Method for purifying rubber vulcanization accelerator MBT (2-mercaptobenzothiazole)

A purification method and rubber vulcanization technology, which is applied in the direction of organic chemistry, can solve the problem of low MBT purity, and achieve the effects of high purity, easy industrialization, and simple process

Active Publication Date: 2014-04-23
SHANDONG SUNSINE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method can only remove a small amount of resin and impurities, and the purity of the refined MBT is not high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0014] The crude M with a mass content of 50-80% is dissolved in alkali, that is, the sodium hydroxide solution with a weight concentration of 30% dissolves the crude M completely and has a pH of 9.5, and then dilutes it to a weight concentration of 3% with deionized water, and then performs blowing oxidation For 1.5 hours, add dropwise a sulfuric acid solution with a weight concentration of 3% at a rate of 3 L / min until pH = 9, and the solution is clear and transparent. After filtration, raise the temperature of M-Na salt solution to 25°C, and when it reaches a clear and transparent state, add dropwise sulfuric acid solution with a weight concentration of 10% to neutralize to PH = 5, then filter and take the solid, dehydrate, wash with water, and dry to obtain the finished product MBT . The 2-mercaptobenzothiazole accelerator has a mass content of 99.1% and a melting point of 181.1°C.

example 2

[0016] The crude M with a mass content of 50-80% is dissolved in alkali, that is, the sodium hydroxide solution with a weight concentration of 30% dissolves the crude M completely and has a pH of 9.5, and then dilutes it to a weight concentration of 5% with deionized water, and then performs blowing oxidation For 2 hours, add dropwise a sulfuric acid solution with a weight concentration of 2% at the same time at a rate of 2 L / min until pH = 9, and the solution is clear and transparent. After filtering, raise the temperature of the M-Na salt solution to 55°C, and when it reaches a clear and transparent state, add dropwise a sulfuric acid solution with a weight concentration of 8% to neutralize it to PH=6, and then filter to take the solid, dehydrate, wash with water, and dry to obtain the finished product MBT. The 2-mercaptobenzothiazole accelerator has a mass content of 99.3% and a melting point of 181.8°C.

example 3

[0018] The crude M with a mass content of 50-80% is dissolved in alkali, that is, the sodium hydroxide solution with a weight concentration of 30% dissolves the crude M completely and has a pH of 9.5, and then dilutes it to a weight concentration of 8% with deionized water, and then performs blowing oxidation For 2.5 hours, add a sulfuric acid solution with a weight concentration of 1% dropwise at the same time at a rate of 1L / min until pH = 9, and the solution is clear and transparent. After filtering, raise the temperature of M-Na salt solution to 95°C, and when it reaches a clear and transparent state, add dropwise sulfuric acid solution with a weight concentration of 5% to neutralize to PH = 7, then filter to take the solid, dehydrate, wash with water, and dry to obtain the finished product MBT. The 2-mercaptobenzothiazole accelerator has a mass content of 99.7% and a melting point of 182.8°C.

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Abstract

The invention discloses a method for purifying a rubber vulcanization accelerator MBT (2-mercaptobenzothiazole). The method comprises the following steps: completely dissolving crude M by using a sodium hydroxide solution with the weight concentration of 30%, controlling the final pH of the sodium salt solution to be 9.5, adding deionized water to dilute, controlling the weight concentration of the sodium salt solution to be 3-8%, blowing and oxidizing for 1.5-2.5 hours, dropwise adding a sulfuric acid solution with the weight concentration of 1-3% at the speed of 1-3L / min at the same time till the pH is 9 and the solution is clear and transparent, filtering, heating the sodium salt solution to 25-95 DEG C till a clear and transparent state is achieved, dropwise adding a sulfuric acid solution with the weight concentration of 5-10% to neutralize till the pH is 5-7, filtering, dewatering, washing and drying the solid to obtain the finished product MBT. The method disclosed by the invention has the advantages that the method is simple in process and easy in industrialization; the purity of the prepared high content MBT is up to more than 99%.

Description

technical field [0001] The invention relates to a method for purifying rubber vulcanization accelerator 2-mercaptobenzothiazole (MBT), which belongs to the technical field of rubber vulcanization accelerator MBT purification. Background technique [0002] With the development of the rubber industry, people pay more and more attention to the research and production of vulcanization accelerators. Vulcanization accelerator plays a very important role in the rubber vulcanization process. It can greatly accelerate the reaction between rubber and vulcanizing agent, improve productivity, and at the same time improve the physical and mechanical properties of vulcanized rubber. MBT is an indispensable one in the rubber industry. main accelerator. [0003] Usually, the impurities in the accelerator are mainly resin and intermediate products (such as benzothiazole), and the existence of impurities makes the product quality not high. Literature (Fine Chemical Raw Materials and Interme...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D277/72
CPCC07D277/72
Inventor 周福朋朱国旭杨春霞鲍翠张凤丽
Owner SHANDONG SUNSINE CHEM
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