Process for cleaning accelerator NS produced by oxygen oxidation method of crude product M

A technology of oxygen oxidation and accelerator, which is applied in the field of rubber accelerators, can solve the problems of failure to meet quality requirements, low yield of accelerator NS, large amount of tert-butylamine, etc., to improve product color, low production cost, and product quality high effect

Pending Publication Date: 2019-06-21
淄博拓研化学科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0017] 2.2.1 Due to the use of hydrogen peroxide as the oxidant, waste water is generated in the oxidation reaction, water washing, and M recovery processes. Although compared with the sodium hypochlorite method, the amount of waste water is reduced, but a large amount of waste water will still be produced
[0018] 2.2.2 Raw materials must use industrial products M, otherwise the quality requirements will not be met
[0019] 2.2.3 This method uses a large amount of tert-butylamine, and the yield of accelerator NS is not high

Method used

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  • Process for cleaning accelerator NS produced by oxygen oxidation method of crude product M

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Add aniline, carbon disulfide, and sulfur into a closed container at a ratio of 1:1.2:1, and conduct a condensation reaction at 265°C under a controlled pressure of 11MPa for 8 hours to obtain a crude accelerator M with a content of 93%; mix the crude accelerator M with 10% mass The concentrated ammonia water was stirred at 45°C with a ratio of 1:4 (mass ratio), and air was blown in. After the upper layer RS- became a transparent liquid, the stirring was stopped and the interface phenomenon appeared (the time for blowing air was 0.5 hours), liquid separation, the lower layer of precipitation as solid waste treatment, get the supernatant for use;

[0048] After inserting the solid catalyst, stir the supernatant and tert-butylamine evenly at a ratio of 1:3.6 (molar ratio); after sealing the container, introduce oxygen, control the oxygen pressure to maintain at 0.4MPa, and stop the reaction after the oxygen is no longer consumed. After centrifugal separation, washing and ...

Embodiment 2

[0052] Stir the residual crude product M with a content of 77% (the impurity is tar resin) and 20% mass concentration of ammonia water at a ratio of 1:5.5 (mass ratio) at 55°C, blow in air, and wait until the upper RS- When it is a transparent liquid, stop stirring and precipitate and appear interface phenomenon (the time of air bubbling is 1 hour), separate the liquid, and the lower layer of sediment is treated as solid waste, and the supernatant is taken for use;

[0053] After inserting the solid catalyst, stir the supernatant and tert-butylamine at a ratio of 1:2.7 (molar ratio); after sealing the container, introduce oxygen, control the oxygen pressure to maintain at 0.35MPa, and stop the reaction after the oxygen is not consumed. After centrifugal separation, washing and drying, the product is obtained. The product yield is 96.5%, the initial melting point is 105.8° C., and the product purity is 97%. The product quality has reached the national standard.

[0054] Where...

Embodiment 3

[0057] Stir the residual crude product M with a content of 77% (the impurity is tar resin), 30% mass concentration of ammonia water at a ratio of 1:5.5 (mass ratio) at 50°C, blow in air, and wait for the upper layer RS - After turning into a transparent liquid, stop stirring and settling, and interface phenomena will appear (the time for air bubbling is 0.8 hours), separate the liquid, and the lower layer of precipitation will be treated as solid waste, and the supernatant liquid will be taken for use;

[0058] After inserting the solid catalyst, stir the supernatant and tert-butylamine at a ratio of 1:3 (molar ratio); after sealing the container, introduce oxygen and keep the pressure at 0.2MPa, and the reaction will be terminated after the oxygen is no longer consumed. After centrifugal separation, washing and drying, the product is obtained. It is known that the product yield is 96.9%, the initial melting point is 106.2°C, and the product purity is 98.6% through assay. The...

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Abstract

The invention relates to a rubber accelerator, in particular to a process for cleaning an accelerator NS by an oxygen oxidation method of a crude product M. The process comprises the following steps:(1) dissolving the crude product M in ammonia water with a mass concentration of 10-30 percent, blowing air, performing liquid separation after layering and taking a liquid supernatant; (2) after theliquid supernatant, tert-butylamine and a sold catalyst are uniformly mixed, controlling the temperature to be 55-70 DEG C, introducing oxygen for reaction, maintaining the reaction pressure to be 0.15-0.4 MPa and ending up the reaction after no oxygen consumption; (3) centrifugally separation, washing and drying to obtain a product; the solid catalyst is activated carbon loaded with cobalt sulfate by a dipping method. The process provided by the invention has the benefits that the situation that a large amount of salty wastewater is caused by the use of acids and alkalis when the M is refinedis avoided; compared with a sodium hypochlorite method and a hydrogen peroxide method which are widely used at home, the process has Obvious quality cost advantages, so that the use rate of the disabled crude product M is improved; no overreaction exists, the product color is good, the production cost is low, and the product quality is high.

Description

technical field [0001] The invention relates to a rubber accelerator, in particular to a NS cleaning process for producing the accelerator by oxygen oxidation of crude M. Background technique [0002] Rubber vulcanization accelerator NS, alias: N-tert-butyl-2-benzothiazole sulfenamide; Accelerator NS is suitable for NR, SBR, BR and their mixtures, with fast vulcanization speed and high modulus of vulcanized rubber. Or use a small amount of super speed accelerator alone or in combination in the formula of rubber industrial products. Accelerator NS has the functions of anti-scorch, safe, non-toxic, fast vulcanization, etc. It is especially suitable for synthetic rubber and can improve the modulus and tensile strength of vulcanized rubber. It is mainly used in the manufacture of tires, rubber shoes, hoses, tapes, cables and general industrial products. It belongs to the technical field of rubber vulcanization sulfenamide accelerator NS production. [0003] At present, the sy...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D277/80
Inventor 姬拓
Owner 淄博拓研化学科技有限公司
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