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Novel method for preparing vulcanized rubber accelerant DZ with cooling-down circulating water system

A technology of circulating water system and rubber vulcanization, applied in the direction of organic chemistry, etc., can solve the problem of low yield of accelerator DZ, and achieve the effect of good cooling effect, high yield and less dicyclohexylamine

Inactive Publication Date: 2008-12-10
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 200ml of isopropanol and 100 grams of dicyclohexylamine into an oxidation kettle equipped with a new circulating water cooling system, and fully dissolve dicyclohexylamine in isopropanol at 30°C and a speed of 400 rpm. In, add the sulfuric acid that mass content is 10% with the flow rate of 20ml / min, control pH value to be 9.0, then add M-Na salt with the flow rate of 30ml / min, simultaneously add the mass content of 8.0% with the flow rate of 30ml / min The oxidizing agent sodium hypochlorite, the dropping time is 1.5 hours, and the pH value is controlled during the process to be 9.0. After the reaction is completed, the rubber accelerator DZ product is obtained by suction filtration, washing with water, filtration, and drying. The N,N-dicyclohexyl-2-benzo The purity of thiazole sulfenamide reaches 99.2%.

example 2

[0010] The MBT used in this example is the same as in Example 1. Add 400ml of isopropanol and 300 grams of dicyclohexylamine to an oxidation kettle equipped with a new circulating water cooling system. Next, dicyclohexylamine is fully dissolved in isopropanol, with a flow rate of 30ml / min, add sulfuric acid with a mass content of 13%, control the pH value to 11.0, then add M-Na salt with a flow rate of 50ml / min, At the same time, add the oxidizing agent sodium hypochlorite with a mass content of 10.0% at a flow rate of 50 ml / min. The time for dropping is 1.0 hour, and the pH value is controlled during the process to be 11.0. After the reaction is completed, suction filter, wash with water, filter, and dry to obtain the rubber accelerator DZ product , the purity of the N, N-dicyclohexyl-2-benzothiazole sulfenamide reaches 99.3%.

example 3

[0012] The process of synthesizing MBT adopted in this embodiment is the same as that of Example 1. 800 ml of isopropanol and 500 grams of dicyclohexylamine are added to an oxidation kettle equipped with a novel circulating water cooling system. Under the condition of 1 minute, dicyclohexylamine is fully dissolved in isopropanol, with the flow velocity of 40ml / minute, add the sulfuric acid that mass content is 25%, control pH value is 12.0, then add M- with the flow velocity of 80ml / minute Na salt, add the oxidizing agent sodium hypochlorite that mass content is 12.0% with the flow velocity of 80ml / min simultaneously, dropwise time is 2.0 hours, control pH value in the process to be 12.0, suction filtration, washing with water, filtration, drying after reaction finishes to get rubber accelerator DZ product, the purity of the N,N-dicyclohexyl-2-benzothiazole sulfenamide reaches 99.5%.

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Abstract

The invention discloses a method for producing a rubber vulcanization accelerator DZ by a novel circulating water cooling system. The method comprises the following steps of: adding 100 to 1,000ml of isopropanol and 100 to 1,000g of dicyclohexylamine into an oxidation kettle provided with the novel circulating water cooling system; sufficiently dissolving the dicyclohexylamine in the isopropanol at a temperature of between 20 and 70 DEG C and at a rotational speed of between 100 and 1,400 revolutions / minute; adding sulphuric acid with a mass content of between 10 and 35 percent into the mixed solution at a flow speed of between 20 and 50ml / minute with a pH value controlled between 9.0 and 12.0; then, adding M-Na salt into the mixed solution at a flow speed of between 30 and 100ml / minute, and simultaneously adding sodium hypochlorite with a mass content of between 8.0 and 18.0 percent as an oxidizing agent into the mixed solution at a flow speed of between 30 and 100ml / minute for 1.0 to 3.0 hours, with the pH value controlled between 9.0 and 12.0 during the process; and obtaining a product of the rubber vulcanization accelerator DZ through pumping and extracting, water scrubbing, filtering and drying after the reaction is completed. The purity of the vulcanization accelerator DZ reaches over 99 percent. The method has the advantages of simple process, easy industrialization, good cooling effect, less dicyclohexylamine, high yield, and over 99 percent purity of the vulcanization accelerator DZ.

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): C07D277/80C08K5/47C08C19/20
Inventor 王树华洪学斌王树领王树恒
Owner KEMAI CHEM
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