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Method of producing rubber vulcanization accelerator DZ

A technology of rubber accelerator and production method, which is applied in the direction of organic chemistry, can solve the problem of low yield of accelerator DZ, and achieve the effect of simple process and easy industrialization

Inactive Publication Date: 2008-03-19
KEMAI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The yield of accelerator DZ is low in this method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0008] Condensation reaction is carried out with aniline, carbon disulfide and sulfur at 270-280°C and pressure of 9-10Mpa to generate MBT with a mass content of 92%. Add 100 grams of M-Na salt to an oxidation kettle equipped with catalyst KM-01, and add bicycline with a mass content of 90% at a flow rate of 30 ml / min at 40°C and a speed of 400 rpm. Hexylamine, then with the flow rate of 30ml / min, in solution, dripping mass content is the sulfuric acid solution of 30%, then with the flow rate of 30ml / min, feeds oxygen in solution, after 40 minutes, take a sample and observe material color, when When the color of the material is gray or white, stop feeding oxygen, sulfuric acid and dicyclohexylamine, filter with suction, wash with water, filter, and dry to obtain the rubber accelerator DZ product. The yield of the N,N-bicyclohexyl-2-benzothiazole sulfenamide reached 99.1%.

example 2

[0010] The MBT used in this example is the same as in Example 1. 200 grams of M-Na salt is added to an oxidation kettle equipped with catalyst KM-01, and at 50°C and a rotating speed of 500 rpm, 40 ml / min The flow rate of 1 minute, add the dicyclohexylamine that mass content is 85%, then with the flow rate of 40ml / min, drip the sulfuric acid solution that mass content is 40% in the solution, then with the flow rate of 40ml / min, pass in solution After 60 minutes, take a sample to observe the color of the material. When the color of the material is gray or white, stop feeding oxygen, sulfuric acid and dicyclohexylamine, filter with suction, wash with water, filter, and dry to obtain the rubber accelerator DZ product. The yield of the N,N-bicyclohexyl-2-benzothiazole sulfenamide reached 99.2%.

example 3

[0012] The process for the synthesis of MBT used in this example is the same as in Example 1. 300 grams of M-Na salt is added to an oxidation kettle equipped with catalyst KM-01, and at 60° C. and a rotating speed of 600 rpm, With the flow velocity of 50ml / min, add the dicyclohexylamine that mass content is 90%, then with the flow velocity of 50ml / min, in solution, drip the sulfuric acid solution that mass content is 50%, then with the flow velocity of 50ml / min, to Oxygen is introduced into the solution, and after 80 minutes, a sample is taken to observe the color of the material. When the color of the material is gray or white, the introduction of oxygen, sulfuric acid and bicyclic cyclohexylamine is stopped, and the rubber accelerator DZ is obtained by suction filtration, water washing, filtration and drying. product. The yield of the N,N-bicyclohexyl-2-benzothiazole sulfenamide reached 99.5%.

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PUM

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Abstract

The invention discloses a production method of rubber vulcanization accelerator DZ. 100 to 500 grams of M-Na salt is added into an oxygenation kettle containing catalyst KM-01; under the conditions of temperature between 20 DEG C and 70 DEG C and rotational speed between 100 rotations per minute and 1400 rotations per minute, at a flow speed between 30 ml per minute and 70 ml per minute, dicyclohexylamine with eighty to ninety percent of mass content is added into the oxygenation kettle; at a flow speed between 30 ml per minute and 50 ml per minute, sulphuric acid solution with thirty to sixty percent of mass content is dripped into the solution; at a flow speed between 30 ml per minute and 110 ml per minute, oxygen is pumped into the solution; after forty to one hundred and fifty minutes, the color of the sampled material is observed, when the color of the material is gray or white, the addition of oxygen, sulphuric acid and dicyclohexylamine is stopped, a rubber vulcanization accelerator DZ product is produced by pumping filtration, water washing, filtration and drying, and the purity of the accelerator DZ reaches over ninety nine percent. The invention has the advantages of simple process of the method, easy industrialization, little usage of dicyclohexylamine and usage of environment-friendly oxidant oxygen, and the yield rate of the accelerator DZ reaches over ninety nine percent.

Description

technical field [0001] The invention relates to a production method of rubber vulcanization accelerator N, N-dicyclohexyl-2-benzothiazole sulfenamide (DZ), belonging to the technical field of rubber vulcanization accelerator DZ production. Background technique [0002] With the development of the rubber industry, people pay more and more attention to the research and production of vulcanization accelerators. Vulcanization accelerator plays a very important role in the rubber vulcanization process. It can greatly accelerate the reaction between rubber and vulcanizing agent, improve productivity, and at the same time improve the physical and mechanical properties of vulcanized rubber. DZ is an essential in the rubber industry. main accelerator. Literature (Science and Technology Information, 2005, 7: 23) reported a method for synthesizing DZ by a large proportion oxidation method. Add accelerator M, dicyclohexylamine, and isopropanol into the reactor and stir to make it into...

Claims

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Application Information

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IPC IPC(8): C07D277/36C08K5/47C08C19/20
Inventor 王树华洪学斌王树领王树恒孟庆保
Owner KEMAI CHEM
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