Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Process for preparing relevent aniline kind compound of ammonolysis of partial nitro benzene halide kind compound

A technology of aniline compounds and nitrohalobenzene, which is applied in the field of preparation of organic compounds, can solve problems such as poor safety, low product purity, and excessive sulfur-containing waste water in waste gas, and achieve good economic and social benefits, process simplification, The effect of less investment

Inactive Publication Date: 2013-02-27
YANCHENG SHIHONG CHEM
View PDF2 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, to prepare m-nitroaniline compounds, m-dinitrobenzene compounds are usually obtained by nitration, and then refined and purified, and then incompletely reduced, and one of the nitro groups is reduced to an amino group. The disadvantage is that it is safe The dinitration of benzene is an extremely dangerous production process, and there have been many major accidents reported. Secondly, the product isomers obtained by nitration are difficult to separate, and the product purity is not high, resulting in high production costs.
The iron powder method is not easy to stir evenly, is highly corrosive, has serious corrosion of equipment, discharges a lot of waste residue and wastewater, is difficult to control the reduction end point, and has a low yield; High temperature and high pressure equipment, dangerous operation, limited by quality hydrogen source

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
  • Process for preparing relevent aniline kind compound of ammonolysis of partial nitro benzene halide kind compound
  • Process for preparing relevent aniline kind compound of ammonolysis of partial nitro benzene halide kind compound
  • Process for preparing relevent aniline kind compound of ammonolysis of partial nitro benzene halide kind compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Add 34.2g of 4-chloro-2-nitrotoluene and 100g of water into a 1L stainless steel autoclave, add 100g of liquid ammonia under airtight conditions; then raise the temperature and pressurize to 200-240°C, 5-6MPa, and react for 14 hours . According to HPLC analysis, the raw material peak disappeared, cooled to 30°C, filtered, washed with water, purified, and dried to obtain 23.6g of 4-amino-2-nitrotoluene with a purity of 99.0% and a yield of 83.6%. Ammonia water is recovered for reuse.

Embodiment 2

[0022] Add 34.2g of 6-chloro-2-nitrotoluene, 150g of 18% ammonia water recovered in Example 1, and 1g of CuCl into a 1L stainless steel autoclave, add 34.5g of liquid ammonia under airtight conditions, heat up and pressurize to 200- 240°C, 5-6MPa, react for 10 hours. According to HPLC analysis, the raw material peak disappeared, cooled to 30°C, filtered, washed with water, and dried to obtain 25.7g of 6-amino-2-nitrotoluene with a purity of 99.2% and a yield of 91.1%.

Embodiment 3

[0024] Add 34.2g of 6-chloro-2-nitrotoluene, 100g of water, 1g of CuCl and 1g of tetrabutylammonium bromide into a 1L stainless steel autoclave, add 100g of liquid ammonia under airtight conditions, raise the temperature and pressurize to 200-240 ℃, 5~6MPa, react for 7 hours. According to HCLP analysis, the raw material peak disappeared, cooled to 30°C, filtered, washed with water, and dried to obtain 26.1g of 6-amino-2-nitrotoluene with a purity of 99.3% and a yield of 92.5%.

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

This invention provides a preparation method of aminolysising partial nitro halogen benzene compound to obtain corresponding aniline compounds. The process is mixing partial nitro halogen benzene compound with water, adding ammonia under the conditions of a confine, and taking reaction under140-300deg C, 3-15MPa, then gain the aniline compounds. The mole ratio of partial nitro halogen benzene compounds and ammonia is 1:7 ~ 200, the ammonia concentration of 20 ~ 55% (m / m). The reaction mixture can also add appropriate catalyst and dispersant. The invention process is simplification, less investment, low cost, safe, reliable, low pollution, and high yield, with good economic and social benefits.

Description

Technical field [0001] The invention relates to a method for preparing organic compounds, in particular to a method for preparing corresponding aniline compounds by ammonolysis of part of nitrohalobenzene compounds. Background technique [0002] Aniline compounds are important organic intermediates. The preparation of corresponding aniline compounds by ammonolysis of halogen on the benzene ring has many studies and applications, such as the preparation method of o-nitroaniline with the Chinese patent application number 200410023991.1, which discloses a kind of o-nitrochlorinated benzene and Ammonia water is carried out ammonification reaction, then adds the method for preparing o-nitroaniline of caustic; -4,6-Dinitrochlorobenzene is obtained as a dinitrochlorobenzene derivative by ammoniation treatment in the presence of an anionic active dispersant in an aqueous medium or an aqueous-organic medium at a temperature of 86-90°C The method of 2-bromo-4,6-dinitroaniline; "Dye ...

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 Patents(China)
IPC IPC(8): C07C209/10C07C211/52
Inventor 李松跃朱立家
Owner YANCHENG SHIHONG CHEM
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products