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Method for synthesizing TBBS (Tertiarybutyl Benzothiazole Sulfenamide) by mechanically applying mother solution

A mother liquor application and mother liquor technology, which is applied in the field of rubber accelerator N-tert-butyl-2-benzothiazole sulfenamide, can solve the problems of production and development limitations, difficulty in treatment, high energy consumption and the like, and achieves product yield Increase, reduce consumption, reduce emissions

Inactive Publication Date: 2010-12-08
KEMAI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, a large amount of high-salinity wastewater is produced during the production process, which is difficult to treat, and excessive tert-butylamine needs to be recovered, which consumes a lot of energy and causes serious pollution.
Therefore, due to the pressure of energy and environmental protection, the production and development of TBBS are subject to certain restrictions.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0008] Add water or mother liquor and rubber accelerator M in a weight ratio of 1:2 into the tank for beating, the proportion of mother liquor is 100%, and add tert-butylamine with a molar ratio of 1:1.5 to rubber accelerator M for beating, at 20°C , add sodium hypochlorite oxidant solution dropwise to the material, detect the end point with copper acetate and starch potassium iodide reagent, stop adding oxidant dropwise when the end point is reached, filter, wash with water, and dry to obtain the accelerator TBBS product. The invention has the advantages of directly reusing the mother liquor and mother liquor, which not only reduces the discharge of high-salinity sewage, reduces the pressure of distillation and recovery of t-butylamine, reduces energy consumption, and conforms to the national environmental protection policy. The yield of the accelerator TBBS can reach 98%, the purity can reach 98.2%, and the melting point is above 105°C.

example 2

[0010] Add water or mother liquor and rubber accelerator M in a weight ratio of 1:4 into the tank for beating, the proportion of mother liquor is 80%, and add tert-butylamine with a molar ratio of rubber accelerator M of 1:2 for beating, at 30°C , add sodium hypochlorite oxidant solution dropwise to the material, detect the end point with copper acetate and starch potassium iodide reagent, stop adding oxidant dropwise when the end point is reached, filter, wash with water, and dry to obtain the accelerator TBBS product. The invention has the advantages of directly reusing the mother liquor and mother liquor, which not only reduces the discharge of high-salinity sewage, reduces the pressure of distillation and recovery of t-butylamine, reduces energy consumption, and conforms to the national environmental protection policy. The yield of the accelerator TBBS reaches over 98.1%, the purity can reach 98.5%, and the melting point is over 105°C.

example 3

[0012] Add water or mother liquor and rubber accelerator M in a weight ratio of 1:5 into the tank for beating, the proportion of mother liquor is 50%, and add tert-butylamine with a molar ratio of rubber accelerator M of 1:3 for beating, at 50°C , add sodium hypochlorite oxidant solution dropwise to the material, detect the end point with copper acetate and starch potassium iodide reagents, stop adding the oxidant dropwise when the end point is reached, filter, wash with water, and dry to obtain the accelerator TBBS product. The invention has the advantages of directly reusing the mother liquor and mother liquor, which not only reduces the discharge of high-salinity sewage, reduces the pressure of distillation and recovery of t-butylamine, reduces energy consumption, and conforms to the national environmental protection policy. The yield of the accelerator TBBS reaches over 98.2%, the purity can reach 98.5%, and the melting point is over 105°C.

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PUM

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Abstract

The invention discloses a method for synthesizing TBBS (Tertiarybutyl Benzothiazole Sulfenamide) by mechanically applying a mother solution, comprising the following steps of: adding water or mother solution and a rubber accelerator according to the mass ratio of 1:2-6 in a kettle for pulping, wherein the mechanical apply ratio of the mother solution is 20-100 percent; adding tert-butylamine, wherein the mol ratio of the tert-butylamine to the rubber accelerator is 1:1.05-5; dropping an NaCLO oxidant solution in the material at the temperature of 20-70DEG C, detecting the ending point with copper acetate and starch potassium iodide and stopping dropping the oxidant at the ending point; and carrying out the filtering, the washing and the drying to obtain the accelerator TBBS product. The invention has the advantages that: the mother solution is directly recycled, thereby not only reducing the discharge of high-salinity sewage, the pressure of distilling and recovering the tert-butylamine and energy consumption, but also according with the environment-friendly policy of the state. The accelerator TBBS has over 98 percent of yield, 98 percent of purity and over 105DEG C of melting point. The invention also has the advantages that the method has simple process and is easy to industrialize and the mother solution is directly recycled, thereby reducing the discharge of high-salinity sewage, the pressure of distilling and recovering the tert-butylamine and energy consumption; in addition, the yield of the product is improved and the consumption of the tert-butylamine is reduced, so that the invention reduces the production cost and accords with the environment-friendly policy of the state.

Description

technical field [0001] The invention relates to a production method of rubber accelerator N-tert-butyl-2-benzothiazole sulfenamide (TBBS, NS), belonging to the technical field of accelerator TBBS production. Background technique [0002] Rubber vulcanization accelerator TBBS is a post-effect accelerator, which is very safe at operating temperature, has good scorch resistance and high elongation strength, can increase the proportion of synthetic rubber used, increase the amount of filler carbon black, and is more active than accelerators. CBS, NOBS, etc. have slight discoloration and pollution, so they have excellent performance, so they become "standard accelerators". 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 the total accelerator consumption. TBBS is synthesized from tert-butylamine and accelerator M, and there is no carcinogenic problem of nitrosam...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D277/80
Inventor 洪学斌尹红伟张超义
Owner KEMAI CHEM
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