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Method for preparing rubber vulcanization accelerator CBS by using microchannel reactor

A microchannel reactor and rubber vulcanization technology, applied in the field of fine chemical product production, can solve the problems of large influence of batch human operation factors, environmental pollution, unstable quality, etc., and achieve good industrial application prospects, high safety performance, The effect of shortened reaction time

Inactive Publication Date: 2017-06-06
山东斯递尔化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The sodium hypochlorite oxidation method is a relatively traditional method, which produces more saline wastewater, which is difficult to post-treatment and causes environmental pollution due to discharge.
In the industry, large reactors are used for intermittent production, and the batches are greatly affected by human operation factors, resulting in unstable quality

Method used

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  • Method for preparing rubber vulcanization accelerator CBS by using microchannel reactor
  • Method for preparing rubber vulcanization accelerator CBS by using microchannel reactor
  • Method for preparing rubber vulcanization accelerator CBS by using microchannel reactor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Take 1 mol of accelerator M and add 1.2 mol of cyclohexylamine to make a solution, then take 1.25 mol of hydrogen peroxide, drive the two-phase solution through the flow pump and enter the reactor with a coil diameter of 5 mm through the Y mixer. The flow rate of the microreactor is 5mL / min, the residence time of the reaction liquid in the reactor is 5min, and the reaction temperature is 40°C. After one cycle, the reaction solution was collected. The yield was determined to be 94.9%, the melting point was 99.2°C, and the appearance was off-white powder.

Embodiment 2

[0034] Take 1 mol of accelerator M and add 1.5 mol of cyclohexylamine to prepare a solution, then take 1.5 mol of hydrogen peroxide, and drive the two-phase solution through the flow pump to enter the reactor with a coil diameter of 5 mm through the Y mixer. The flow rate of the microreactor is 5mL / min, the residence time of the reaction liquid in the reactor is 5min, and the reaction temperature is 40°C. After one cycle, the reaction solution was collected. The yield was determined to be 89.2%, the melting point was 98.5°C, and the appearance was off-white powder.

Embodiment 3

[0036] Take 1 mol of accelerator M and add 1.8 mol of cyclohexylamine to prepare a solution, then take 1.5 mol of hydrogen peroxide, and drive the two-phase solution through the flow pump to enter the reactor with a coil diameter of 5 mm through the Y mixer. The flow rate of the microreactor is 10mL / min, the residence time of the reaction liquid in the reactor is 5min, and the reaction temperature is 45°C. After one cycle, the reaction solution was collected. The yield was determined to be 87.2%, the melting point was 98.5°C, and the appearance was off-white powder.

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Abstract

The invention relates to the field of fine chemical product production, in particular to a method for preparing a rubber vulcanization accelerator CBS by using a microchannel reactor. In the method for preparing the rubber vulcanization accelerator CBS by using the microchannel reactor, the microchannel reactor consisting of a micro mixer and a micro reactor which are connected together is included. The method is characterized by comprising the following steps: dissolving an accelerator M into excessive cyclohexylamine to form a solution, introducing cyclohexylamine together with an oxidant into a micro mixer for mixing, and feeding into the micro reactor for an oxidation reaction; and after the reaction is completed, performing suction filtration, washing filter cakes with water, and drying, thereby obtaining the rubber vulcanization accelerator CBS. As the microchannel reactor is adopted to prepare the rubber vulcanization accelerator CBS, the reaction time and the reaction temperature can be precisely controlled, the reaction time can be shortened, the reaction conversion rate can be increased, high throughput can be achieved, the product quality can be stable, production can be enlarged, high security can be achieved, and defects of a conventional reaction kettle can be effectively overcome.

Description

[0001] (1) Technical field [0002] The invention belongs to the production field of fine chemical products, in particular to a method for preparing a rubber vulcanization accelerator CBS by using a microchannel reactor. [0003] (2) Background technology [0004] Rubber vulcanization accelerator CBS, also called rubber vulcanization accelerator CZ, chemical name is N-cyclohexyl-2-benzothiazole sulfenamide, molecular formula: C 13 h 16 N 2 S 2 , relative molecular mass is 264.41, this product is off-white or light yellow powder, melting point 90~108℃. Non-toxic, specific gravity 1.27~1.30, soluble in benzene, chloroform, carbon tetrachloride, ethyl acetate, acetone, slightly soluble in ethanol and gasoline, insoluble in water. The storage is stable for half a year. It is easy to agglomerate, but it does not affect the use. It is easy to gradually decompose when heated for a long time. The decomposition is aggravated when it is above 60°C or under vacuum conditions. It shoul...

Claims

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Application Information

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IPC IPC(8): C07D277/80
CPCC07D277/80
Inventor 朱嘉震尹传祥赵新远李海存田旭赵文超
Owner 山东斯递尔化工科技有限公司
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