Method for using rubber accelerator M to synthesize sulfonamide accelerator CBS by solvent purification method

A technology of rubber accelerator and sulfenamides, which is applied in the field of solvent purification rubber accelerator M to synthesize sulfenamide accelerator CBS, to achieve the effect of reducing dried sludge, reducing CODcr, and strong repeatability

Inactive Publication Date: 2017-12-08
QINGDAO AUX CHEM
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  • Abstract
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  • 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 CBS 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 problem

Method used

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  • Method for using rubber accelerator M to synthesize sulfonamide accelerator CBS by solvent purification method
  • Method for using rubber accelerator M to synthesize sulfonamide accelerator CBS by solvent purification method
  • Method for using rubber accelerator M to synthesize sulfonamide accelerator CBS by solvent purification method

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Embodiment

[0028] 1. Determine the best production process conditions through the following experiments:

[0029] (1) The influence of raw material ratio on product quality and yield

[0030] When the reaction temperature is controlled at 35-40°C and the reaction time is 2.0-3.0 hours, the influence of the experimental raw material ratio on product quality and yield:

[0031]

[0032] Note: The dual oxidant system is used, and the amount of sodium hypochlorite used is subject to the end point detection.

[0033] According to experimental data analysis, when M and cyclohexylamine are in molar ratio of 1:1.8, the product appearance is light yellow, and yield, fusing point are all on the low side, along with the reduction of M and cyclohexylamine mol ratio, appearance, yield, The melting point is all improved, when there is too much cyclohexylamine, because the product is dissolved in the cyclohexylamine solution, the yield is reduced, and the post-treatment recovery of cyclohexylamine ...

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Abstract

The invention discloses a method for using a rubber accelerator M to synthesize an sulfonamide accelerator CBS by a solvent purification method. The method comprises the following steps of: by adopting the rubber accelerator M and cyclohexylamine as materials, adopting hydrogen peroxide and sodium hypochlorite as oxidants, adopting sulfuric acid as a catalyst, reacting to synthesize the accelerator CBS, wherein the optimum production process conditions include: (1) the molar ratio between all the materials and the oxidants is as follows: n(M):n(cyclohexylamine) is equal to 1:2.2; n(M):n(20% hydrogen peroxide):n(15% sodium hypochlorite) is equal to 1:0.6:0.65-0.75; (2) the reaction temperature is 35-40 DEG C; and (3) the reaction time is 2.0-2.5 hours. The method disclosed by the invention has the advantages that the technical problem in using the rubber accelerator M to synthesize the sulfonamide accelerator CBS by the solvent purification method is comprehensively solved, the product quality index is higher than international level, the consumption index reaches lower industrial level, and the problem of treatment of waste water, solid wastes and odor pollutants is solved.

Description

technical field [0001] The invention belongs to chemical technology, in particular to a method for synthesizing a sulfenamide accelerator CBS 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 charac...

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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