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Method for synthesizing sulfenamide-like accelerator TBBS by using solvent purification method rubber accelerator M

A technology of rubber accelerator and sulfenamide, which is applied in the field of rubber accelerator M to synthesize sulfenamide accelerator TBBS by solvent purification method, so as to reduce the generation of dried sludge, stabilize various indicators, and realize clean and civilized production Effect

Inactive Publication Date: 2017-12-22
QINGDAO AUX CHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] Purpose of the invention: In order to overcome the defects of the prior art, the present invention provides a method for the synthesis of sulfenamide accelerator TBBS by solvent purification method rubber accelerator M, improves product quality index, reduces raw material and energy consumption level and can solve waste water, solid waste , Odor pollutants treatment problems

Method used

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  • Method for synthesizing sulfenamide-like accelerator TBBS by using solvent purification method rubber accelerator M
  • Method for synthesizing sulfenamide-like accelerator TBBS by using solvent purification method rubber accelerator M
  • Method for synthesizing sulfenamide-like accelerator TBBS by using solvent purification method rubber accelerator M

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Embodiment

[0029] 1. Determine the best production process conditions through the following experiments:

[0030] (1) The influence of raw material ratio on product quality and yield

[0031] When the reaction temperature is controlled at 40-60°C and the reaction time is 2.0-3.0 hours, the influence of the raw material ratio on the product quality and yield is tested

[0032]

[0033] Note: The dual oxidant system is used, and the amount of sodium hypochlorite used is subject to the end point detection.

[0034] According to the analysis of experimental data, when the molar ratio of M and tert-butylamine is 1:1.5, the appearance of the product is light yellow, and the yield and melting point are all on the low side. With the decrease of the molar ratio of M and tert-butylamine, the appearance, yield and melting point are all improved. When the tert-butylamine is too much, because the product is dissolved in the tert-butylamine solution, the yield is reduced, and the post-treatment re...

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Abstract

The invention discloses a method for synthesizing sulfenamide-like accelerator TBBS (N-cyclohexyl-2-benzothiazolylsulfenamide) by using a solvent purification method rubber accelerator M. The accelerator TBBS is synthesized by using the rubber accelerator M and tert-butylamine as raw materials, by using hydrogen peroxide and sodium hypochlorite as oxidants and by using sulfuric acid as a catalyst; and the method comprises the following optimal production process conditions: (1) a molar ratio of the rubber accelerator M to the tert-butylamine is 1:2.4; and a molar ratio of the rubber accelerator M to the hydrogen peroxide to the sodium hypochlorite is 1:0.6:(0.55-0.65); (2) a reaction temperature is 55-60 DEG C; and (3) reaction time is 2.0-3.0h. The method disclosed by the invention comprehensively solves a technical problem of synthesizing the sulfenamide-like accelerator TBBS by using the solvent purification method rubber accelerator M, product quality indexes are higher than Chinese standard levels, consumption indexes achieve industry relatively-low standards, and the method solves treatment problems of pollutants including wastewater, solid waste and cacosmia.

Description

technical field [0001] The invention belongs to chemical technology, in particular to a method for synthesizing a sulfenamide accelerator TBBS from a rubber accelerator M by a solvent purification method. Background technique [0002] Rubber accelerator M (chemical name is 2-thiobenzothiazole) itself is an important rubber accelerator and an important intermediate for the synthesis of other accelerators. It has excellent vulcanization accelerator performance and is widely used. The largest amount, it is the precursor for the synthesis of other post-effect accelerators (such as thiazole accelerators, sulfenamide accelerators), such as rubber accelerators DM, MZ, CBS (CZ), TBBS (NS), NOBS, DZ, etc. etc. are derived from the parent M. [0003] The most widely used purification process for the production of rubber accelerator M is the acid-base method, which produces a large amount of wastewater (20 tons of wastewater per ton of product). Moreover, the wastewater has the chara...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D277/80
CPCC07D277/80
Inventor 刘凤轩陈学良周永红
Owner QINGDAO AUX CHEM
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