Supercharge Your Innovation With Domain-Expert AI Agents!

Method for preparing phenylhydrazine

A technology for phenylhydrazine and phenol, applied in the field of preparing phenylhydrazine, can solve the problems of many reaction steps, easy decomposition and high cost, and achieve the effects of less by-products and wastes, mild reaction conditions and low production cost

Inactive Publication Date: 2018-06-22
张晓玲
View PDF0 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Synthesis of phenylhydrazine by diazotization reaction, the intermediate diazonium salt is unstable and easy to decompose, it needs to be carried out under low temperature conditions, the reaction steps are many, the production process is complicated, the energy consumption is high, and the total yield is only about 80%. There are many products and wastes, and a large amount of organic salty wastewater will be produced. Environmental protection treatment is difficult and costly, and it is easy to pollute the environment.

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Put 188g of phenol, 166.7g of hydrazine hydrate with a content of 90% and 37.6g of HD-8 macroporous resin into a four-neck flask equipped with stirring, thermometer and rectification column, start stirring, and heat up to 110°C-120°C. Extract water vapor at the rectification column top temperature of 98°C to 100°C, take samples for analysis after 6 to 8 hours of reaction, end the reaction when the phenol content in the reaction liquid is lower than 0.3%, and then recover excess hydrazine hydrate by vacuum distillation, hydration After the recovery of hydrazine, the HD-8 macroporous resin was separated with a centrifugal filter device, and the remaining liquid was washed with an appropriate amount of sodium carbonate solution and pure water to obtain 199.2 g of phenylhydrazine.

Embodiment 2

[0014] Put 188g of phenol, 184.2g of hydrazine hydrate with a content of 95% and 56.4g of HD-8 macroporous resin into a four-necked flask equipped with a stirring, thermometer and rectification column, start stirring, and heat up to 110°C to 120°C. Extract water vapor at the rectification column top temperature of 98°C to 100°C, take samples for analysis after 6 to 8 hours of reaction, end the reaction when the phenol content in the reaction liquid is lower than 0.3%, and then recover excess hydrazine hydrate by vacuum distillation, hydration After the recovery of hydrazine, the HD-8 macroporous resin was separated with a centrifugal filter device, and the remaining liquid was washed with an appropriate amount of sodium carbonate solution and pure water to obtain 206.3 g of phenylhydrazine.

Embodiment 3

[0016] Put 188g of phenol, 202g of hydrazine hydrate with a content of 99%, and 18.8g of HD-8 macroporous resin into a four-necked flask equipped with a stirring, thermometer and rectification column, start stirring, and heat up to 110°C to 120°C. The rectification column top temperature is 98 ℃ ~ 100 ℃ to extract water vapor, after 6 ~ 8 hours of reaction, sampling analysis, when the content of phenol in the reaction liquid is less than 0.3%, the reaction is ended, and then the excess hydrazine hydrate is recovered by vacuum distillation, hydrazine hydrate After recovery, the HD-8 macroporous resin was separated with a centrifugal filter device, and the remaining liquid was washed with an appropriate amount of sodium carbonate solution and pure water to obtain 201.8 g of phenylhydrazine.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention discloses a method for preparing phenylhydrazine. The method uses phenol and hydrazine hydrate as raw materials, and uses HD-8 macroporous strong acid cation exchange resin as a catalyst, a reaction is performed at a certain temperature to prepare the phenylhydrazine, the hydrated hydrazine is kept excess in the reaction system to make the phenol reacted fully, water formed by the reaction is continuously separated and removed in the reaction process, after the reaction is completed, reduced-pressure distillation is performed to recover the hydrazine hydrate, the catalyst is recovered, the remaining liquid is washed by using a sodium carbonate solution and pure water, and therefore a finished product of the phenylhydrazine is obtained. Compared with a traditional diazotization reaction process for synthesizing the phenylhydrazine, the method provided by the invention has mild reaction conditions, less reaction steps, simple operation, less by-products and waste and low energy consumption, the yield is 90% or more, the catalyst can be recycled, the production costs are low, and the method is a novel energy-saving environmentally-friendly process.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a method for preparing phenylhydrazine. Background technique [0002] Phenylhydrazine is a white monoclinic prism crystal or oily liquid, slightly soluble in water, with a melting point of 19.5°C and a boiling point of 243.5°C. It has an aromatic smell and gradually oxidizes to yellow in air. 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 g...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): C07C241/02C07C243/22
CPCY02P20/584C07C241/02C07C243/22
Inventor 张晓玲
Owner 张晓玲
Features
  • R&D
  • Intellectual Property
  • Life Sciences
  • Materials
  • Tech Scout
Why Patsnap Eureka
  • Unparalleled Data Quality
  • Higher Quality Content
  • 60% Fewer Hallucinations
Social media
Patsnap Eureka Blog
Learn More