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Novel production method of rubber vulcanization accelerant CZ

A production method and rubber vulcanization technology, which is applied in the field of rubber vulcanization accelerator N-cyclohexyl-2-benzothiazole sulfenamide, can solve the problem of low yield of accelerator CZ, and achieve the effect of simple process and easy industrialization

Inactive Publication Date: 2009-02-18
KEMAI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has a low yield of accelerator CZ

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 55%. Add 50ml of water and 30ml of cyclohexylamine mixed liquid into the oxidation kettle, and add 25ml of accelerator M slurry with a mass content of 55% at a flow rate of 200ml / min at 35°C and a speed of 500 rpm , then with a flow rate of 30ml / min, in the solution, dropwise adding a mass content of 5% hydrogen peroxide solution, after 10 minutes, with a flow rate of 50ml / min, dropwise adding a mass content of 55% accelerator M slurry in the solution, After 45 minutes, take a sample and test the reaction end point with starch KI test paper. When the starch KI test paper changes color, stop dripping hydrogen peroxide and accelerator M, suction filter, wash with water, filter, and dry to obtain the rubber accelerator CZ product. The yield of this N-cyclohexyl-2-benzothiazole sulfenamide was 99.1%.

example 2

[0010] The MBT used in this embodiment is the same as that in Example 1, except that the mass content of MBT generated is 80%, and the mixed liquid of 100ml water and 100ml cyclohexylamine is added to the oxidation kettle, and at 100°C, the rotating speed is 2000 rpm Under condition, with the flow velocity of 5ml / min, add the accelerator M slurry 100ml that mass content is 80%, then with the flow velocity of 10ml / min, in solution, drip the hydrogen peroxide solution that mass content is 10%, after 70 minutes, with Flow rate of 60ml / min, in the solution, drip the accelerator M slurry that mass content is 80%, after 200 minutes, take a sample, test reaction end point with starch KI test paper, when starch KI test paper changes color, stop dripping hydrogen peroxide and promote Agent M, suction filtration, water washing, filtration, and drying to obtain the rubber accelerator CZ product. The yield of this N-cyclohexyl-2-benzothiazole sulfenamide was 99.3%.

example 3

[0012] The process of synthesizing MBT used in this example is the same as Example 1, except that the mass content of MBT is 90%, and the mixed liquid of 100ml water and 200ml cyclohexylamine is added to the oxidation kettle, and the mixture is heated at 170°C and the rotating speed is 3000 rpm Under the condition of / minute, with the flow rate of 400ml / minute, add the accelerator M slurry 200ml that mass content is 90%, then with the flow rate of 75ml / minute, drip the hydrogen peroxide solution that mass content is 35% in solution, 10 Minutes later, at a flow rate of 80ml / min, add dropwise the accelerator M slurry with a mass content of 90% in the solution. After 30 minutes, take a sample and test the reaction end point with starch KI test paper. When the starch KI test paper changes color, stop dripping Hydrogen peroxide and accelerator M are suction filtered, washed with water, filtered, and dried to obtain the rubber accelerator CZ product. The yield of this N-cyclohexy...

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Abstract

The present invention discloses a novel production method of thiofide CZ. The method comprises the following steps: the mixed solution of water and cyclohexane with a volume ratio of 1 to (0.5 to 2.0) is added into an oxidization reactor; under the conditions with the temperature between 20 DEG C and 200 DEG C and the rotating speed of 100 to 4000 rounds per minute, 10 to 30 ml of an accelerant M material slurry with a weight content between 50 percent and 99 percent is added at a flow rate between 5 ml / m and 500 ml / m; hydrogen peroxide solution with a weight content between 1 percent and 35 percent is dropped at a flow rate between 10 ml / m and 150 ml / m; after 1 to 90 minute(s), the accelerant M material slurry with a weight content between 50 percent and 99 percent is dropped into the solution at a flow rate between 10 ml / m and 200 ml / m; after 5 to 300 minutes, a sample is taken, starch KI test paper is used for testing the reaction end point; when the color of the starch KI test paper is changed, the hydrogen peroxide solution and the accelerant M are stopped to be added; the thiofide CZ can be produced after pumping, washing, filtering and drying, and the yield rate of the thiofide CZ reaches above 99 percent. The present invention has the advantages that the process is simple, the industrialization of the process can be easily realized, a small amount of cyclohexane is used, no wastewater with salt is discharged, and the yield rate of the thiofide CZ reaches above 99 percent.

Description

technical field [0001] The invention relates to a novel production method of a rubber vulcanization accelerator N-cyclohexyl-2-benzothiazole sulfenamide (CZ), belonging to the technical field of rubber vulcanization accelerator CZ 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. CZ is an indispensable one in the rubber industry. main accelerator. Accelerator CZ is a highly active post-effect semi-overspeed accelerator with excellent anti-scorch performance, safe processing and short vulcanization time. Literature (Fine Chemical Industry, 2006, 23: 923) reported the ...

Claims

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Application Information

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IPC IPC(8): C07D277/80C08K5/47C08L21/00
Inventor 王树华洪学斌王树领王树恒孟庆保
Owner KEMAI CHEM
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