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Method for synthesizing thiofide NS by oxygen oxidation method

A vulcanization accelerator and a technology for synthesizing rubber, which is applied in the field of rubber vulcanization accelerator N-tert-butyl-2-benzothiazole sulfenamide, can solve the problems of low yield of accelerator NS, and achieve good product quality and low consumption. The effect of small amount and high yield

Inactive Publication Date: 2010-06-16
KEMAI CHEM
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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 NS

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 30 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 a reaction temperature of 40° C. and a stirring speed of 300 rpm, oxygen was introduced into the autoclave, and the reaction was carried out for 1 hour at a reaction pressure of 0.2 MPa. With a constant pressure injection pump, 21.3 grams of tert-butylamine with a mass percentage of 97% is added into the autoclave at a flow rate of 0.5 ml / min, and the reaction is continued until 0.2 hours after the oxygen flow is s...

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 a reaction temperature of 55° C. and a stirring speed of 600 rpm, oxygen was introduced into the autoclave, and the reaction was carried out for 3 hours at a reaction pressure of 0.5 MPa. With a constant pressure injection pump, 53.7 grams of tert-butylamine with a mass percentage of 99% is added in the autoclave at a flow rate of 2 ml / min, and the reaction is continued until 0.5 hours...

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 30 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 a reaction temperature of 70° C. and a stirring speed of 1000 rpm, oxygen was introduced into the autoclave, and the reaction was carried out for 5 hours under a reaction pressure of 0.7 MPa. With a constant pressure injection pump, 60.0 grams of tert-butylamine with a mass percentage of 99.5% is added into the autoclave at a flow rate of 3 ml / min, and the reaction is continued until 0...

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PUM

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Abstract

The invention discloses a method for synthesizing thiofide NS by an oxygen oxidation method. The method comprises the following steps of: adding promoter MBT and ammonia water in the molar ratio of 1:2-7 into a three-neck flask, dissolving and adding in a high-pressure oxidation kettle, dissolving the catalyst of copper sulfate with the ammonia water and adding into the high-pressure oxidation kettle, reacting at a temperature of 40-70 DEG C, introducing oxygen in the high-pressure oxidization kettle at a reaction pressure of 0.2-0.7MPa, adding tert-butylamine into the high-temperature oxidation kettle by using a constant-pressure sampling pump, reacting continuously for 0.2-0.7h after oxygen introduction, maintaining the pressure of the high-pressure oxidation kettle, stopping reaction; storing mother liquor into a sealed flask after filtering, preparing for reuse, washing and drying the product to obtain the thiofide NS with a product purity of above 98 percent. The invention has the advantages that the method has simple process and is easy to industrialized, the products have good quality and high yield as the mother liquor can be recycled and a small amount of tert-butylamine is consumed, and no three wastes are discharged in the synthesizing process.

Description

technical field [0001] The invention relates to a production method of rubber vulcanization accelerator N-tert-butyl-2-benzothiazole sulfenamide (NS), belonging to the technical field of rubber vulcanization accelerator NS 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. NS is an essential in the rubber industry. main accelerator. Accelerator NS has the functions of anti-scorch, safe, non-toxic, and fast vulcanization. The literature (Guangdong Chemical Industry, 2006, 5:16) reported the method of synthesizing NS by oxidation. Add accelerator M, tert-butylamine, di...

Claims

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Application Information

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IPC IPC(8): C07D277/80
Inventor 洪学斌尹红伟张超义
Owner KEMAI CHEM
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