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Method for preparing rubber peptizer DBD

A technology of rubber peptizer and oxidant, which is applied in the preparation of hydrogenated polysulfide/polysulfide, organic chemistry, etc., can solve the problems of high material cost and power cost, direct treatment without separation, and difficult control of the production process. Achieve the effects of reducing the cost of three wastes treatment, facilitating popularization and application, and easy control

Active Publication Date: 2014-04-16
HEZE JIACHENG CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] 1. Due to the hydrogenation reduction reaction in this process, high temperature and high pressure equipment is used, which requires large production investment and high energy consumption;
[0011] 2. The production process of this process is difficult to control, the product yield is low, and the cost is high
[0012] 3. Due to the high cost of materials and power, the market price is obviously inferior to that of thiophenol products. The market price of thiophenol products is between 40,000 and 50,000 yuan, while the price of DBD is more than 100,000 yuan.
[0017] 3. Chloroform was used as solvent, and the reaction was directly processed without separation

Method used

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  • Method for preparing rubber peptizer DBD

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] The preparation method of rubber peptizer DBD adopts the following steps:

[0038] (1) Put 500 kg of water and 110 kg of sodium hydroxide in turn into a reaction kettle equipped with a thermometer and agitator, stir to dissolve, then add 200 kg of benzothiazole, heat up to 80°C, and react for 3 hours to normal temperature spare;

[0039] (2) 200 kilograms of water, 70 kilograms of sulfuric acid with a concentration of 98% and 90 kilograms of aqueous hydrogen peroxide with a concentration of 40% are prepared as an oxidant, and pumped to a metering tank for standby; the prepared oxidant is dripped into the step (1) In the reaction solution, the pH value is controlled to 6-7 at the end point, and the temperature is reduced to suction filtration at the end point, and washed to obtain diphenylamine disulfide;

[0040] (3) Put 606 kg of toluene and 300 kg of diphenylamine disulfide in turn into the reaction kettle equipped with a thermometer and agitator, start stirring, hea...

Embodiment 2

[0042] The preparation method of rubber peptizer DBD adopts the following steps:

[0043] (1) Put 600 kg of water and 150 kg of sodium hydroxide in turn into a reaction kettle equipped with a thermometer and agitator, stir to dissolve, then add 250 kg of benzothiazole, heat up to 75°C, and react for 3.5 hours to normal temperature spare;

[0044] (2) 250 kilograms of water, 95 kilograms of sulfuric acid with a concentration of 95% and 130 kilograms of aqueous hydrogen peroxide with a concentration of 50% are prepared as an oxidant, and pumped to a metering tank for standby; the prepared oxidant is dripped into the step (1) In the reaction solution, the pH value is controlled to 6-7 at the end point, and the temperature is reduced to suction filtration at the end point, and washed to obtain diphenylamine disulfide;

[0045] (3) Put 693 kg of toluene and 350 kg of diphenylamine disulfide in sequence into the reaction kettle equipped with a thermometer and agitator, start stirri...

Embodiment 3

[0047] The preparation method of rubber peptizer DBD adopts the following steps:

[0048] (1) Put 400 kg of water and 90 kg of sodium hydroxide in turn into a reaction kettle equipped with a thermometer and agitator, stir to dissolve, then add 150 kg of benzothiazole, heat up to 70°C, and react for 2.5 hours to normal temperature spare;

[0049](2) 150 kilograms of water, 60 kilograms of sulfuric acid with a concentration of 93% and 80 kilograms of aqueous hydrogen peroxide with a concentration of 27.5% are prepared as an oxidant, and pumped to a metering tank for standby; the prepared oxidant is dripped into the step (1) In the reaction solution, the pH value is controlled to 6-7 at the end point, the temperature is lowered and the suction is filtered at the end point, and diphenylamine disulfide is obtained by washing;

[0050] (3) Put 433 kg of toluene and 250 kg of diphenylamine disulfide into the reaction kettle equipped with a thermometer and agitator in sequence, start...

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Abstract

The invention relates to a method for preparing a rubber auxiliary agent, and particularly discloses a method for preparing rubber peptizer 2,2-dibenzoylamino diphenyl disulphide (DBD). The method for preparing the rubber peptizer DBD is characterized by comprising the following steps of: performing ring opening reaction on benzothiazole to obtain a ring opening product; oxidizing the ring opening product to prepare diphenylamine disulphide; and performing acylation reaction on the diphenylamine disulphide and benzoyl chloride to generate the DBD. According to the method for preparing the rubber peptizer DBD, compared with the conventional process, the product cost is remarkably reduced; the method is favorable for popularization and application of the environmentally-friendly peptizer DBD, and simultaneously breaks through the situation that the product depends on import for a long term; the organic solvent is used as a reaction medium and can be recycled, so little three-waste is discharged; and the production flow is simple and easily controlled, high-temperature and high-pressure reaction does not exist in the method, the equipment investment is low, and the method is easy for production and operation.

Description

(1) Technical field [0001] The invention relates to a preparation method of a rubber auxiliary agent, in particular to a preparation method of a rubber peptizer DBD. (2) Background technology [0002] my country is already a big country in rubber processing in the world, with an annual rubber consumption of more than 7 million tons, ranking first in the world, of which natural rubber accounts for 46% and synthetic rubber accounts for 54%. The output of tires ranks first in the world, and the output of bicycle tires, power tires and rubber shoes ranks first in the world. However, my country's rubber additives industry gradually developed after liberation, especially after the 1980s, with the implementation of the reform and opening up policy, the application and development of rubber additives has made great progress, but compared with developed countries , there is still an obvious gap. [0003] For a long period of time, the only rubber peptizers are pentachlorothiophe...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C323/42C07C319/22C08K5/375C08L21/00
Inventor 王平生刘志强崔平刚梁志红赵士杰
Owner HEZE JIACHENG CHEM CO LTD
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