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Producing method for brominating butyl rubber

A technology of brominated butyl rubber and its production method, which is applied in the field of butyl rubber bromination, can solve the problems of slow bromination reaction rate and long bromination time, so as to increase the bromination reaction rate, enhance the dispersion performance, and improve the conversion The effect of rate and utilization

Active Publication Date: 2015-12-02
CHAMBROAD CHEM IND RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the reaction medium usually used in these patents is a non-polar solvent, the bromination time is relatively long, and the bromination reaction rate is relatively slow

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] In this embodiment, chloroform is used as the reaction medium, and Br 2 As a brominating agent, sodium hypochlorite (NaClO) is an oxidizing agent, sodium hydroxide is an acid-binding agent, and surfactant OP-10 is used to brominate butyl rubber to obtain brominated butyl rubber. The specific steps are as follows:

[0027] 1) Weigh 60 g of butyl rubber, add 340 g of chloroform, swell and stir to obtain glue, the concentration of the glue is 15%wt. Raw gum unsaturation is 1.8±0.2%mol, Mooney viscosity ML(1+8) 125℃ It is 51±5.

[0028] 2) Dissolve 1.75g ​​NaClO, 0.08g sodium hydroxide, 5.0g deionized water and 0.25g surfactant in 20mL chloroform solvent, vibrate and stir vigorously to form an emulsion.

[0029] 3) Under the condition of 35°C, dilute 3.1g of liquid bromine and the emulsion formed in step 2) respectively and dropwise into the glue solution obtained in step (1) at the same time, after the dropwise addition is completed, stir and react for 20 minutes.

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Embodiment 2

[0033] Present embodiment is the mixed solvent of 80 / 20 with chloroform / methylene chloride as reaction medium, Br 2 As a brominating agent, sodium hypochlorite (NaClO) is an oxidizing agent, sodium hydroxide is an acid-binding agent, and surfactant OP-10 is used to brominate butyl rubber to obtain brominated butyl rubber. The specific steps are as follows:

[0034] 1) Weigh 20 g of butyl rubber, add 380 g of solvent, swell, and stir to obtain a glue solution with a concentration of 5% wt. Raw gum unsaturation is 1.8±0.2%mol, Mooney viscosity ML(1+8) 125℃ It is 51±5.

[0035] 2) Dissolve 1.33g NaClO, 0.05g sodium hydroxide, 5g deionized water and 0.25g surfactant in 20mL mixed solvent, vibrate and stir vigorously to form an emulsion.

[0036] 3) Under the condition of 55°C, dilute 1.44g of liquid bromine and the emulsion formed in step 2) respectively and dropwise into the glue solution obtained in step (1) at the same time, after the dropwise addition is completed, stir and...

Embodiment 3

[0040] In this embodiment, chloroform / dichloromethane is a mixed solvent of 70 / 30 as the reaction medium, and Br 2 As a brominating agent, sodium hypochlorite (NaClO) is an oxidizing agent, sodium hydroxide is an acid-binding agent, and surfactant OP-10 is used to brominate butyl rubber to obtain brominated butyl rubber. The specific steps are as follows:

[0041] 1) Weigh 40 g of butyl rubber, add 360 g of solvent, swell and stir to obtain glue, the concentration of the glue is 10%wt. Raw gum unsaturation is 1.8±0.2%mol, Mooney viscosity ML(1+8) 125℃ It is 51±5.

[0042] 2) Dissolve 0.81g NaClO, 0.05g sodium hydroxide, 5g deionized water and 0.25g surfactant in 20mL mixed solvent, vibrate and stir vigorously to form an emulsion.

[0043] 3) Under the condition of 45°C, dilute 1.44g of liquid bromine and the emulsion formed in step 2) respectively and dropwise into the glue obtained in step (1) at the same time, after the dropwise addition is completed, stir for 10 minutes ...

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Abstract

The invention belongs to the technical field of butyl rubber brominating, and particularly relates to a producing method for brominating butyl rubber. According to the producing method, the butyl rubber is bromized by mainly adopting weak-polar organic solvents as reacting solvents, the brominating reaction speed is increased, the converting ratio and the using ratio of bromine atoms are increased, and side reactions are effectively avoided.

Description

technical field [0001] The invention belongs to the technical field of bromination of butyl rubber, in particular to a production method of brominated butyl rubber. Background technique [0002] Bromobutyl rubber (BIIR) has the advantages of fast vulcanization speed, good adhesion and heat resistance, good scorch safety, and can be vulcanized with zinc oxide alone. It has gradually replaced ordinary butyl rubber in various application fields. , such as industrial products such as radial tires, heat-resistant inner tubes, container linings, pharmaceutical bottle stoppers and machine liners. [0003] The bromination reaction process conditions of butyl rubber are demanding, and the bromination temperature, glue viscosity, bromine dosage and bromination reaction time all affect the quality of the obtained brominated butyl rubber. WO2010 / 006983 discloses a standard halogenation process with bromine as the brominating agent. The main problem of this method is that the utilizati...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F210/12C08F8/20C08F8/22
Inventor 张另见马韵升姚刚史庆苓刘振学柳金章李立霞李卫卫
Owner CHAMBROAD CHEM IND RES INST CO LTD
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