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Electrolytic oxidation preparation method of sulfenamide accelerator

A sulfenamide, electrolytic oxidation technology, applied in the electrolysis process, electrolysis components, electrolytic organic production and other directions, can solve the problems of difficult to achieve green cleaning, difficult environmental protection, equipment corrosion, etc., to simplify the production process and reduce production costs. , the effect of saving energy

Inactive Publication Date: 2016-05-04
WILLING NEW MATERIALS TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This process uses a large amount of oxidant in the production process, which seriously corrodes the equipment, and produces a large amount of wastewater, about 5-8 tons of wastewater per ton of product, which brings great difficulties to environmental protection and it is difficult to achieve "green cleaning" "Production

Method used

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  • Electrolytic oxidation preparation method of sulfenamide accelerator

Examples

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Embodiment 1

[0021] An electrolytic oxidation preparation method of N-tert-butyl-2-benzothiazole sulfenamide, comprising the following steps:

[0022] (1) Adding 100ml concentration of 4.7mol / L sodium chloride solution and 60ml chloroform to the electrolytic cell, then adding 0.04mol2-mercaptobenzothiazole and 0.36mol tert-butylamine to the electrolytic cell, after stirring and mixing evenly, put Put platinum anode and stainless steel net negative electrode, under agitation constant current electrolysis, when passing electricity is 4F / mol, stop reaction; Wherein, the current density of described constant current electrolysis is 30mA / cm 2 ;

[0023] (2) The reaction solution is left to stand until the two phases are completely separated, the aqueous phase and the organic phase are separated, and the recovered aqueous phase solution is recycled. At the same time, the organic phase solution is washed with water, and the organic phase solution is recovered after washing, and then the recovered...

Embodiment 2

[0026] An electrolytic oxidation preparation method of N-tert-butyl-2-benzothiazole sulfenamide, comprising the following steps:

[0027] (1) Add 100ml of sodium chloride solution and 60ml of carbon tetrachloride with a concentration of 4.7mol / L in the electrolytic cell, then add 0.04mol2-mercaptobenzothiazole and 0.4mol tert-butylamine in the electrolytic cell, after stirring and mixing , put into the titanium-based metal oxide coating anode and the stainless steel mesh cathode, and perform constant current electrolysis under stirring. When the electricity passing through is 5F / mol, stop the reaction; wherein, the current density of the constant current electrolysis is 40mA / cm 2 ;

[0028] (2) The reaction solution is left to stand until the two phases are completely separated, the aqueous phase and the organic phase are separated, and the recovered aqueous phase solution is recycled. At the same time, the organic phase solution is washed with water, and the organic phase sol...

Embodiment 3

[0031] An electrolytic oxidation preparation method of N-tert-butyl-2-benzothiazole sulfenamide, comprising the following steps:

[0032] (1) adding 100ml concentration in the electrolytic cell is 4.7mol / L sodium chloride solution and 60ml carbon tetrachloride, then in the electrolytic cell, add 0.04mol2-mercaptobenzothiazole and 0.32mol tert-butylamine, after stirring and mixing, Put a titanium-based metal oxide coating anode and a stainless steel mesh cathode, and perform constant current electrolysis under stirring. When the electricity passing through is 4F / mol, stop the reaction; wherein, the current density of the constant current electrolysis is 30mA / cm 2 ;

[0033] (2) The reaction solution is left to stand until the two phases are completely separated, the aqueous phase and the organic phase are separated, and the recovered aqueous phase solution is recycled. At the same time, the organic phase solution is washed with water, and the organic phase solution is recovered...

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Abstract

The invention discloses an electrolytic oxidation preparation method of a sulfenamide rubber vulcanization accelerator. The electrolytic oxidation preparation method comprises the following steps that 1, 100 ml of an electrolyte solution and 60 ml of an organic solvent are added into an electrolytic cell, then corresponding reacting raw materials are added into the electrolytic cell according to the molar ratio of benzothiazyl disulfide or 2-benzothiazolethiol to amine or morpholine of 1:(8-10), after the raw materials are stirred and mixed evenly, an anode and a cathode are put in the electrolytic cell, constant-current electrolysis is carried out while stirring is carried out, and the reaction is stopped when the passing electric quantity is 3-5 F / mol; and 2, reaction liquid is subjected to standing till two phases are completely separated, the water phase and the organic phase are separated, an organic phase solution is washed with water and is recycled after being washed, then the recycled organic phase solution is distilled, smashed, sieved and packaged, and the corresponding finished sulfenamide rubber vulcanization accelerator is obtained. According to the preparation method, the production process is simple, cleanliness and environment friendliness are achieved, and the obtained product is high in yield and purity.

Description

technical field [0001] The invention belongs to the technical field of rubber vulcanization accelerator preparation, and in particular relates to an electrolytic oxidation preparation method of a sulfenamide accelerator. Background technique [0002] Since the 1980s, my country's rubber additives industry has been developing continuously, healthily and steadily. Especially in recent years, the rapid development of the domestic automobile industry and communication industry has driven the rapid growth of the rubber processing industry and given the development of the rubber additives industry. An unprecedented good opportunity has been provided. However, although the production of rubber accelerators in my country has been greatly improved, compared with developed countries in the world, there is still a big gap in product intrinsic quality and "green" environmental protection technology. China's additive industry will expand the market share of green and non-toxic products, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25B3/02C25B3/23
CPCC25B3/23
Inventor 丁俊杰王志强郭同新高新端屈军伟李宏喜宋风朝王飞钱娟娟
Owner WILLING NEW MATERIALS TECH CO LTD