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Method for producing rubber vulcanization accelerator NS by two-dropping method

A technology for rubber vulcanization and accelerators, which is applied in the production of rubber vulcanization accelerator NS and rubber vulcanization accelerator N-tert-butyl-2-benzothiazole sulfenamide by two-drop method, which can solve the problem of low yield of accelerator NS and other issues, to achieve the effect of simple process

Inactive Publication Date: 2015-04-29
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

[0008] Get 75 grams of tert-butylamine and join in the reaction kettle, under the condition of 40 ℃ and rotating speed of 600 rpm, with a flow rate of 2ml / min, add accelerator mass content 85% M50g, isopropanol 75g slurry, simultaneously with The flow rate of 1ml / min is added the oxidizing agent sodium hypochlorite that available chlorine is 16mg / 100ml, and dropwise time is 2.0 hours, judges reaction terminal point with starch potassium iodide test paper, when test paper turns black, stop adding sodium hypochlorite dropwise. After the reaction is completed, suction filtration, water washing, filtration, and drying are used to obtain the rubber accelerator NS product. The purity of the accelerator NS reaches more than 98.7%, and the yield reaches 95.2%.

Embodiment 2

[0010] Get 75 grams of tert-butylamine and join it in the reaction kettle. Under the conditions of 50° C. and a rotating speed of 600 rpm, with a flow rate of 2 ml / min, add accelerator mass content 87% M50g, isopropanol 75g slurry, and simultaneously The flow rate of 1ml / min is added the oxidizing agent sodium hypochlorite that available chlorine is 17mg / 100ml, and dropwise time is 2.0 hours, judges reaction terminal point with starch potassium iodide test paper, when test paper turns black, stops dripping sodium hypochlorite. After the reaction is completed, suction filtration, water washing, filtration, and drying are used to obtain the rubber accelerator NS product. The purity of the accelerator NS reaches more than 98.8%, and the yield reaches 95.3%.

Embodiment 3

[0012] Get 75 grams of tert-butylamine and join in the reaction kettle, under the condition of 60°C and rotating speed of 600 rpm, with a flow rate of 2ml / min, add accelerator mass content 90% M50g, isopropanol 75g slurry, simultaneously with The flow rate of 1ml / min is added the oxidizing agent sodium hypochlorite that available chlorine is 18mg / 100ml, and dropwise time is 2.0 hours, judges reaction terminal point with starch potassium iodide test paper, when test paper turns black, stop adding sodium chlorate dropwise. After the reaction is completed, suction filtration, water washing, filtration, and drying are used to obtain the rubber accelerator NS product. The purity of the accelerator NS reaches more than 98.9%, and the yield reaches 95.4%.

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Abstract

The invention discloses a method for producing a rubber vulcanization accelerator NS by a two-dropping method. The method comprises the following steps: adding tert-butylamine into an oxidation kettle according to the weight ratio of M with mass content of 85%-90% to tert-butylamine of 1: 1.5, dropping slurry of an accelerator M and isopropanol in the mass ratio of 1: 1.5 at the flow rate of 2ml / min under the conditions that the temperature is 40-60 DEG C and the rotational speed is 600 revolutions / min, simultaneously dropping a sodium hypochlorite solution containing 16-18mg / 100ml of available chlorine into a solution at the flow rate of 1ml / min, judging a reaction terminal point with starch-potassium iodide test paper after 90 minutes, stopping the dropping of sodium hypochlorite when the test paper becomes black, and performing suction filtration, water washing, filtration and drying to obtain a rubber accelerator NS product. The method is simple in process, an M purification process step is omitted, isopropanol is used to replace water, production waste water is reduced by above 60% in comparison with a relatively old process, the purity of the synthesized accelerator NS is above 98%, and the yield is above 95%.

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. In particular, it relates to a method for producing rubber vulcanization accelerator NS by two-drop method. 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 sa...

Claims

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Application Information

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IPC IPC(8): C07D277/80
CPCC07D277/80
Inventor 李树东
Owner KEMAI CHEM
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