Method for synthesizing rubber vulcanization accelerator CZ by two-step process by using sodium hypochlorite as oxidizer

By using sodium hypochlorite and M-Na salt to generate rubber vulcanization accelerator CZ in the reaction of sulfuric acid and cyclohexylamine, the problems of large dosage of cyclohexylamine and low yield in the existing technology are solved, and a high-purity, high-yield product is achieved. and process simplification, suitable for industrial production.

CN102827104AInactive Publication Date: 2012-12-19KEMAI CHEM
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Patent Information

Application Number
CN201210361986.6
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2012-09-25
Publication Date
2012-12-19
Estimated Expiration
Not applicable · inactive patent

AI Technical Summary

Technical Problem

In the existing synthesis method of rubber vulcanization accelerator CZ, a large amount of cyclohexylamine is used and the yield is low, and the cyclohexylamine needs to be recovered by distillation, which is a complicated process and affects industrial application.

Method used

Using sodium hypochlorite as the oxidant and M-Na salt as the raw material, react with sulfuric acid and cyclohexylamine at 50°C to generate M-cyclohexylamine salt, and add sodium hypochlorite dropwise at a flow rate of 5 ml/min until the end of the reaction, and then pump Filter, wash and dry, eliminating the need for cyclohexylamine recovery and acidification processes.

Benefits of technology

A rubber vulcanization accelerator CZ with small dosage of cyclohexylamine, high product purity and high yield has been realized, which simplifies the process flow and improves the convenience of industrial application. The purity reaches more than 99% and the yield reaches more than 97%.

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Abstract

The invention discloses a method for synthesizing a rubber vulcanization accelerator CZ by a two-step process by using sodium hypochlorite as an oxidizer, which comprises the following steps: weighing 150-300g of 98% sulfuric acid, preparing into 10-30% sulfuric acid, adding the 10-30% sulfuric acid into a reaction kettle filled with 100-800g of cyclohexylamine, reacting the sulfuric acid and the cyclohexylamine at 20-80 DEG C at the rotation speed of 200-1000 rpm, dropwisely adding 200-1000ml of M-Na salt, dropwisely adding 8.0-18.0% oxidizer sodium hypochlorite at the flow rate of 20-100ml / minute for 1.0-3.0 hours, judging the reaction end point with starch iodide test paper, and stopping the dropwise addition of the sodium chlorate when the test paper becomes black; and after the reaction finishes, carrying out vacuum filtration, washing with water, filtering, and drying to obtain the rubber accelerator CZ product. The method is simple, and can easily implement industrialization; and the purity of the synthesized accelerator CZ is up to higher than 99%, and the yield is up to higher than 97%.
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