared by solution method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] At -100°C, add hexane and methyl chloride to the reaction kettle to form a mixed solvent (hexane 160mL, methyl chloride 72mL), the mass ratio of methyl chloride to hexane is 38:62; mix well and then add 140mL to the solvent Isobutene and isoprene, the mass ratio of isobutene and isoprene is 97:3. The monomer concentration is 36wt%. The molar ratio of sesquiethylaluminum chloride (0.0036mol / L) is 1:3, and the initiator system is added to the polymerization kettle to initiate polymerization, and the polymerization is carried out for 30 minutes to obtain butyl rubber glue. The molecular weight of butyl rubber is determined to be 500 , 000g / mol, the molecular weight distribution is 1.9, and the isoprene content is 2.0mol%. After entering reactor 3 to settle for 100 minutes, enter reactor 4 after extracting the water layer with a pump, remove monochloromethane, unreacted isobutylene and part of hexane, and the glue concentration is 65 wt%. Add hexane, glue The liquid concen...

Embodiment 2

[0024] At -80°C, add hexane and methyl chloride to the reaction kettle to form a mixed solvent (hexane 120mL, methyl chloride 90mL), the mass ratio of methyl chloride to hexane is 50:50; mix well and then add 155mL to the solvent Isobutylene and isoprene, the mass ratio of isobutylene and isoprene is 98:2. The monomer concentration is 45wt%. The initiator system consists of cumyl chloride, ethyl aluminum dichloride and formamide, and the cumyl chloride is 0.01mol / L, ethylaluminum dichloride is 0.24mol / L, and formamide is 0.01mol / L. The molar ratio of water: formamide: ethyl aluminum dichloride is 1:1:24. Add an initiator system to the polymerization kettle to initiate polymerization, and polymerize for 60 minutes to obtain butyl rubber glue. The molecular weight of butyl rubber is determined to be 55 , 000g / mol, the molecular weight distribution is 1.9, and the isoprene content is 1.5mol%. After entering reactor 3 to settle for 180 minutes, enter reactor 4 after extracting t...

Embodiment 3

[0026] At -50°C, add hexane and methyl chloride to the reaction kettle to form a mixed solvent (hexane 160mL, methyl chloride 30mL), the mass ratio of methyl chloride to hexane is 20:80; mix well and then add 35mL to the solvent Isobutene and isoprene, the mass ratio of isobutene and isoprene is 85:15. The monomer concentration is 15wt%. The initiator system consists of dicumyl chloride, aluminum trichloride and acetone, and the content of dicumyl chloride is 0.01mol / L, aluminum trichloride is 0.6mol / L, and acetone is 0.1mol / L. Dicumyl chloride: acetone: the molar ratio of aluminum trichloride is 1:10:60. Add initiating system in polymerization kettle and initiate polymerization, polymerization 60 minutes, obtain butyl rubber glue, the molecular weight of butyl rubber after measuring is 10,000g / mol, the molecular weight distribution is 1.9, and the isoprene content is 10mol%. After entering reactor 3 to settle for 80 minutes, enter reactor 4 after extracting the water layer ...

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Abstract

The invention discloses a technology for directly producing halogenated butyl rubber using butyl glue prepared by a solution method. The technology sequentially comprises the four steps as follows: (I), synthetizing butyl rubber; (II), removing methyl chloride; (III), settling for separation; and (IV), halogenating the butyl rubber. Halogenated butyl rubber is prepared through a halogenating reaction of solution method butyl rubber. In a mixed solvent of alkane and the methyl chloride, the solution method butyl rubber is prepared by copolymerising isobutylene and isoprene positive ions, halogenated butyl glue is prepared by removing the methyl chloride, settling for separation and halogenating the butyl glue at low temperature. The detailed technology can be consulted on the specification. The technology of the invention has the advantages that the butyl rubber not only forms additional crosslinking positions after being halogenated, but also increases double bond reactivity, increases the curing speed of the butyl rubber, improves the co-curing behavior with unsaturated rubber, and increases the adhesiveness and the cure efficiency of metal and the rubber, thereby avoiding solvent switching or rubber stock dissolving of a slurry process.

Description

technical field [0001] The invention relates to a process for preparing halogenated rubber, in particular to a process for directly producing halogenated butyl rubber by preparing butyl glue in a solution method. Background technique [0002] Halogenated butyl rubber can be divided into two types: chlorobutyl rubber and bromobutyl rubber, which are butyl rubber with a certain degree of unsaturation in aliphatic hydrocarbons (such as hexane) and chlorine or Product of bromine reaction. The reaction is completed under strictly controlled conditions, so the original double bond in the butyl rubber molecule can be maintained, and the halogen is combined in the form of an allyl group. [0003] At present, Exxon and Lanxess prepare halogenated butyl rubber through slurry technology. The production process includes the synthesis of butyl rubber, the removal of unreacted monomers, the exchange of methyl chloride and good solvent, halogenation and neutralization after halogenation ...

Claims

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Application Information

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IPC IPC(8): C08F210/12C08F2/06C08F8/22
Inventor 郭文莉伍一波李树新商育伟
Owner BEIJING INSTITUTE OF PETROCHEMICAL TECHNOLOGY
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