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Process for preparing rubber accelerator TBBS

A technology of rubber accelerator and production method, applied in organic chemistry and other directions, can solve the problems of large distillation load, large amount of waste water and high COD, and achieve the effects of reducing waste water discharge, saving energy and improving M conversion rate

Inactive Publication Date: 2010-09-08
SHANDONG SUNSINE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method has low yield, large distillation load, high energy consumption, large amount of waste water, high COD, and contains a large amount of inorganic salts, which is difficult to handle

Method used

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  • Process for preparing rubber accelerator TBBS
  • Process for preparing rubber accelerator TBBS

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] The production method of rubber accelerator TBBS of the present invention is made up of following steps successively:

[0016] a, oxidation reaction: with 500 kilograms of raw material M, 600 kilograms of tert-butylamine and 0.5 kilogram of carbonic acid, add 5500 kilograms of water and stir evenly, keep the temperature in the oxidation kettle at 30-50 ° C, add 436 kilograms of hydrogen peroxide solution with a mass content of 28% (hydrogen peroxide molecular weight: 34.01) was oxidized, and the oxidation time was 7 hours;

[0017] b. The oxidized material is distilled to recover tert-butylamine: adopt the vacuum distillation method, the vacuum degree is 0.03-0.09MPa, the temperature at the top of the tower is 20-25°C, the temperature at the bottom of the tower is 20-25°C, and the distillation time is 5 hours;

[0018] c. The remaining material after distillation is placed in a centrifuge and washed with water in a conventional manner until pH = 7 to obtain a finished p...

Embodiment 2

[0021] The production method of rubber accelerator TBBS of the present invention is made up of following steps successively:

[0022] a, oxidation reaction: with 500 kilograms of raw materials M, 2000 kilograms of tert-butylamine and 50 kilograms of acetic acid, add 7500 kilograms of water and stir evenly, keep the temperature in the oxidation kettle at 30-50 ° C, add 654 kilograms of hydrogen peroxide solution with a mass content of 28% (hydrogen peroxide molecular weight: 34.01) is oxidized, and the oxidation time is 3 hours;

[0023] b. The oxidized material is distilled to recover tert-butylamine: adopt the vacuum distillation method, the vacuum degree is 0.03-0.09MPa, the temperature at the top of the tower is 60-65°C, the temperature at the bottom of the tower is 75-80°C, and the distillation time is 2 hours;

[0024] c. The remaining material after distillation is washed with water in a centrifuge until pH = 7 to obtain the finished product of TBBS.

[0025] All the ot...

Embodiment 3

[0027] The production method of rubber accelerator TBBS of the present invention is made up of following steps successively:

[0028] a. Oxidation reaction: Add 500 kg of raw material M, 1300 kg of tert-butylamine and 25 kg of oxalic acid, add 6500 kg of water and stir evenly, keep the temperature in the oxidation kettle at 30-50 ° C, add 550 kg of hydrogen peroxide solution with a mass content of 28% for oxidation , the oxidation time is 5 hours;

[0029] b. Distillation of the oxidized material to recover tert-butylamine: adopt vacuum distillation method, the vacuum degree is 0.03-0.09MPa, the temperature at the top of the tower is 40-45°C, the temperature at the bottom of the tower is 50-55°C, and the distillation time is 3.5 hours;

[0030] c. The remaining material after distillation is washed with water in a centrifuge until pH = 7 to obtain the finished product of TBBS.

[0031] All the other are identical with embodiment 1.

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Abstract

The invention provides a production method of a rubber promoter TBBS, sequentially comprising the following steps of: a. oxidation reaction: materials of M, tert-butylamine and an additive are added with water for even agitation and is then added with an oxidizing agent for oxidation, all materials are present in a weight ratio of M: tert-butylamine: water=1:1.2-4.0: 11-15; b. recovery of tert-butylamine through material distillation after the oxidation; and c. putting the distillated residual material in a centrifuge for dewatering by washing until the pH value is equal to 7, so as to obtainthe TBBS finished product. The production method has the advantages of optimized process flow, increased M conversion rate, reduced dissolution of product in tert-butylamine, greatly reduced tert-butylamine consumption, lowered distillation load by 70 percent, reduced energy consumption, reduced wastewater discharge by over two third, saved energy, more importantly, non saline matter in the process wastewater, and easy biochemical treatment.

Description

(1) Technical field [0001] The invention relates to a production method of a rubber accelerator TBBS. (2) Background technology [0002] TBBS (that is, N-tert-butyl-2-benzothiazole sulfenamide) is an important rubber accelerator with excellent vulcanization performance and is an ideal replacement product. The existing production method is that M (ie, 2-mercaptobenzothiazole, molecular weight 167.24) reacts with excess tert-butylamine under the action of an oxidizing agent, and the reacted material is washed with water, then dehydrated and dried to obtain a finished product. Mother liquor and washing water are distilled to recover excess tert-butylamine. The method has low yield, large distillation load, high energy consumption, large amount of waste water, high COD, and contains a large amount of inorganic salts, which is difficult to handle. (3) Contents of the invention [0003] In order to make up for the deficiencies in the prior art, the invention provides a product...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D277/80C08K5/47C08C19/20
Inventor 徐承秋苗静吕桂中谢耿柱刘经福王桂玲刘文娜
Owner SHANDONG SUNSINE CHEM
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