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Co-production synthesizing technology of rubber vulcanization promoter NS

A technology of rubber vulcanization and accelerator, which is applied in the field of rubber accelerator NS co-production technology, to achieve the effects of easy industrialization, reduced production, and simple process

Active Publication Date: 2013-10-09
SHANDONG YANGGU HUATAI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to solve the problem of mother liquor treatment after the synthesis of NS by the oxygen oxidation method in the prior art, the present invention proposes a process for producing rubber vulcanization accelerator NS by co-production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Embodiment 1: Coproduction method produces accelerator NS

[0032] First, 400ml of water was added into a 2L autoclave, and then 170.66g of vulcanization accelerator M with a purity of 98% and 190.74g of tert-butylamine with a purity of 99.7% were added in sequence. Then raise the temperature to 35°C, keep the temperature, stir for 30min at a stirring rate of 30rpm, and mix well.

[0033] Dissolve 0.04 g of catalyst copper acetate with 10 g of 10% ammonia water by mass, add it into the above-mentioned autoclave for stirring, and mix with M and tert-butylamine solution evenly. The autoclave was then sealed and heated to 55°C. Keep the temperature between 55-65°C, increase the stirring speed to 300 rpm, start to feed oxygen into the closed autoclave until the pressure in the autoclave reaches 0.7MPa, stop feeding oxygen, continue stirring, and the reaction starts conduct. The pressure drops slowly. When the pressure drops below 0.2MPa and not lower than 0.1MPa, oxygen ...

Embodiment 2

[0037] Embodiment 2: Coproduction method produces accelerator NS

[0038]First, 1000ml of water was added to an autoclave with a volume of 5L, and then 512.12g of vulcanization accelerator M with a purity of 98% and 550.24g of tert-butylamine with a purity of 99.7% were added in sequence. Stir for 40 minutes to make it evenly mixed. 0.16 g of catalyst copper acetate was dissolved in 15 g of 20% ammonia water by mass, added to the autoclave and stirred, and mixed with M and tert-butylamine solution evenly. Then the autoclave was sealed and the temperature was raised to 60°C. Under the conditions of a reaction temperature of 55-65°C and a stirring rate of 600 rpm, start to feed oxygen into the airtight autoclave until the pressure in the autoclave reaches 0.8 MPa, stop feeding oxygen, continue stirring, and the reaction begins. The pressure drops slowly. When the pressure drops to 0.2MPa, oxygen is introduced again; when the pressure reaches 0.8MPa, the oxygen is stopped and t...

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Abstract

The invention relates to a technology for producing a rubber vulcanization promoter NS by using a co-production method. According to the method, raw materials M, tert-butylamine and water are added into an autoclave; oxygen is adopted as an oxidizing agent, copper acetate is adopted as a catalyst, and NS is synthesized for a first time; 2-mercaptobenzothiazole (M) is added to the obtained mother liquor, the mixture is oxidized by using sodium hypochlorite, and NS is synthesized again. The purity of the obtained NS is higher than 99.2%, and a total yield of NS is higher than 98.2%. With the technology provided by the invention, the consumption of tert-butylamine is reduced, and the consumptions of time and energy used for recycling tert-butylamine are reduced.

Description

technical field [0001] The invention relates to a rubber accelerator NS (N-tert-butyl-2-benzothiazole sulfenamide) co-production technology, which belongs to the field of fine chemicals. Background technique [0002] With the development of the rubber industry, the research and production of rubber additives have attracted more and more attention. Rubber vulcanization accelerator NS (also known as TBBS), the chemical name is N-tert-butyl-2-benzothiazole sulfenamide, is one of the important varieties of sulfenamide vulcanization accelerators, and has both scorch resistance and Fast vulcanization speed has two advantages. Used in natural rubber, styrene-butadiene rubber, cis-butadiene rubber, and isoprene rubber, especially suitable for furnace-process carbon black rubber with high alkalinity, its activity is greater than that of widely used accelerators CBS, NOBS, etc., with slight discoloration and pollution , can replace the carcinogenic NOBS containing secondary amino gr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D277/80
Inventor 杜孟成马德龙宋彦哲田路宾
Owner SHANDONG YANGGU HUATAI CHEM
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