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Method for synthesizing rubber vulcanization accelerator DM by oxygen oxidization

A technology of vulcanization accelerator and synthetic rubber, applied in the direction of organic chemistry, etc., can solve the problems of low DM yield, etc., and achieve the effects of high yield, simple process and good product quality

Active Publication Date: 2010-06-02
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

This method has a low yield of accelerator DM

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0008] Condensation reaction of aniline with carbon disulfide and sulfur at 270-280°C and pressure of 9-10MPa produces MBT with a mass content of 92%, and after purification, 95% MBT is obtained. Add 50 grams of MBT and 97 grams of 10% ammonia water into a three-necked flask, and dissolve them at a temperature of 35° C. and a stirring speed of 20 rpm. When all the MBT is dissolved, the solution is added to the autoclave. Dissolve 0.04 g of catalyst copper sulfate with 10 g of 10% ammonia water by mass percentage, and add it to the autoclave. Under the conditions of the reaction temperature of 40°C and the stirring speed of 300 rpm, oxygen was introduced into the autoclave, and the reaction was carried out at a reaction pressure of 0.2 MPa for 3 hours until 0.2 hours after the oxygen supply was stopped. If the pressure in the kettle remains constant, the reaction will reach the end point. After the reaction is completed, the product is washed with water and dried to obtain th...

example 2

[0010] Condensation reaction of aniline with carbon disulfide and sulfur at 270-280°C and pressure of 9-10MPa produces MBT with a mass content of 92%, and after purification, 97% MBT is obtained. 50 grams of MBT and 123 grams of ammonia water with a mass percentage of 20% were added into a three-necked flask, and dissolved at a temperature of 40° C. and a stirring speed of 30 rpm. When all the MBT is dissolved, the solution is added to the autoclave. Dissolve 0.16 g of catalyst copper sulfate with 15 g of 20% ammonia water by mass percentage, and add it to the autoclave. Under the conditions of the reaction temperature of 55°C and the stirring speed of 600 rpm, oxygen was introduced into the high-pressure oxidation kettle, and the reaction was carried out at a reaction pressure of 0.5 MPa for 4 hours, until 0.5 hours after the oxygen flow was stopped, the high-pressure oxidation If the pressure in the kettle remains constant, the reaction will reach the end point. After the ...

example 3

[0012] Condensation reaction of aniline with carbon disulfide and sulfur at 270-280°C and pressure of 9-10MPa produces MBT with a mass content of 92%, and after purification, 99% MBT is obtained. 50 grams of MBT and 126 grams of ammonia water with a mass percentage of 25% were added into a three-necked flask, and dissolved at a temperature of 45° C. and a stirring speed of 40 rpm. When all the MBT is dissolved, the solution is added to the autoclave. Dissolve 0.28 g of catalyst copper sulfate with 20 g of 25% ammonia water by mass percentage, and add it to the autoclave. Under the conditions of the reaction temperature of 70°C and the stirring speed of 700 rpm, oxygen was introduced into the autoclave, and the reaction was carried out at a reaction pressure of 0.7 MPa for 5 hours until 0.7 hours after the oxygen supply was stopped. If the pressure in the kettle remains constant, the reaction will reach the end point. After the reaction is completed, the product is washed wit...

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PUM

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Abstract

The invention discloses a method for synthesizing rubber vulcanization accelerator DM by oxygen oxidization. The process of the method comprises: adding a 95 to 99 mass percent accelerator MBT and a 10 to 25 mass percent aqueous ammonia into a three-neck flask in a molar ratio of 1:2-7 to dissolve the 95 to 99 mass percent accelerator MBT under the conditions of a temperature of 35 to 45 DEG C and a stirring speed of 10 to 100 r / min; after the MBT dissolves completely, adding the solution into a high-pressure oxidizing kettle; dissolving a copper sulfate catalyst in 10 to 20 grams of 10 to 25 mass percent of aqueous ammonia (the molar ratio of the catalyst to the MBT is 0.001-0.007:1) and adding the solution into the high-pressure oxidizing kettle; introducing oxygen into the high-pressure oxidizing kettle under the conditions of a reaction temperature of 40 to 70 DEG C and a stirring speed of 300 to 1,000 r / min to perform reaction for 1 to 5 hours under a condition of a reaction pressure of 0.2 to 0.7MPa till 0.2 to 0.7 hour after the oxygen introduction is stopped, wherein if the pressure in the high-pressure oxidizing kettle keeps constant, the reaction is finished; after the reaction is finished, reducing the pressure in the high-pressure oxidizing kettle to normal pressure; washing and drying the product to obtain a rubber vulcanization accelerator DM product; and distilling mother solution to recycle the aqueous ammonia. The purity of the product is up to over 98 percent. The invention has the advantages that: the method is simple in process and easy to industrialize; due to the recycling of the aqueous ammonia, the product has high quality and yield; and the synthesis process is free from the discharge of 'three wastes'.

Description

technical field [0001] The invention relates to a new production method of a rubber vulcanization accelerator dibenzothiazole disulfide (DM), which belongs to the technical field of rubber vulcanization accelerator DM production. 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. DM is an essential in the rubber industry. main accelerator. Literature (Advances in Fine Petrochemical Industry, 2006, 7:35) reported a method for synthesizing DM by means of molecular oxidation reaction. Put a certain amount of M-Na salt and isopropanol into the reactor and stir, add dropwise a mixture...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D277/78
Inventor 洪学斌尹红伟张超义
Owner 内蒙古科迈化工有限公司
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