Method for producing o-chloroaniline

A technology of o-chloroaniline and a production method is applied in the field of liquid-phase catalytic hydrogenation of o-chloroaniline to produce o-chloroaniline, and can solve the problems of difficult continuous industrial production, decreased catalyst activity, large catalyst dosage, etc., and achieves simplified operation and high catalyst dosage. Reduced, low-cost effects

Inactive Publication Date: 2008-12-31
淮安嘉诚高新化工股份有限公司
View PDF0 Cites 30 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The pollution in the first two synthesis methods is serious, the energy consumption of the electrolysis method is high, the catalyst consumption of the hydrogen transfer method is large, and the cost of methanol i

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

example 1

[0011] Example 1, add 350g o-nitrochlorobenzene, 12g Raney nickel (water content 20%), 12g monoethanolamine, 350g methyl alcohol in 1L stainless steel autoclave, close reactor, replace air 3 times with nitrogen, then replace 3 times with hydrogen Once, start stirring, raise the temperature to 60°C, start to flow hydrogen, the reaction pressure is 0.8MPa, until the hydrogen pressure no longer drops, take out the reaction solution, separate the catalyst, and analyze the content of each component by gas chromatography. The results show that the o-nitro The conversion rate of chlorobenzene is 100%, the selectivity of o-chloroaniline is 98%, and the aniline content is 2%.

example 2

[0012] Example 2, add 350g o-nitrochlorobenzene, 3g Raney nickel (water content 20%), 12g monoethanolamine, 350g methyl alcohol in 1L stainless steel autoclave, close reactor, replace air 3 times with nitrogen, then replace 3 times with hydrogen Once, start stirring, raise the temperature to 60°C, start to flow hydrogen, the reaction pressure is 0.8MPa, until the hydrogen pressure no longer drops, take out the reaction solution, separate the catalyst, and analyze the content of each component by gas chromatography. The results show that the o-nitro The conversion rate of chlorobenzene is 85%, the selectivity of o-chloroaniline is 70%, and the selectivity of aniline is 25.5%.

example 3

[0013] Example 3, feed 0.4kg / h o-nitrochlorobenzene, 0.4kg / h99% methanol, 0.016kg / h hydrogen into three 5L stainless steel reactors connected in series with self-priming stirring at 60°C and 0.8MPa , 0.012kg / h monoethanolamine, 0.001kg / h Raney nickel, the content of each component is analyzed by gas chromatography, the results show that the conversion rate of o-nitrochlorobenzene is 99.7%, and the selectivity of o-chloroaniline is 99.82% , Aniline selectivity 0.18%.

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

An o-chloroaniline production method takes o-nitrochlorobenzene as raw material and is characterized in that the o-nitrochlorobenzene is dissolved in alcohol solvent in the presence of catalyst and additive and reacted with hydrogen at 10-120 DEG C and under 0.3-4.0 MPa; the reaction process is continuous reaction; after the completion of the reaction, the o-chloroaniline is obtained through treatment, wherein, the catalyst can be selected from one of the following: Ni/Al2O3, Raney Ni, Pt/C and Pd/C; while the additive can be selected from one, or two, or three of the following compounds: cyclohexylamine, ethylenediamine, ethanolamine, diethanolamine, triethanolamine, pyridine, liquid ammonia, ammonium bicarbonate, ammonium carbonate, sodium carbonate, sodium bicarbonate, potassium bicarbonate, potassium carbonate, potassium hydrogen phosphate, potassium dihydrogen phosphate, sodium hydrogen phosphate and sodium dihydrogen phosphate; the dosage of the catalyst takes up 0.05% to 20% of the mass of the o-nitrochlorobenzene; the dosage of the additive takes up 0. 5% to 20% of the mass of the o-nitrochlorobenzene; the alcohol can be methanol or ethanol; the dosage of alcohol takes up 30% to 150% of the dosage of the o-nitrochlorobenzene; the continuous reaction is realized through 1 to 6 tank reactors which are connected in series.

Description

(1) Technical field [0001] The invention relates to a production method of o-chloroaniline, in particular to a method for producing o-chloroaniline by liquid-phase catalytic hydrogenation of o-chloroaniline. (2) Background technology [0002] O-Chloroaniline is an important chemical intermediate in medicine, pesticide, dyestuff, fragrance and polyurethane industry, with a wide range of uses. The synthesis methods of o-chloroaniline include iron powder reduction method, alkali sulfide reduction method, electrolytic reduction method, catalytic hydrogenation method, and hydrogen transfer method. The pollution in the first two synthesis methods is serious, the energy consumption of the electrolysis method is high, the catalyst consumption of the hydrogen transfer method is large, and the cost of methanol is high. [0003] The main problem of catalytic hydrogenation is that hydrodechlorination and tank-type hydrogenation are difficult for continuous industrial production. Dechl...

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): C07C209/36C07C211/52
Inventor 王士玉
Owner 淮安嘉诚高新化工股份有限公司
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

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

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap