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Method for producing rubber vulcanization accelerator CZ (N-Cyclohexyl-Benzothiazole Sulfenamide,) by two-drop method

A technology for rubber vulcanization and accelerator, which is applied in the field of rubber vulcanization accelerator N-cyclohexyl-2-benzothiazole sulfenamide, can solve the problem of low salt formation rate of M and cyclohexylamine, and achieves easy industrial production, The effect of reducing links and wastewater

Inactive Publication Date: 2017-05-10
KEMAI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The yield of accelerator CZ in this method is also only about 90%, and the reason is also that the salt-forming rate of M and cyclohexylamine is not high.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] Add 160ml of methanol to cyclohexylamine mixed liquid with a volume ratio of 2:1 into the oxidizer, and add 140g of molten crude M at 170°C to 180°C under the condition of a stirring speed of 400 rpm, and stir fully to make the crude M and Cyclohexylamine generates M-cyclohexylamine salt, and then at a flow rate of 1ml / min, drip a hydrogen peroxide solution with a mass content of 8% in the solution. After 80 minutes, change the sodium hypochlorite to find the end point, and judge the reaction end point with starch potassium iodide test paper. When the test paper turns black, stop adding sodium chlorate dropwise and start distillation to recover methanol; the product is filtered, washed with water, filtered, and dried to obtain the rubber accelerator CZ product. The yield of accelerator CZ reaches over 99%.

Embodiment 2

[0013] Add 200ml of the mixed liquid of methanol and cyclohexylamine with a volume ratio of 2:1 into the oxidizer, and add 120g of molten crude M at 170°C to 180°C under the condition of a stirring speed of 600 rpm, and stir thoroughly to make the crude M and Cyclohexylamine generates M-cyclohexylamine salt, and then at a flow rate of 3ml / min, drip a hydrogen peroxide solution with a mass content of 10% in the solution, after 100 minutes, change the sodium hypochlorite to find the end point, judge the reaction end point with starch potassium iodide test paper, When the test paper turns black, stop adding sodium chlorate dropwise and start distillation to recover methanol; the product is filtered, washed with water, filtered, and dried to obtain the rubber accelerator CZ product. The yield of accelerator CZ reaches over 99%.

Embodiment 3

[0015] Add 240ml of methanol to cyclohexylamine mixed liquid with a volume ratio of 2:1 into the oxidizer, and add 100g of molten crude M at 170°C to 180°C under the condition of stirring speed of 800 rpm, and stir fully to make the crude M and Cyclohexylamine generates M-cyclohexylamine salt, and then at a flow rate of 5ml / min, drip a hydrogen peroxide solution with a mass content of 12% in the solution, after 120 minutes, change the sodium hypochlorite to find the end point, judge the reaction end point with starch potassium iodide test paper, When the test paper turns black, stop adding sodium hypochlorite dropwise and start distillation to recover methanol; the product is suction filtered, washed with water, filtered, and dried to obtain the rubber accelerator CZ product. The yield of accelerator CZ reaches over 99%.

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PUM

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Abstract

The invention discloses a method for producing a rubber vulcanization accelerator CZ (N-Cyclohexyl-Benzothiazole Sulfenamide) by a two-drop method. The method comprises the following steps of, according to a volume ratio, which is 2 to 1, of methanol to cyclohexylamine, adding the mixed liquid of the methanol and the cyclohexylamine into an oxidation device, in an agitation condition, adding a fused coarse M at a temperature of 170 to 180 DEG C, making the M and the cyclohexylamine generate an M-cyclohexylamine salt, afterwards, dropwise adding a hydrogen peroxide solution into a solution, then, after 80 to 120 minutes, replacing the hydrogen peroxide solution with sodium hypochlorite, dropwise adding the sodium hypochlorite to find an endpoint, carrying out a judgment by using starch-potassium iodide test paper, when the test paper becomes black, stopping dropwise adding the sodium hypochlorite, and starting distillation to recover the methanol; carrying out suction filtration, water scrubbing, filtration and drying on a product, so as to obtain the rubber vulcanization accelerator CZ. The yield of the accelerator CZ reaches 99 percent or above; the use level of the cyclohexylamine in the method is low; an M purification process as well as a pulping procedure and a cyclohexylamine distillation procedure in an old process is reduced; the link of producing the CZ is reduced; produced wastewater is decreased by 70 percent or above compared with that in the old process; the method is easy for industrialized production.

Description

technical field [0001] The invention relates to a 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 method ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D277/80
CPCC07D277/80
Inventor 朱军孙风娟
Owner KEMAI CHEM
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