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Preparation method of halogenated butyl rubber

A technology of halogenated butyl rubber and butyl rubber, which is applied in the field of rubber, can solve the problems of affecting product quality, high degree of isomerization of brominated products, and increased content of III structure, so as to improve product quality, eliminate the risk of foaming, The effect of increasing content

Active Publication Date: 2020-11-03
山东京博中聚新材料有限公司
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  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For the solvent stripping process, the residual catalyst in the polymer slurry will always exist in the sol process, the longer the existence time, the greater the Mooney drop, and it will also lead to an increase in the content of the III structure of the brominated product, that is, the brominated product is iso A high degree of structuring affects product quality

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  • Preparation method of halogenated butyl rubber
  • Preparation method of halogenated butyl rubber
  • Preparation method of halogenated butyl rubber

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preparation example Construction

[0038] The invention provides a kind of preparation method of halogenated butyl rubber, comprises the following steps:

[0039]a) sending butyl rubber glue, halogenating agent, oxidizing agent and modifier into a halogenation reactor to carry out halogenation reaction to obtain halogenated butyl rubber liquid;

[0040] b) using an alkali metal hydroxide to neutralize the halogenated butyl rubber solution to obtain a primary neutralization solution;

[0041] c) using calcium chloride to carry out secondary neutralization to the primary neutralization solution to obtain a secondary neutralization solution;

[0042] d) removing the solvent from the secondary neutralization solution and drying to obtain halogenated butyl rubber;

[0043] The improver is selected from one or more of stearic acid and stearate;

[0044] The butyl rubber glue is the butyl rubber glue obtained by hexane stripping.

[0045] In the preparation method provided by the invention, in the halogenation reac...

Embodiment 1

[0115] use figure 2 The device shown was prepared, figure 2 It is a schematic diagram of the production equipment used in the examples of the present invention. Among them, 1-6 are systems for preparing butyl rubber glue, and 7-12 are systems for preparing butyl rubber glue into halogenated butyl rubber. Specifically: 1 is a polymerization reactor, 2 is a flash tank, 3 is a stripper, 4 is the first high-speed mixer, 5 is a buffer device, 6 is a concentration regulator; 7 is a halogenation reactor, 8 and 9 are Neutralization system (8 is the first tank, 9 is the second neutralization tank), 10 is the flash tank, 11 is the stripping tank, and 12 is the drying system.

[0116] 1.1 Preparation of butyl rubber glue:

[0117] With methyl chloride as the medium, AlEtCl 2 and HCl as catalyst (AlEtCl 2 : The mass ratio of HCl is 18:1), and isobutylene and isoprene are monomers (the mass ratio of isobutylene:isoprene is 100:3). AlEtCl 2 Dissolve in methyl chloride to obtain a c...

Embodiment 2

[0136] 1.1 Preparation of butyl rubber glue

[0137] Prepare butyl rubber glue according to the preparation process of Example 1, the difference is that the catalyst deactivator added in flash tank 2 is n-butyl ether, and the n-butyl ether content in glue A is 210ppm; add the first high-speed mixing The amount of water added to device 4 is 3.5wt%. After the heat exchange treatment of the heat exchanger, the temperature of the glue solution is 40°C. The concentration of the final butyl rubber solution is 18.3wt%, the monomer content is 1.9ppm, and the water content is 0.37 wt%, the temperature is 40°C.

[0138] 1.2 Preparation of halogenated butyl rubber

[0139] Utilize gained butyl rubber solution to prepare brominated butyl rubber according to the preparation process of embodiment 1, difference is:

[0140] Bromine sent to the halogenation reactor: the flow rate is 89.5g / h, the weight ratio of bromine to dry glue is 33.0:1000; hydrogen peroxide: the flow rate is 44.38g / h, ...

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Abstract

The invention provides a preparation method of halogenated butyl rubber. According to the preparation method provided by the invention, in a halogenation reaction unit, besides butyl rubber liquid, which serves as a reaction raw material, obtained by hexane steam stripping and a halogenating agent, an oxidizing agent and an improver (the improver being selected from one or more of stearic acid andstearate) are also fed together. By adding the specific improver and the oxidizing agent, isomerization from a Type II secondary structure to a Type III primary structure in a halogenated product canbe effectively inhibited, and the product quality is improved. Meanwhile, the utilization rate of the halogenating agent and the oxidizing agent can be improved. In a neutralization unit, two steps of neutralization are adopted, the first step of neutralization is metal hydroxide neutralization, then calcium chloride is introduced for neutralization, water-soluble stearate generated by the halogenation unit is converted into calcium stearate, the foaming risk of a subsequent coagulation desolvation system is eliminated, and the influence on a downstream sewage treatment system is reduced.

Description

technical field [0001] The invention relates to the technical field of rubber, in particular to a preparation method of halogenated butyl rubber. Background technique [0002] At present, the industrial production of halogenated butyl rubber adopts the solution method. Specifically, the base rubber butyl rubber is dissolved in a solvent to obtain a certain concentration of butyl rubber glue, and then reacted with halogen to obtain halogenated butyl rubber. Therefore, the acquisition of butyl rubber glue is very important to the preparation of halogenated butyl rubber. Usually, the base rubber butyl rubber is prepared first, and then the product is processed to obtain the butyl rubber glue. [0003] Among them, the industrial production of base rubber butyl rubber is the most commonly used slurry method. Specifically, firstly, the monomer is dissolved in methyl chloride to obtain a mixed material, and the mixed material enters a polymerization reactor after multi-stage cooli...

Claims

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Application Information

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IPC IPC(8): C08F8/22C08F210/12C08F236/08
CPCC08F8/22C08F210/12C08F236/08
Inventor 徐宏德卜立敏崔红梅王衍金任学斌栾波
Owner 山东京博中聚新材料有限公司
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