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Synthesis method of rubber vulcanization accelerator TBBS (N-tert-butyl-2-benzothiazolesulfenamide)

A synthesis method and rubber vulcanization technology are applied in the synthesis field of crude MBT to produce TBBS, which can solve the problems of increased production cost, increased equipment investment, product pollution, etc., and achieves the effects of reducing three wastes, low cost and environmental friendliness

Inactive Publication Date: 2012-12-26
KEMAI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method saves the MBT refining process and has certain advantages, but adding a decoking agent (one of cyclohexanol, isobutanol, aniline, and cyclohexylamine) during the synthesis process will inevitably lead to Increase production costs, and cause organic matter to remain in the product, causing pollution to the product, and requires equipment to recycle the added decoking agent, increasing equipment investment

Method used

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  • Synthesis method of rubber vulcanization accelerator TBBS (N-tert-butyl-2-benzothiazolesulfenamide)
  • Synthesis method of rubber vulcanization accelerator TBBS (N-tert-butyl-2-benzothiazolesulfenamide)
  • Synthesis method of rubber vulcanization accelerator TBBS (N-tert-butyl-2-benzothiazolesulfenamide)

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Add 100.00 g of crude MBT (measured to have a purity of 75%, mass percentage) into a reactor filled with 392.85 g of tert-butylamine aqueous solution with a mass content of 25% (the molar ratio of MBT to tert-butylamine after conversion is 1:3 ), and stir evenly; to the above reaction mixture, add a sodium hypochlorite solution with 13% available chlorine to oxidize and synthesize until the end of the reaction, the synthesis temperature is maintained at 30°C, and the oxidation time is 1.5h. The end of the oxidation is detected by copper acetate solution and starch potassium iodide solution ; The reaction mixture reacted to the end is suction filtered, and the filter cake is washed 5 times with 5% tert-butylamine aqueous solution by mass content, and the consumption of each tert-butylamine is 12.77g (65% of the amount of tert-butylamine added before the reaction). Then wash to neutrality with water, obtain qualified vulcanization accelerator TBBS 100.33g after filter cake...

Embodiment 2

[0020] Add 100.00g of crude MBT (measured to have a purity of 80%, mass percentage) into a reactor filled with 232.8g of tert-butylamine aqueous solution with a mass content of 45% (the molar ratio of MBT to tert-butylamine after conversion is 1:3 ), and stir evenly; to the above reaction mixture, add a sodium hypochlorite solution with 18% available chlorine to oxidize and synthesize until the end of the reaction, the synthesis temperature is maintained at 30°C, and the oxidation time is 1.5h. The end of the oxidation is detected by copper acetate solution and starch potassium iodide solution ; The reaction mixture reacted to the end is suction filtered, and the filter cake is washed 5 times with 5% tert-butylamine aqueous solution by mass content, and the consumption of each tert-butylamine is 12.77g (65% of the amount of tert-butylamine added before the reaction). Then wash to neutrality with water, obtain qualified vulcanization accelerator TBBS 100.02g after filter cake dr...

Embodiment 3

[0022] 100.00g of crude MBT (measured as 90% in purity, mass percentage) was added to a reactor filled with 436.50g of tert-butylamine (fresh) aqueous solution with a mass content of 45% (the molar ratio of MBT to tert-butylamine after conversion was 1:5), stir evenly; to the above reaction mixture, add sodium hypochlorite solution with 15.5% available chlorine to oxidize and synthesize until the end of the reaction, the synthesis temperature is maintained at 45°C, and the oxidation time is 2.5h. Potassium iodide solution detection; the reaction mixture that has reacted to the end is suction filtered, and the filter cake is washed twice with tert-butylamine (fresh) aqueous solution with a mass content of 45%, and the amount of tert-butylamine is 83.48g each time 85%), and then washed with water until neutral, and the filter cake was dried to obtain 118.61 g of qualified vulcanization accelerator TBBS.

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Abstract

The invention relates to a synthesis method of a rubber vulcanization accelerator TBBS (N-tert-butyl-2-benzothiazolesulfenamide), which comprises the following steps: adding crude MBT (2-mercaptobenzthiazole) into a reactor filled with a tert-butylamine water solution, stirring evenly, and adding an oxidizer sodium hypochlorite for oxidation synthesis; and after the reaction reaches the end point, carrying out vacuum filtration, washing the filter cake with the tert-butylamine water solution for 2-5 times, washing with water to a neutral state, and drying the filter cake to obtain the qualified vulcanization accelerator TBBS. The mother liquor obtained by carrying out vacuum filtration on the reaction product and the washing liquid obtained by washing the material for the first time are distilled to recycle the tert-butylamine, and the washing liquid obtained after the second time can be repeatedly used as a reaction solution or washing liquid. The MBT crude product is used as the raw material to directly synthesize the accelerator TBBS without adding coke remover or any other raw material; and thus, the technique saves the MBT refinement process, does not need to add other solvents, is simple to operate, and has the advantages of low cost, low environmental pollution and high yield.

Description

technical field [0001] The invention relates to a preparation process of a rubber vulcanization accelerator TBBS (the chemical name is N-tert-butylbenzothiazole sulfenamide), specifically, it relates to a synthesis method for producing TBBS with crude MBT, which belongs to the accelerator TBBS production technology field. Background technique [0002] Accelerator N-tert-butylbenzothiazole sulfenamide (TBBS, NS) is a post-effect accelerator, which is very safe at operating temperature, has good scorch resistance, high elongation strength, and can improve the use of synthetic rubber. Ratio, increase the amount of filler carbon black, the activity is greater than the accelerator CBS, NOBS, etc., the discoloration and pollution are slight, so its performance is excellent, so it is called "standard accelerator". NS has now become one of the leading accelerator varieties in domestic and foreign markets, and the consumption of NS in developed countries accounts for 35% to 45% of t...

Claims

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Application Information

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IPC IPC(8): C07D277/80
Inventor 尹红伟
Owner KEMAI CHEM
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