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Preparation method of rubber vulcanization accelerator n-tert-butyl-2-benzothiazole sulfenamide (ns)

A technology of benzothiazole sulfenamide and dibenzothiazole disulfide is applied in the field of preparation of rubber vulcanization accelerators, and can solve the problems of large discharge of organic waste water, low product yield and quality, reduced reaction selectivity and the like, To achieve the effect of reducing the amount of wastewater treatment, less variety of materials, and short production cycle

Active Publication Date: 2017-02-15
WILLING NEW MATERIALS TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The problem with this method is that the process is complicated, the amount of auxiliary raw materials is large, and the reactant chlorine gas is a corrosive and highly toxic gas, and sodium hydroxide is a strong alkali, which not only requires high equipment, but also causes quite serious damage to the environment. Pollution, high production costs, and at the same time, it is difficult to avoid excessive oxidation of products, resulting in reduced reaction selectivity, low product yield and quality
In this method, there are few types of raw materials and simple equipment in the synthesis, but the amount of solvent required is large, the cost is high, the reaction selectivity is not high, and the discharge of organic wastewater is relatively large.

Method used

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  • Preparation method of rubber vulcanization accelerator n-tert-butyl-2-benzothiazole sulfenamide (ns)

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Add 35ml of ammonia water in a 1L high-pressure reactor equipped with a temperature and pressure detection device and a permanent magnetic stirrer, and put in the reactant dibenzothiazole disulfide 33.25g (0.1mol), copper ammonia catalyst 0.12g and surfactant under strong stirring TW-20 0.005g, control the temperature to 20°C, feed oxygen to make the pressure 0.4MPa, add 16.09g of tert-butylamine within 2.5h, at this time, the temperature in the kettle rises, control the temperature to 40°C, react for 1.5h, absorb oxygen When it is rare, the reaction reaches the end and the stirring is stopped. The white precipitate is washed with water, dehydrated and dried to obtain the product. Its appearance is off-white. It is determined that the reaction yield is 96.2%. The product obtained after the reaction has an initial melting point of 106.3° C. and a purity of 98.6%.

Embodiment 2

[0042] Add 42ml of ammonia water in a 1L high-pressure reactor equipped with a temperature and pressure detection device and a permanent magnetic stirrer, and put in reactant dibenzothiazole disulfide 33.25g (0.1mol), copper ammonia catalyst 0.18g and surfactant under strong stirring TW-20 0.006g, control the temperature to 16°C, feed oxygen to make the pressure 0.6MPa, add 15.36g of tert-butylamine within 2h, at this time, the temperature in the kettle rises, control the temperature to 38°C, react for 1.5h, oxygen absorption is very When it is small, the reaction will reach the end, so stop stirring. The white precipitate is washed with water, dehydrated and dried to obtain the product. Its appearance is off-white. It is determined that the reaction yield is 95.8%. The product obtained after the reaction has a melting point of 106.8° C. and a purity of 98.9%.

Embodiment 3

[0044] Add 50ml of ammonia water to a 1L high-pressure reactor equipped with a temperature and pressure detection device and a permanent magnetic stirrer, and add 33.25g (0.1mol) of dibenzothiazole disulfide, 0.20g of cuproammonia catalyst and surfactant under strong stirring. TW-20 0.008g, control the temperature to 10°C, feed oxygen to make the pressure 0.5MPa, add 17.55g of tert-butylamine within 3.0h, at this time, the temperature in the kettle rises, control the temperature to 35°C, react for 2h, and absorb oxygen very quickly When it is small, the reaction will reach the end, so stop stirring. The white precipitate is washed with water, dehydrated and dried to obtain the product. Its appearance is white. It is determined that the reaction yield is 97.4%. The product obtained after the reaction has a melting point of 107.2° C. and a purity of 99.1%.

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Abstract

The invention provides a method for preparing rubber vulcanization accelerator N-tert-butyl-2-benzothiazole sulfenamide (NS), the specific process of which is as follows: 30-60ml of ammonia water is put in, under the oxygen pressure of 0.2-0.8MPa , Weigh 33.25g of dithiodibenzothiazole, 0.10-0.25g of cuproammonia catalyst and a very small amount of surfactant into the reaction kettle, slowly inject 15.36-19.02g of tert-butylamine using a metering pump, and generate the target at a reasonable reaction temperature product, after centrifugation, washing, drying and other processes, the desired product NS is obtained. The method of the present invention effectively reduces the amount of organic wastewater to be treated, and the overall cost is reduced. At the same time, the method has the advantages of less raw material varieties, high reaction selectivity, high yield, and short cycle, which is obviously superior to the current production method, and can be extremely Well meet the needs of the high-end market.

Description

[0001] 1. Technical field [0002] The invention belongs to the technical field of preparation of rubber vulcanization accelerators, in particular to a preparation method of rubber vulcanization accelerator N-tert-butyl-2-benzothiazole sulfenamide (NS). [0003] 2. Background technology [0004] In recent years, the toxicity of carcinogenic nitrosamines, which are easily produced by vulcanization accelerators in rubber processing, has been paid more and more attention internationally. After research, it was found that the production of nitrosamines is due to the use of accelerators containing secondary amine groups in the processing of rubber products. Common accelerators of this type are N-oxydiethylenebenzothiazole-2-sulfenamide (NOBS), N, N-diisopropyl-2-benzothiazole sulfenamide (DIBS) and N, N-dicyclohexyl-2-benzothiazole sulfenamide (DZ), etc., this is due to the preparation These accelerators all use secondary amine group raw materials such as morpholine, diisopropylami...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D277/80
Inventor 王志强郭同新李宏喜王飞宋风朝钱娟娟
Owner WILLING NEW MATERIALS TECH CO LTD
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