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Preparation method and synthesis system of N-tert-butyl-2-benzothiazole sulfenamide

A technology of benzothiazole sulfenamide and mercaptobenzothiazole, which is applied in the field of materials and can solve problems such as equipment corrosion and the use of oxidants

Pending Publication Date: 2022-03-01
WILLING NEW MATERIALS TECH CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The first object of the present invention is to provide a kind of preparation method of N-tert-butyl-2-benzothiazole sulfenamide, to solve the problem of using a large amount of oxidant in the process of producing NS existing in the prior art, serious corrosion to equipment, Technical Problems in Generating Large Volumes of Saline Wastewater

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  • Preparation method and synthesis system of N-tert-butyl-2-benzothiazole sulfenamide
  • Preparation method and synthesis system of N-tert-butyl-2-benzothiazole sulfenamide

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preparation example Construction

[0051] In the first aspect, the present invention provides a method for preparing N-tert-butyl-2-benzothiazole sulfenamide, the reaction equation is as follows figure 1 shown, including the following steps:

[0052] a. Mix tert-butylamine, mother liquor, 2-mercaptobenzothiazole and catalyst to obtain a mixed solution. In the step a, there is no specific limitation on the way of mixing, as long as it can achieve sufficient mixing of each substance, for example, stirring can be used for mixing.

[0053] b. The mixed solution obtained in step a and oxygen are mixed and reacted in a membrane dispersion micro-mixer. Membrane dispersion micro-mixer is a membrane dispersion micro-reactor, a micro-reactor formed by utilizing the characteristics of many microporous structures of the membrane, which is conducive to the efficient mixing of the mixed solution and oxygen, and the reaction is sufficient.

[0054] c. Aging the solution after the b step reaction, so that the insufficiently ...

Embodiment 1

[0093] The preparation method of N-tert-butyl-2-benzothiazole sulfenamide, the preparation process is as follows figure 2 As shown, the steps are as follows:

[0094] First, tert-butylamine and water are prepared in a certain proportion into a 20% tert-butylamine aqueous solution, and then a certain amount of M (the molar ratio of M to tert-butylamine is 1:2) and sulfonated cobalt phthalocyanine (sulfonated cobalt phthalocyanine and The mass ratio of M is 1:10000), stirred at a temperature of 20° C. for 10 min to obtain a mixed solution of M-tert-butylamine. M-tert-butylamine and liquid oxygen are mixed at a molar ratio of 1:0.25 through a membrane dispersion micro-mixer, stay at 50°C for 2s (the average pore size of the membrane is 10um, the thickness is 0.1mm, and the porosity is 10%), and enter the packing aging tower at React at 30°C for 10 minutes, filter and dry (at a temperature of 70°C for 12 hours), and finally obtain an off-white finished product. The yield of the...

Embodiment 2

[0096] The preparation method of N-tert-butyl-2-benzothiazole sulfenamide, the steps are as follows:

[0097] First, tert-butylamine and water are prepared in a certain proportion into an aqueous solution of tert-butylamine with a mass fraction of 50%, and then a certain amount of M (the molar ratio of M to tert-butylamine is 1:6), sulfonated cobalt phthalocyanine (sulfonated cobalt phthalocyanine and The mass ratio of M is 1:8000), stirred at a temperature of 50° C. for 30 min to obtain a mixed solution of M-tert-butylamine. M-tert-butylamine and liquid oxygen are mixed at a molar ratio of 1:0.25 through a membrane dispersion micro-mixer, stay at 80°C for 30s (the average pore diameter of the membrane is 50um, the thickness is 0.3mm, and the porosity is 30%), and enter the packing aging tower at React at 80°C for 20 minutes, filter and dry (at a temperature of 80°C for 10 hours), and finally obtain an off-white finished product. The yield of the product is 98.6%, the initial...

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Abstract

The invention provides a preparation method of N-tert-butyl-2-benzothiazole sulfenamide and a synthesis system of the N-tert-butyl-2-benzothiazole sulfenamide, and relates to the technical field of materials. The preparation method of the N-tert-butyl-2-benzothiazole sulfenamide provided by the invention comprises the following steps: a, mixing tert-butylamine, a mother solution, 2-mercaptobenzothiazole and a catalyst to obtain a mixed solution; b, mixing and reacting the mixed solution obtained in the step a and oxygen in a membrane dispersion micro-mixer; and c, sequentially aging and filtering the solution after the reaction in the step b to prepare the N-tert-butyl-2-benzothiazole sulfenamide. The method has the advantages that a reaction byproduct is water, and oxygen oxidation is free of byproducts, so that environmental protection is facilitated; according to the technical scheme, the mother liquor and the catalyst can be repeatedly used; the effective utilization rate of oxygen in the reaction system is close to 100%; according to the technology disclosed by the invention, a continuous process for synthesizing the N-tert-butyl-2-benzothiazole sulfenamide is realized.

Description

technical field [0001] The invention relates to the field of material technology, in particular to a preparation method of N-tert-butyl-2-benzothiazole sulfenamide and a synthesis system thereof. Background technique [0002] NS (N-tert-butyl-2-benzothiazole sulfenamide) is the main product of sulfenamides, which has the advantages of fast vulcanization speed, short vulcanization time, excellent scorch resistance and safe processing. The most ideal accelerator for rubber, butadiene rubber, isoprene rubber, and radial tires. It does not produce amine nitrite after decomposition, and has no carcinogenic problems to the human body. It is called an environmentally friendly accelerator in the industry and is a product with great development prospects. [0003] At present, the synthesis method of NS is to use accelerator M (2-mercaptobenzothiazole) as raw material, carry out catalytic oxidation in oxygen atmosphere to generate intermediate accelerator DM, and then react accelerato...

Claims

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Application Information

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IPC IPC(8): C07D277/80
CPCC07D277/80
Inventor 章娟王飞高岩王志强郭同新邵明锐
Owner WILLING NEW MATERIALS TECH CO LTD
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