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Preparation method of continuously synthesized rubber vulcanization accelerator CBS

A technology of vulcanization accelerator and synthetic rubber, applied in chemical instruments and methods, organic chemistry, chemical/physical process, etc., can solve the problems of difficult recovery of cyclohexylamine, high activity of hydrogen peroxide, large salt-containing wastewater, etc. The effect of phase mass transfer rate, environmental protection, and reaction rate improvement

Inactive Publication Date: 2021-02-05
SHANDONG YANGGU HUATAI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the traditional method of synthesizing CBS mostly adopts sodium hypochlorite oxidation method, which has mature technology, simple equipment and easy operation, but it is difficult to recover cyclohexylamine during the synthesis process, and a large amount of saline wastewater is produced, causing environmental pollution
Although the oxygen catalytic oxidation method has the advantages of being green and environmentally friendly, it can greatly reduce the waste water production and is beneficial to environmental protection, but due to the high activity of hydrogen peroxide, there are many side reactions in the oxidation process, resulting in a low conversion rate.

Method used

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  • Preparation method of continuously synthesized rubber vulcanization accelerator CBS
  • Preparation method of continuously synthesized rubber vulcanization accelerator CBS
  • Preparation method of continuously synthesized rubber vulcanization accelerator CBS

Examples

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Effect test

Embodiment 1

[0035] A preparation method for continuously synthesizing a rubber vulcanization accelerator CBS, utilizing a capillary microreactor to continuously synthesize a rubber vulcanization accelerator CBS under ultrasonic action, which specifically includes the following steps:

[0036] Step 1, completely dissolve 2-mercaptobenzothiazole in organic solvent, the mass ratio of 2-mercaptobenzothiazole to organic solvent is 1:3~7, the mixing time of 2-mercaptobenzothiazole and organic solvent is 10min ~30min, stir evenly to obtain a mixture;

[0037] Step 2, according to 2-mercaptobenzothiazole: cyclohexylamine: H 2 o 2 The molar ratio is 1:1~3:1.5~4, and the mixed liquid, cyclohexylamine, and hydrogen peroxide in step 1 are fed into the capillary microreactor 1 through the micro mixer according to a certain feed rate for oxidation reaction, and the oxidation reaction time is 5s ~30s. The concentration of the hydrogen peroxide solution is 10wt%-20wt%, and the capillary microreactor 1...

Embodiment 2

[0041] A preparation method for continuously synthesizing a rubber vulcanization accelerator CBS, utilizing a capillary microreactor to continuously synthesize a rubber vulcanization accelerator CBS under ultrasonic action, which specifically includes the following steps:

[0042] Step 1, completely dissolve 2-mercaptobenzothiazole in organic solvent, the mass ratio of 2-mercaptobenzothiazole to organic solvent is 1:5, the mixing time of 2-mercaptobenzothiazole and organic solvent is 15min, stir Uniformly, a mixed solution is obtained;

[0043]Step 2, according to 2-mercaptobenzothiazole: cyclohexylamine: H 2 o 2 The molar ratio is 1:1.5:2.5. The mixed solution, cyclohexylamine, and hydrogen peroxide in step 1 are entered into the capillary microreactor 1 through the micro mixer according to a certain feed rate for oxidation reaction. The oxidation reaction time is 15s. Device 1 enters the capillary microreactor for oxidation reaction, wherein the concentration of hydrogen p...

Embodiment 3

[0047] A preparation method for continuously synthesizing a rubber vulcanization accelerator CBS, utilizing a capillary microreactor to continuously synthesize a rubber vulcanization accelerator CBS under ultrasonic action, which specifically includes the following steps:

[0048] Step 1, weigh 30g of 2-mercaptobenzothiazole and 150g of ethyl acetate, completely dissolve 2-mercaptobenzothiazole in methyl acetate, stir and mix at room temperature for 15min, stir evenly to obtain a mixed solution, and set aside;

[0049] Step 2, weigh 26.73g cyclohexylamine, 109.3g mass fraction of 12% hydrogen peroxide solution in two beakers, set aside; turn on the ultrasonic cleaner, immerse the capillary microreactor 1, the inner diameter of the capillary microreactor 1 It is 0.6mm and made of stainless steel. The temperature of the ultrasonic water bath 2 is controlled at 40°C, and then the mixture of 2-mercaptobenzothiazole and ethyl acetate, cyclohexylamine, and hydrogen peroxide solution ...

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Abstract

The invention discloses a preparation method of a continuously synthesized rubber vulcanization accelerator CBS, which belongs to the technical field of rubber vulcanization accelerators, and particularly relates to a preparation method of a continuously synthesized rubber vulcanization accelerator CBS. The method is characterized in that the rubber vulcanization accelerator CBS is continuously synthesized by using a capillary microreactor under the ultrasonic action, and the method comprises the following steps of 1, completely dissolving 2-mercaptobenzothiazole in an organic solvent to obtain a mixed solution, 2, enabling the 2-mercaptobenzothiazole, cyclohexylamine and H2O2 to enter a capillary microreactor according to a molar ratio of 1: (1-3): (1.5-4), and carrying out an oxidation reaction, wherein the ultrasonic water bath temperature of the capillary microreactor is 25-50 DEG C, and 3, after the oxidation reaction is finished, recovering the solvent and collecting a product toobtain the rubber vulcanization accelerator CBS. The method has the positive effects that side reactions are reduced, the product quality and yield are improved, a large amount of salt-containing wastewater is prevented from being generated, the cost is saved, and the environment is protected.

Description

technical field [0001] The invention belongs to the technical field of rubber vulcanization accelerators, in particular to a preparation method of a continuous synthetic rubber vulcanization accelerator CBS. Background technique [0002] Accelerator CBS, also known as accelerator CZ or N-cyclohexyl-2-benzothiazole sulfenamide, is one of the important varieties of sulfenamide accelerators. It is a highly flexible post-effect accelerator with excellent scorch resistance, safe processing and short vulcanization time. It is widely used in the manufacture of industrial rubber products such as tires, rubber hoses, rubber shoes, and cables. There are many types of rubber vulcanization accelerators, and there are many synthetic methods. At present, the traditional method of synthesizing CBS mostly adopts the sodium hypochlorite oxidation method, which has mature technology, simple equipment and easy operation, but it is difficult to recover cyclohexylamine during the synthesis proc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D277/80B01J19/00C08K5/47
CPCC07D277/80B01J19/0093C08K5/47
Inventor 王克军宋彦哲杜孟成韩涛黄存影徐思明孟祥克杜嘉乐
Owner SHANDONG YANGGU HUATAI CHEM
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