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Bromination process of star-branched butyl rubber

A bromination and process technology, applied in the field of rubber, can solve the problems affecting the processing performance of brominated butyl rubber and the low content of Type II secondary structure rubber.

Active Publication Date: 2021-03-30
山东京博中聚新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] But, in the prior art, after the star-branched butyl rubber is brominated, the isomerization of the Type II secondary structure rubber to the Type III primary structure in the resulting product is obvious, and the Type II secondary structure rubber content is relatively low. Affects the processability of bromobutyl rubber

Method used

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  • Bromination process of star-branched butyl rubber
  • Bromination process of star-branched butyl rubber

Examples

Experimental program
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Effect test

Embodiment 1

[0064] With n-hexane as aliphatic hydrocarbon and cyclohexane as branching agent capture agent; Br 2 is a brominating agent, and NaOH solution (mass fraction 2wt%) is a neutralizing agent. The specific process is as follows:

[0065] S1. Weigh 30g of star-branched butyl rubber, add 170g of n-hexane, swell, stir and dissolve, and obtain a glue solution with a mass fraction of 15wt%.

[0066] S2. Add 9 g of cyclohexane to the obtained glue solution, and stir for 30 minutes to obtain a mixed solution.

[0067] S3. Add Br to the obtained mixed solution under the condition of avoiding light at 40°C 2 n-hexane solution (Br 2 0.42mL, n-hexane 15mL; Br 2 The molar ratio to the unsaturated double bond in the star-branched butyl rubber is 0.92:1), stirred and reacted for 10 minutes to obtain the brominated glue.

[0068] S4. Add 25g NaOH solution (mass fraction 2wt%, the molar ratio of NaOH to the bromine element in the brominating agent is 0.76:1) to the obtained brominated glue, ...

Embodiment 2

[0072] With n-hexane as aliphatic hydrocarbon and cyclohexane as branching agent capture agent; Br 2 is a brominating agent, NaClO is an oxidizing agent, and NaOH solution (mass fraction 2wt%) is a neutralizing agent. The specific process is as follows:

[0073] S1. Weigh 30 g of star-branched butyl rubber, add 157.5 g of n-hexane, swell, stir and dissolve, and obtain a glue solution with a mass fraction of 16 wt%.

[0074] S2. Add 3 g of cyclohexane to the obtained glue solution, and stir for 30 minutes to obtain a mixed solution.

[0075] S3, under the condition of 40°C in the dark, add 10g NaClO solution (mass fraction is 10wt%), Br 2 n-hexane solution (Br 2 0.34mL, n-hexane 10mL; Br 2 The molar ratio to the unsaturated double bond in the star-branched butyl rubber is 0.74:1), stirred and reacted for 10 minutes to obtain the brominated glue.

[0076] S4, add 20g NaOH solution (mass fraction 2wt%, the molar ratio of NaOH to the bromine element in the brominating agent i...

Embodiment 3

[0080] With n-hexane as aliphatic hydrocarbon, benzene as branching agent and capture agent; HBr as bromination agent, NaBrO 3 is an oxidizing agent, and NaOH solution (mass fraction 2wt%) is a neutralizing agent. The specific process is as follows:

[0081] S1. Weigh 30g of star-branched butyl rubber, add 120g of n-hexane, swell, stir and dissolve, and obtain a glue solution with a mass fraction of 20wt%.

[0082] S2. Add 15 g of benzene to the obtained glue solution, and stir for 30 minutes to obtain a mixed solution.

[0083] S3. Add 10 g of NaBrO to the resulting mixed solution under the condition of 40°C in the dark. 3 Aqueous solution (mass fraction is 20wt%), 4g HBr aqueous solution (massfraction is 40wt%; The molar ratio of bromine element and unsaturated double bond in the star-branched butyl rubber is 3.64: 1), stirring reaction 10min, obtains bromination After glue.

[0084] S4, add 50g NaOH solution (mass fraction 2wt%, the molar ratio of NaOH and the bromine e...

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Abstract

The invention provides a bromination process of star-branched butyl rubber, which comprises the following steps: a) dissolving the star-branched butyl rubber in aliphatic hydrocarbon to obtain a rubber solution; b) mixing the glue solution with a branching agent capturing agent to obtain a mixed solution; c) performing bromination, neutralization and product recovery on the mixed solution to obtain brominated star-shaped branched butyl rubber, wherein the branching agent capturing agent is selected from one or more of ethanol, isopropanol, acetone, methyl ether, cyclohexane, dichloromethane, benzene and methylbenzene. The method is completed by dissolving star-shaped branched butyl rubber in aliphatic hydrocarbon, adding a certain amount of a branching agent capturing agent, adding an oxidant, and carrying out subsequent bromination, neutralization and product recovery; therefore, the residual branching agent in the star-branched butyl rubber can be dissolved before bromination, and isprevented from being combined with an HBr by-product generated in the bromination process, so that the neutralization efficiency is improved, and isomerization conversion from a Type II secondary structure to a Type III primary structure is inhibited.

Description

technical field [0001] The invention relates to the field of rubber, in particular to a bromination process of star branched butyl rubber. Background technique [0002] Butyl rubber is the most airtight rubber material. As one of the modified products of butyl rubber (IIR), brominated butyl rubber (BIIR) not only maintains the excellent air tightness, heat aging resistance, damping performance and other characteristics of butyl rubber, but also has fast vulcanization speed, resistance Good heat resistance, good compatibility with other rubbers, strong self-adhesiveness and inter-adhesiveness, can be vulcanized with ZnO and other excellent properties. Therefore, BIIR is gradually replacing IIR in the fields of radial tires, heat-resistant inner tubes, container linings, medicine bottle stoppers and machine liners. The increasing development of the above application fields determines that there is an urgent need to increase BIIR production capacity, improve the utilization r...

Claims

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Application Information

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IPC IPC(8): C08F8/22C08F8/20C08F210/12
CPCC08F8/22C08F8/20C08F210/12
Inventor 李立霞栾波任学斌牟庆平
Owner 山东京博中聚新材料有限公司
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