Check patentability & draft patents in minutes with Patsnap Eureka AI!

Preparation method of p-phenylenediamine

A technology of p-phenylenediamine and p-dichlorobenzene, which is applied in the field of synthesis of p-phenylenediamine, can solve the problems of low atom utilization rate, cumbersome synthesis of raw materials, increased equipment investment, etc., and achieves low cost, easy separation and recovery, The effect of long catalyst life

Inactive Publication Date: 2019-06-18
JIANGSU YANGNONG CHEM GROUP +2
View PDF7 Cites 1 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] Among the above synthetic routes, route one is the main method of industrialization at present, with mature technology, high yield and good selectivity, but the raw material p-nitroaniline needs to be obtained by nitration of chlorobenzene and ammonolysis, the synthesis of raw materials is cumbersome, the utilization rate of atoms is low, and the nitration The process is seriously polluted; the raw material of route 2 is easy to obtain, and can be directly obtained by benzene chlorination, with high atomic utilization rate and low pollution, but high temperature and high pressure must be used in the ammonolysis process to increase equipment investment, and there are potential safety hazards

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

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Preparation method of p-phenylenediamine
  • Preparation method of p-phenylenediamine
  • Preparation method of p-phenylenediamine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Add 117.72g p-dichlorobenzene (99.9%, 0.8mol) in 1L autoclave, 437.14g ammoniacal liquor (35%, 9.0mol), 19.16g copper ferrite (99.9%, 0.08mol), feed intake complete, be warming up to 130 ℃, stirring speed 600rpm, heat preservation reaction 6hr, pressure 2.2-2.5MPa, after the reaction, after cooling down and releasing the pressure to recover ammonia, 25.21g of copper ferrite was recovered by hot filtration at 60℃, and the filtrate was desolvated and negative pressure distillation to obtain 77.15g of Phenylenediamine, content 99.9%, yield 89.2%.

[0020] Apply mechanically recovery copper ferrite catalyst, repeat above-mentioned reaction process, catalyst apply mechanically 3 times, reaction situation is as follows.

[0021] Table 1 reclaims the reaction result 1 of nano-copper ferrite

[0022]

Embodiment 2

[0024] In 1L autoclave, add 58.86g p-dichlorobenzene (99.9%, 0.4mol), 302.3g water (45%, 8.0mol), 0.48g copper ferrite (99.9%, 0.002mol), after feeding, the temperature is raised to 150 ℃, stirring speed 600rpm, heat preservation reaction 10hr, pressure 4.2-4.8MPa, after the reaction, after cooling down and releasing the pressure to recover ammonia, 0.82g of copper ferrite was recovered by hot filtration at 80℃, and the filtrate was desolvated and negative pressure distilled to obtain 39.18g of Phenylenediamine, content 99.9%, yield 90.6%.

[0025] Apply mechanically recovery copper ferrite catalyst, repeat above-mentioned reaction process, catalyst apply mechanically 3 times, reaction situation is as follows.

[0026] Table 2 reclaims the reaction result 2 of nano-copper ferrite

[0027]

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 provides an efficient preparation method of p-phenylenediamine. According to the method, the p-phenylenediamine is prepared by taking p-dichlorobenzene and ammonia water as raw materialsand nano copper ferrite as a catalyst. Compared with a reported method, the method uses the nano copper ferrite as a catalyst, meanwhile has a bimetallic catalytic effect of iron and copper, and hasstrong catalytic activity. The temperature and pressure of reaction are reduced, and reaction conditions are mild; and after the reaction is finished, the catalyst can be recycled only by conventionalfiltration. The physical and chemical properties of the recycled nano copper ferrite are not changed, and the service life of the catalyst is long. The cost is low, and separation and recycling are facilitated; and the p-phenylenediamine is recyclable and environmentally friendly.

Description

technical field [0001] The invention belongs to the field of organic synthesis, and in particular relates to a preparation method for synthesizing p-phenylenediamine by using p-dichlorobenzene as a raw material. Background technique [0002] p-Phenylenediamine, also known as Wuersi D, is one of the simplest aromatic diamines, with a white to lavender crystal appearance, a melting point of 140°C, a boiling point of 264°C, and a relative density of 1.21. Slightly soluble in cold water, soluble in hot water, easily soluble in alcohol, ether and chloroform. As a traditional chemical intermediate, it is widely used in dyestuff, rubber, national defense and other industries. Azo dyes can be produced in the dye industry, rubber antioxidants can be produced in the rubber industry, and para-aramid fibers can be produced in the national defense industry. In addition, p-phenylenediamine is also the main raw material of gasoline polymerization inhibitor and photographic developer. At...

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
IPC IPC(8): C07C209/10C07C211/51
CPCY02P20/584
Inventor 刘补娥丁克鸿徐林王怡明顾峰孙伟许少文
Owner JIANGSU YANGNONG CHEM GROUP
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

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2025 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com