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Preparation method of phenylhydrazine

A technology for phenylhydrazine and phenylhydrazine hydrochloride, which is applied in the fields of hydrazine preparation, organic chemistry, etc., can solve the problems of complex production process, many reaction steps, environmental pollution, etc., and achieves simple operation, few reaction steps, and low consumption of raw materials. Effect

Inactive Publication Date: 2017-06-13
李亚杉
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

To prepare phenylhydrazine by diazotization reaction, the intermediate diazonium salt is unstable and easy to decompose, and needs to be carried out under low temperature conditions. There are many reaction steps, complex production process, high energy consumption, and the product yield is only about 80%. Many products will produce a large amount of organic wastewater, which is easy to pollute the environment

Method used

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  • Preparation method of phenylhydrazine

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Experimental program
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Effect test

Embodiment 1

[0012] Put 343g of monochloramine solution with a concentration of 15% into a four-necked flask equipped with a stirring, thermometer and reflux condensation device, then add 186g of aniline to the four-necked flask, start stirring, and control the reaction temperature at 50°C. Reaction 6 After standing for 1 hour, the upper oil phase containing aniline was separated from the reaction solution to obtain phenylhydrazine hydrochloride solution; the concentration of 30% sodium hydroxide solution 160g was slowly added to the phenylhydrazine hydrochloride solution , stirred at a temperature of 50°C for 1 hour, and after standing still for 5 hours, the aqueous solution of the lower layer was separated to obtain 99.4 g of phenylhydrazine.

Embodiment 2

[0014] Put 258g of monochloramine solution with a concentration of 20% into a four-necked flask equipped with stirring, a thermometer and a reflux condensing device, then add 168g of aniline to the four-necked flask, start stirring, and control the reaction temperature at 65°C. After standing for 1 hour, the upper oil phase containing aniline was separated from the reaction solution to obtain phenylhydrazine hydrochloride solution; 210 g of sodium hydroxide solution with a concentration of 25% was slowly added to the phenylhydrazine hydrochloride solution , stirred at a temperature of 55°C for 1 hour, and after standing still for 5 hours, the aqueous solution of the lower layer was separated to obtain 100.5 g of phenylhydrazine.

Embodiment 3

[0016] Put 206 g of monochloramine solution with a concentration of 25% into a four-necked flask equipped with a stirring, thermometer and reflux condensing device, then add 140 g of aniline to the four-necked flask, start stirring, and control the reaction temperature at 80 ° C. Reaction 3 After standing for 1 hour, the upper oil phase containing aniline was separated from the reaction solution to obtain phenylhydrazine hydrochloride solution; the concentration of 20% sodium hydroxide solution 300g was slowly added to the phenylhydrazine hydrochloride solution , stirred at a temperature of 60° C. for 1 hour, and after standing still for 5 hours, the aqueous solution of the lower layer was separated to obtain 98.3 g of phenylhydrazine.

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Abstract

The invention discloses a preparation method of phenylhydrazine. The method comprises the following steps: taking monochloramine and aniline to react, so as to prepare phenylhydrazine hydrochloride; neutralizing the phenylhydrazine hydrochloride with alkali liquid to prepare the phenylhydrazine. Compared with a traditional method for preparing the phenylhydrazine through a diazotization reaction process, the method provided by the invention has the advantages of moderate reaction conditions, few reaction steps, simplicity in operation, a few of byproducts, low energy consumption, high yield, less consumption of raw materials and low production cost, and is a novel energy-saving and environment-friendly process.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a preparation method of phenylhydrazine. Background technique [0002] Phenylhydrazine is a white monoclinic prism crystal or oily liquid, slightly soluble in water, has an aromatic smell, and gradually oxidizes in the air to turn yellow. Phenylhydrazine is used in the production of pesticides to synthesize the intermediate 1-phenylsemicarbazide of the organophosphorus insecticide triazophos and the intermediate 1-phenyl-3,6-dihydroxypyridazine of pyridazine, which is also bactericidal In addition, as an organic synthesis raw material, phenylhydrazine is also used as an intermediate in dyes, pharmaceuticals and other industries, and is also used as an analytical reagent. It can react with the aldehyde and ketone groups of sugars to form stable glycosides, and use the crystal form and melting point of glycosides to identify different reducing sugars. [00...

Claims

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Application Information

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IPC IPC(8): C07C243/22C07C241/02
CPCC07C241/02C07C243/22
Inventor 李亚杉
Owner 李亚杉
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