Method for directly extracting and purifying rubber vulcanization accelerator MBT granules by methylbenzene

A technology of rubber vulcanization and accelerator, applied in liquid solution solvent extraction, organic chemistry and other directions, can solve the problems of low product purity and long production cycle, and achieve the effect of high purity, short melting range and high melting point

Inactive Publication Date: 2010-06-02
KEMAI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Dissolve the crude MBT with sodium hydroxide solution, let stand and then filter to achieve the purpose of removing the resin, add dilute sulfuric acid to the filtrate to precipitate MBT, filter and wash to neutral to obtain refined MBT, this method has a long production cycle, And the product purity is low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0009] Condensation reaction of aniline with carbon disulfide and sulfur at 270-280°C and pressure of 9-10Mpa produces crude MBT with a mass content of 65%, and the remaining impurities include: resin 30% and intermediate product 5%. 100 grams, 65% by mass percentage of crude MBT is warming up to 200 DEG C, then passes through in the reactor that 20 DEG C, 100 milliliters of distilled water are housed, the MBT temperature is dropped to 30 DEG C rapidly, the water in the reactor is discharged, The obtained MBT particles were dried; 1000 ml of toluene was added into the reactor, heated to 40° C., extracted for 100 minutes at a stirring speed of 50 rpm, filtered and dried. At this time, 67.1 g of vulcanization accelerator MBT were obtained. The 2-mercaptobenzothiazole accelerator has a mass content of 96.2% and a melting point of 172.8°C.

example 2

[0011] The thick MBT used in this embodiment is the same as that in Embodiment 1. 200 grams, 65% by mass percentage of crude MBT is warming up to 230 DEG C, then passes through in the reactor that 30 DEG C, 1000 milliliters of distilled water are housed, the MBT temperature is rapidly dropped to 40 DEG C, the water in the reactor is discharged, The obtained MBT particles were dried; 5000 ml of toluene was added into the reactor, heated to 50° C., extracted for 150 minutes at a stirring speed of 100 rpm, filtered and dried. At this time, 133.2 g of vulcanization accelerator MBT were obtained. The 2-mercaptobenzothiazole accelerator has a mass content of 96.8% and a melting point of 173.4°C.

example 3

[0013] The thick MBT used in this embodiment is the same as that in Embodiment 1. With 500 grams, the thick MBT that mass percent is 65% is warming up to 250 ℃, passes in the reactor that 40 ℃, 2000 milliliters of distilled water are housed then, MBT temperature is dropped to 50 ℃ rapidly, the water in the reactor is discharged, The obtained MBT particles were dried; 8000 ml of toluene was added into the reactor, heated to 60° C., extracted for 200 minutes at a stirring speed of 150 rpm, filtered and dried. At this time, 332.1 g of vulcanization accelerator MBT were obtained. The 2-mercaptobenzothiazole accelerator has a mass content of 97.1% and a melting point of 173.8°C.

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Abstract

The invention discloses a method for directly extracting and purifying rubber vulcanization accelerator MBT granules by methylbenzene. The method comprises the following steps: heating 10-500g of rough MBT (impurities are mainly resin and intermediate products) the mass percentage of which is 40-70 percent to be at 200-250 DEG C, and than leading into a reactor with 100-2000ml of 20-50 DEG C distilled water, quickly cooling the MBT to 30-80 DEG C, discharging water out of the reactor and drying the obtained MBT granules; adding 1000-8000ml of methylbenzene in the reactor, heating to 40-60 DEG C, extracting for 50-200min at the stirring rate of 50-150 turns/min, filtering, drying and obtaining vulcanization accelerator MBT with content higher than 96 percent. The invention has the advantages that the method has simple process and easy industrialization and the obtained MBT has high purity and melting point and short melting range.

Description

technical field [0001] The invention relates to a new purification method of rubber vulcanization accelerator 2-mercaptobenzothiazole (MBT), belonging 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. 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 Intermediates,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D277/72C08K5/47C08L21/00B01D11/04
Inventor 洪学斌孙凤娟孟庆宝
Owner KEMAI CHEM
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