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Method for synthesizing rubber vulcanization accelerator NS (N-tertiary butyl-2-benzothiazole sulfenamide) through two-step method by taking hydrogen peroxide as oxidant

A technology of vulcanization accelerator and synthetic rubber, which is applied in the direction of organic chemistry, can solve the problem of low yield of accelerator NS, and achieve the effect of eliminating the recycling process, simple process, and easy industrialization

Inactive Publication Date: 2012-12-26
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

Embodiment 1

[0009] The first step takes by weighing 80g of 98% sulfuric acid, configures it into 20% sulfuric acid, and adds it to a reaction kettle with 60 grams of tert-butylamine, and makes sulfuric acid fully react with tert-butylamine at 40°C and a rotating speed of 600 rpm. , and then drop 105ml of M-Na salt with a density of 1.5g / ml to generate M-tert-butylamine salt.

[0010] The second step is to add 360ml of oxidant hydrogen peroxide with a mass content of 12.0% at a flow rate of 3ml / min, and the dropwise addition time is 2.0 hours. After the reaction is completed, the rubber accelerator NS product is obtained by suction filtration, water washing, filtration, and drying. The purity of the accelerator NS Reach more than 99%, yield has reached 97.1%.

Embodiment 2

[0012] The first step takes by weighing 80g of 98% sulfuric acid, configures it into 20% sulfuric acid, and adds it to a reaction kettle with 60 grams of tert-butylamine, and makes sulfuric acid fully react with tert-butylamine at 40°C and a rotating speed of 600 rpm. , and then drop 105ml of M-Na salt with a density of 1.5g / ml to generate M-tert-butylamine salt.

[0013] The second step is to add 360ml of oxidant hydrogen peroxide with a mass content of 15.0% at a flow rate of 3ml / min, and the dropwise addition time is 2.0 hours. After the reaction is completed, suction filter, wash with water, filter, and dry to obtain rubber accelerator NS products. The purity reached more than 99%, and the yield reached 97.4%.

Embodiment 3

[0015] The first step takes by weighing 80g of 98% sulfuric acid, configures it into 20% sulfuric acid, and adds it to a reaction kettle with 60 grams of tert-butylamine, and makes sulfuric acid fully react with tert-butylamine at 40°C and a rotating speed of 600 rpm. , and then drop 105ml of M-Na salt with a density of 1.5g / ml to generate M-tert-butylamine salt.

[0016] The second step is to add 360ml of oxidant hydrogen peroxide with a mass content of 18.0% at a flow rate of 3ml / min, and the dropwise addition time is 2.0 hours. After the reaction is completed, the rubber accelerator NS product is obtained by suction filtration, water washing, filtration, and drying. The purity of the accelerator NS Reach more than 99%, yield has reached 97.5%.

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Abstract

The invention discloses a method for synthesizing rubber vulcanization accelerator NS (N-tertiary butyl-2-benzothiazole sulfenamide) through a two-step method by taking hydrogen peroxide as an oxidant. The method comprises the following steps of: (1) weighing 80 g of 98 percent sulfuric acid, preparing 20 percent of sulfuric acid, adding in a reaction kettle with 60 g of tert-butylamine, fully reacting the sulfuric acid with the tert-butylamine under the conditions of 40 DEG C and rotation speed of 600 rpm and dropwise adding 105 ml of M-Na salt with density of 1.5 g / ml to produce M-tert-butylamine salt; and (2) adding 360 ml of oxidant hydrogen peroxide with mass content of 12.0-18.0 percent according to a flow speed of 3 ml / min, wherein the dropwise adding time is 2.0 hours, and performing suction filtration, washing, filtration and drying after reaction to obtain the rubber vulcanization accelerator NS product. The method has the advantages of simple process, use of the environment-friendly hydrogen peroxide as the oxidant, easiness in industrialization, proper amount of the used tert-butylamine, capability of saving acidification, spin-drying and drying steps of an M workshop, high yield of synthesized NS and high quality.

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, NS is suitable for NR, SBR, BR and their mixtures. It has fast vulcanization speed and high vulcanized rubber modulus. It can be used alone or in combination with a small amount of super speed accelerator in the formula of tires or rubber industrial products. Accelerator NS has the functions of anti-scorch, safe, non-toxic, and fast vulcanization. Literature (Guangdong Chemical Industry, 2006, 5:16) reported the method of oxidation synthesis of NS. Add accelerator M, tert-butylamine, dilute sulfuric acid, water, etc. into the reactor and stir to make it into a salt; use hydrogen peroxide as an oxidant to react, cool down, filter with suction, wash with water, filter, an...

Claims

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Application Information

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IPC IPC(8): C07D277/80
Inventor 朱军
Owner KEMAI CHEM
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