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Method for preparing rubber accelerator MBTS

A rubber accelerator and temperature control technology, applied in the direction of organic chemistry, can solve the problems of difficult to meet special industry requirements, low MBTS quality, low added value of products, etc., achieve good application prospects, easy control of the end point, and reuse of mother liquor Effect

Pending Publication Date: 2020-01-17
内蒙古科迈化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the above oxidants have their own advantages, the preparation process all produces a large amount of waste water, which is easy to pollute the environment; especially the oxidation synthesis of MBTS by chlorine gas method, the resulting product quality is poor, and chlorine gas is highly toxic, which is more serious to environmental pollution.
[0004] In addition, the quality of the MBTS prepared by the above-mentioned method is not high. The melting point of the obtained product is generally below 170°C, the purity is only 96-97%, the added value of the product is low, and it is difficult to meet the requirements of special industries.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] (1) Mix industrial-grade MBT and 75% ethanol solution in the oxidation kettle, control the mass ratio of MBT and ethanol to be 1:12, heat up to 45°C, stir for 0.8h to dissolve MBT;

[0032] (2) Pass into hydrogen peroxide and carry out oxidation, control the mass ratio of hydrogen peroxide and MBT to be 1:150, centrifuge after oxidation completes;

[0033] (3) Continue to add hydrogen peroxide to the solution obtained by centrifugation in step (2), control the mass ratio of hydrogen peroxide and MBT to 1:10, then control the temperature to 0°C, stir for 0.5h and carry out crystallization and separation, and obtain wet material after separation MBTS and ethanol mother liquor, dry the wet material MBTS to obtain the MBTS product, and the gained mother liquor can be returned to the step (1) to dissolve MBT;

[0034] (4) After the mother liquor described in step (3) is recycled for 12 times, the mother liquor is distilled to recover ethanol to obtain a concentration of 90% ...

Embodiment 2

[0037] (1) Mix industrial-grade MBT and 55% ethanol solution in the oxidation kettle, control the mass ratio of MBT and ethanol to be 1:20, heat up to 70°C, stir for 0.5h to dissolve MBT;

[0038] (2) Pass into hydrogen peroxide and carry out oxidation, control the mass ratio of hydrogen peroxide and MBT to be 1:100, centrifuge after oxidation completes;

[0039] (3) Continue to add hydrogen peroxide to the solution obtained in step (2), control the mass ratio of hydrogen peroxide and MBT to 0.9:10, then control the temperature to 0°C, and carry out crystallization and separation after stirring for 1 hour. After the separation is completed, the wet material MBTS and Ethanol mother liquor, dry the wet material MBTS to obtain the MBTS product, and the mother liquor of the gained can be returned to the step (1) to dissolve MBT;

[0040] (4) After the mother liquor described in step (3) is recycled for 10 times, the mother liquor is distilled to recover ethanol to obtain a concent...

Embodiment 3

[0043] (1) Mix industrial-grade MBT and 90% ethanol solution in an oxidation kettle, control the mass ratio of MBT and ethanol to be 1:10, heat up to 70°C, and stir for 0.75h to dissolve MBT;

[0044] (2) Pass into hydrogen peroxide and carry out oxidation, control the mass ratio of hydrogen peroxide and MBT to be 1:150, centrifuge after oxidation completes;

[0045] (3) Continue to add hydrogen peroxide to the solution obtained by centrifugation in step (2), control the mass ratio of hydrogen peroxide and MBT to 1:10, then control the temperature to 0°C, stir for 0.75h and carry out crystallization and separation, and obtain wet material after separation MBTS and ethanol mother liquor, dry the wet material MBTS to obtain the MBTS product, and the gained mother liquor can be returned to the step (1) to dissolve MBT;

[0046] (4) After the mother liquor described in step (3) is recycled for 15 times, the mother liquor is distilled to reclaim ethanol to obtain a concentration of...

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Abstract

The invention relates to a method for preparing rubber accelerator MBTS, and the method comprises the following steps: dissolving industrial MBT in ethanol, introducing hydrogen peroxide for oxidation, controlling the mass ratio of hydrogen peroxide to MBT to be 1: (100-200), and separating solid from liquid after oxidation is completed; then continuously adding hydrogen peroxide into the solutionobtained by separation, wherein the mass ratio of hydrogen peroxide to MBT is controlled to be (0.9-1.1): 10, and crystallizing and separating to obtain the MBTS product. According to the invention,firstly, the industrial MBT is refined by utilizing the synergistic effect of ethanol dissolution and hydrogen peroxide oxidation, and then hydrogen peroxide is added for deep oxidation to obtain a high-quality MBTS product with a melting point of more than 178 DEG C and a purity of more than 99%, which can meet the requirements of various industries, and the method has good application prospect and is suitable for industrial popularization.

Description

technical field [0001] The invention relates to the technical field of chemical industry, in particular to a production process of a rubber accelerator, in particular to a method for preparing the rubber accelerator MBTS. Background technique [0002] The rubber accelerator dibenzothiazole disulfide (MBTS) plays a very important role in the rubber vulcanization process. Adding it to the rubber compound can promote the activation of the vulcanizing agent, thereby accelerating the cross-linking reaction between the vulcanizing agent and the rubber molecule. The practical effects of shortening vulcanization time, lowering vulcanization temperature, increasing output and reducing production cost are achieved. [0003] MBTS is an indispensable additive in the rubber accelerator industry. The current mainstream synthetic method is to use industrial-grade synthetic MBT as raw material and oxidize it with an oxidant. Among them, the main oxidizing agents are nitrous acid, oxygen, c...

Claims

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Application Information

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IPC IPC(8): C07D277/78
CPCC07D277/78
Inventor 田少华鞠光史军张毅
Owner 内蒙古科迈化工有限公司
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