Method for producing rubber vulcanization accelerator CZ

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 wastewater reduction and link reduction

Inactive Publication Date: 2017-05-24
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

[0012] According to the volume ratio of methanol and cyclohexylamine as 2:1, add 160ml of mixed liquid into the oxidizer, and add 120g 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 generate M-cyclohexylamine salt, and then with the flow rate of 1ml / min, in the solution, dripping the sodium hypochlorite solution that mass content is 12%, after 80 minutes, sampling observation, judge reaction terminal 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

[0014] According to the volume ratio of methanol and cyclohexylamine as 2:1, add 200ml of the mixed liquid into the oxidizer, and add 100g of molten 170°C to 180°C crude M at a stirring speed of 600 rpm, and stir fully to make the crude M and cyclohexylamine generate M-cyclohexylamine salt, then with the flow rate of 3ml / min, dripping the sodium hypochlorite solution that mass content is 15% in the solution, after 100 minutes, sampling observation, judge reaction terminal 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

[0016] According to the volume ratio of methanol and cyclohexylamine as 2:1, add 240ml of mixed liquid into the oxidizer, and add 140g of molten crude M at 170°C to 180°C under the condition of stirring speed of 400 rpm, and stir fully to make the crude M and cyclohexylamine generate M-cyclohexylamine salt, then with the flow velocity of 5ml / min, in solution, dripping the sodium hypochlorite solution that mass content is 18%, after 120 minutes, sampling observation, judge reaction terminal 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%.

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PUM

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Abstract

The invention discloses a method for producing a rubber vulcanization accelerator CZ. The method comprises the following steps: adding a mixed liquid of methanol and cyclohexane in a volume ratio of 2:1 into an oxidizer, under a stirring condition, adding molten crude M of 170-180 DEG C to generate M-cyclohexylamine from crude M and cyclohexane, dropping a sodium hypochlorite solution into the solution, after 80-120 minutes, sampling and observing, judging a reaction final point by using potassium iodide-starch test paper, stopping dropping sodium chlorate when the test paper is black, and starting distillation to recycle methanol; performing suction filtration, water washing, filtration and drying, thereby obtaining a rubber vulcanization accelerator CZ product. The yield of the rubber vulcanization accelerator CZ is up to 99% or greater; by adopting the method, a small amount of cyclohexane is used, an M purification procedure and a pulping procedure and a cyclohexane distillation procedure in a conventional process can be reduced, procedures for producing CZ can be reduced, wastewater of the production can be reduced by 70% or greater when being compared with that of the conventional process, and industrial production can be easily achieved.

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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