Unlock instant, AI-driven research and patent intelligence for your innovation.

Method for preparing p-phenylenediamine

A technology of p-phenylenediamine and p-chloroaniline, which is applied to the preparation of amino compounds, chemical instruments and methods, and the preparation of organic compounds, and can solve the problems of high price and high cost

Inactive Publication Date: 2015-01-21
王晓伟
View PDF0 Cites 3 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This process effectively solves the problem of environmental pollution, but the biggest disadvantage of this process is the use of expensive noble metal catalysts, which are very expensive

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

[0016] In a 1L high-pressure amination reaction kettle, add 1mol of p-chloroaniline, slowly introduce 4mol of liquid ammonia, and 100ml of dichloroethane, stir evenly, and react for 10 hours at a pressure of 3.0MPa and a temperature of 100°C. After the reaction, cool to room temperature. After the reaction, cool to room temperature, release the pressure to 0.2MPa, press the reactant into the washing tank with water to wash, remove ammonium chloride, and obtain p-phenylenediamine with a yield of 90.1%. The purity is above 98%.

Embodiment 2

[0018] In a 1L high-pressure amination reaction kettle, add 1mol of p-chloroaniline, slowly introduce 5mol of liquid ammonia, and 100ml of dichloroethane, stir evenly, and react at a pressure of 3.0MPa and a temperature of 100°C for 10 hours. After the reaction, cool to room temperature. After the reaction, cool to room temperature, release the pressure to 0.2MPa, press the reactant into the washing kettle with water to wash, remove ammonium chloride, and obtain p-phenylenediamine with a yield of 92.6%. The purity is above 98%.

Embodiment 3

[0020] In a 1L high-pressure amination reaction kettle, add 1mol of p-chloroaniline, slowly introduce 6mol of liquid ammonia, and 100ml of dichloroethane, stir well, and react for 7 hours at a pressure of 5.0MPa and a temperature of 150°C. After the reaction, cool to room temperature. After the reaction, cool to room temperature, release the pressure to 0.2MPa, press the reactant into the water washing tank with water to wash, remove ammonium chloride, and obtain p-phenylenediamine with a yield of 95.3%. The purity is above 98%.

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 belongs to the technical field of fine chemical engineering and mainly relates to a preparation method of p-phenylenediamine. The preparation method comprises the following steps: adding p-chloroanniline into a high-pressure amination kettle, blowing liquefied ammonia, carrying out thermal insulation and reacting for 5-10 h at the temperature 100-200 DEG C and at the pressure of 3.0-5.0 MPa, cooling to room temperature after the end of the reaction, releasing pressure to 0.2 MPa, pumping reactants into a washing kettle by the use of a pump and washing the reactants, and removing ammonium chloride so as to obtain p-phenylenediamine.

Description

technical field [0001] The invention belongs to the field of fine chemicals and relates to a method for preparing p-phenylenediamine from p-chloroaniline. Background technique [0002] P-phenylenediamine is an important organic chemical raw material, which is generally used in the production of dyes, rubber antioxidants, etc. The traditional production method of p-phenylenediamine is to use p-nitrochlorobenzene as raw material, react with ammonia water (or ammonia gas) under high temperature and high pressure conditions to prepare p-nitroaniline, and p-nitroaniline is then reduced to produce p-nitroaniline by alkali sulfide or iron powder The crude p-phenylenediamine is purified by recrystallization to prepare high-purity p-phenylenediamine. The biggest defect of this process is that there is a lot of industrial waste water, and the reduction of iron powder will also produce a large amount of iron sludge, which seriously pollutes the environment. Moreover, the purity of p-p...

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): C07C209/10C07C211/51
Inventor 王晓伟
Owner 王晓伟