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Method for synthesizing rubber vulcanization accelerator CZ

A technology of vulcanization accelerator and synthetic rubber, which is applied in the direction of organic chemistry, can solve the problem of low yield of accelerator CZ, and achieve the effect of saving the recovery process, easy industrialization, and simple process

Inactive Publication Date: 2014-01-29
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

[0011] Take 15 grams of 98% sulfuric acid, 38 grams of 27.5% hydrogen peroxide, and 18.9 grams of water as an oxidizing agent. According to the molar ratio of cyclohexylamine:M-Na salt is 1:1, add 0.3 moles of cyclohexylamine to the reactor, , rotating speed is, under the condition of 600 revs / min, add 0.3 mol of M-Na salt dropwise with the flow velocity of 1.5 mmol / min, dropwise add oxidant simultaneously, the speed and amount of oxidant addition are based on the sulfuric acid mole number in the oxidant 0.75 mmol / min 0.15 moles were added dropwise at a flow rate of 2 hours. After the reaction was completed, suction filtration, washing, filtration, and drying were performed to obtain the rubber accelerator CZ product. The purity of the accelerator CZ reached 98.5%, and the yield reached 97%.

example 2

[0013] Take 15 grams of 98% sulfuric acid, 39.9 grams of 27.5% hydrogen peroxide, and 18.9 grams of water as an oxidizing agent. According to the molar ratio of cyclohexylamine:M-Na salt is 1:1, add 0.3 moles of cyclohexylamine to the reaction kettle, at 40 ° C , rotating speed is, under the condition of 900 revs / min, drip M-Na salt 0.3 mol with the flow velocity of 2.0 mmol / min, dropwise add oxidant simultaneously, oxidant drip speed and amount are sulfuric acid molar number 1.0 mmol / m in oxidant 0.15 moles were added dropwise at a flow rate of 2.5 hours for 2.5 hours. After the reaction was completed, the rubber accelerator CZ product was obtained by suction filtration, water washing, filtration, and drying. The purity of the accelerator CZ reached 98.5%, and the yield reached 97%.

example 3

[0015] Take 15 grams of 98% sulfuric acid, 42.7 grams of 27.5% hydrogen peroxide, and 18.9 grams of water as an oxidizing agent. According to the molar ratio of cyclohexylamine:M-Na salt is 1:1, add 0.3 moles of cyclohexylamine to the reaction kettle, and add 0.3 moles of cyclohexylamine to the reaction kettle. , rotating speed is, under the condition of 1200 revs / min, add 0.3 mole of M-Na salt dropwise with the flow rate of 2.5 mmol / min, dropwise add oxidant simultaneously, the speed and amount of oxidant addition are sulfuric acid mole number in oxidant 1.25 mmol / min 0.15 moles were added dropwise at a flow rate of 3 hours, and after the reaction was completed, suction filtration, washing, filtration, and drying were performed to obtain the rubber accelerator CZ product. The purity of the accelerator CZ reached 98.5%, and the yield reached 97%.

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Abstract

The invention discloses a method for synthesizing a rubber vulcanization accelerator CZ. In the method, hydrogen peroxide and sulfuric acid are mixed to serve as an oxidant, and an M-Na salt and cyclohexylamine serve as raw materials. The method is characterized by comprising the following steps of preparing the oxidant according to the molar ratio of sulfuric acid to hydrogen peroxide to water being 1: 2.05-2.3:7; adding cyclohexylamine into a reaction kettle, dripping the M-Na salt at a flow velocity of 1.5-2.5 millimole / min at the temperature of 30-60 DEG C under the condition that the rotating speed is 600-1200 revolutions per minute, and simultaneously dripping 0.15 mol of oxidant, wherein the molar ratio of cyclohexylamine to the M-Na salt is 1:1, the dripping speed and amount of the oxidant are based on the molar ratio of sulfuric acid in the oxidant to the M-Na salt of 1:2, and the dripping time is 2-3 hours; after the reaction is finished, performing suction filtration, washing, filtering and drying to obtain the rubber vulcanization accelerator CZ. The purity of the accelerator CZ is 98.5 percent, the yield is 97 percent, and the method is simple in process and easy for industrial production.

Description

technical field [0001] The invention relates to a new synthesis method of a rubber vulcanization accelerator N-cyclohexyl-2-benzothiazole sulfenamide (CZ), which belongs 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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Patent Type & Authority Applications(China)
IPC IPC(8): C07D277/80
CPCC07D277/80
Inventor 李树东
Owner KEMAI CHEM
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