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Process route for continuously synthesizing diphenylguanidine

A technology of diphenylguanidine and aniline, applied in the field of organic synthesis, to achieve the effects of high yield, good purity and reduced reaction cost

Inactive Publication Date: 2015-03-04
HEBEI LINGANG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It not only solves the quality problem of diphenylguanidine, but also reduces the production cost of diphenylguanidine and improves the reaction efficiency

Method used

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  • Process route for continuously synthesizing diphenylguanidine

Examples

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Effect test

example 1

[0033] Feed aniline and water into the tubular reactor at a speed of 20 g / min. The purified cyanogen chloride is contacted and reacted in the tubular reactor, the residence time of aniline in the tubular reactor is 2 minutes, and the temperature of the tubular reactor is 170°C. The crude product flows out from the tubular filter and is then filtered, neutralized with 10% sodium hydroxide to pH ≈ 7.0, washed and dried to obtain a diphenylguanidine product. The yield of diphenylguanidine is 96.5%, and the content is 99.71%.

example 2

[0035] Aniline and ethanol are fed into the tubular reactor at a rate of 20 g / min. In the tubular reactor, the purified cyanogen chloride is contacted and reacted. The residence time of aniline in the tubular reactor is 2 minutes, and the temperature of the tubular reactor is 160°C. The crude product flows out from the tubular filter and is then filtered, neutralized with 10% sodium hydroxide to pH ≈ 7.0, washed and dried to obtain a diphenylguanidine product. The yield of diphenylguanidine is 97.2%, and the content is 99.42%.

example 3

[0037] Aniline and toluene were fed into the tubular reactor at a rate of 20 g / min. In the tubular reactor, the purified cyanogen chloride is contacted and reacted. The residence time of aniline in the tubular reactor is 2.5 minutes, and the temperature of the tubular reactor is 170°C. The crude product flows out from the tubular filter and is then filtered, neutralized with 10% sodium hydroxide to pH ≈ 7.0, washed and dried to obtain a diphenylguanidine product. The yield of diphenylguanidine is 97.5%, and the content is 99.02%.

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Abstract

The invention relates to a process route for continuously synthesizing diphenylguanidine. The process route for continuously synthesizing diphenylguanidine comprises the steps of with phenylamine and cyan chloride as raw materials, continuously pressing phenylamine into a tubular reactor, and carrying out contact reaction on phenylamine and purified cyan chloride in the tubular reactor so as to synthesize diphenylguanidine hydrochloride; preparing diphenylguanidine by carrying out continuous steps of decontamination, crystallization and the like. The continuous reaction disclosed by the invention has the advantages that the reaction time is shortened, the reaction efficiency is increased, and the like.

Description

technical field [0001] The invention relates to the synthesis of guanidine compounds, especially diphenylguanidine, and belongs to the field of organic synthesis. Background technique [0002] Diphenylguanidine is an important rubber accelerator, mainly used as a vulcanization accelerator for natural rubber and synthetic rubber. It can also be used as an activator for thiazole thiurams and sulfenamide accelerators. It is used for continuous vulcanization when used together with accelerators DM and TMTD. Has anti-aging properties. Commonly used for natural rubber and synthetic rubber, not suitable for latex. Mainly used in the manufacture of tires, rubber sheets, rubber shoes and other rubber industrial products. [0003] The main manufacturers in my country include Shandong Shanxian Chemical Co., Ltd., Tianjin Organic Chemical No. 1 Factory, Northeast Auxiliary Chemical Co., Ltd., etc. Major foreign manufacturers include Monsanto in the United States, Bayer in the Feder...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C279/18C07C277/08
Inventor 王振宇姚立国程丽华李正杰李成果董津李娟郭翠红彭艳丽
Owner HEBEI LINGANG CHEM
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