Method for separating and comprehensively utilizing nitrobenzene chlorides

A technology of nitrobenzene dichloride and chloride is applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., and can solve the problems of waste of resources, pollution, difficulty in separation of nitrobenzene chloride, etc. Bring economic benefits and solve the effect of environmental pollution

Inactive Publication Date: 2009-12-30
淮安嘉诚高新化工股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The separation of nitrobenzene chloride is quite difficult, the separation cost is high and the separation is incomplete, and has no economic value; the direct utilization of the ...

Method used

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  • Method for separating and comprehensively utilizing nitrobenzene chlorides
  • Method for separating and comprehensively utilizing nitrobenzene chlorides
  • Method for separating and comprehensively utilizing nitrobenzene chlorides

Examples

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example 1

[0027] Put nitrobenzene monochloride, DMF solvent, and anhydrous potassium fluoride into a stirred reactor, use hexadecyltrimethylammonium bromide as a phase transfer catalyst, and control the temperature at 160-180°C for heat preservation reaction , after the reaction is completed, steam distillation is carried out to separate the organic layer, the water layer is incorporated into the next steam distillation, and the organic layer is rectified to obtain the finished products o-, p-nitrofluorobenzene and m-nitrochlorobenzene.

example 2

[0029] (1), using the o- and p-nitrofluorobenzenes obtained in Example 1 as raw materials, using ferric chloride as a catalyst, put them into a chlorination kettle, feed chlorine gas, and control the reaction temperature at 80-95 ° C, and detect with GC Chlorination depth, remove residual chlorine and hydrogen chloride gas after the reaction, and obtain 2-fluoro-5-chloronitrobenzene and 3-chloro-4-fluoronitrobenzene through rectification;

[0030] (2), raise the temperature of the kettle to 200-220 ° C, feed chlorine gas, and continuously add the mixture of 2-fluoro-5-chloronitrobenzene and 3-chloro-4-fluoronitrobenzene that was prepared in the previous step, drop The acceleration is equivalent to the evaporation rate, and the bottom liquid in the reactor is recycled, and more than 80% of the crude product of 2,4-dichlorofluorobenzene is evaporated, and the crude product is rectified, and the fraction at 170-172 ° C is collected to obtain 2 with a purity of more than 99.5%. 4-...

example 3

[0032] (1), nitrobenzene dichloride is dropped in the reaction kettle, with DMF as solvent, Potassium fluoride is fluorinating agent, is the mixture that is 90% with quaternary ammonium salt content and 10% quaternary phosphonium salt content as catalyst, React at 175-185°C to generate 3-chloro-4-fluoronitrobenzene, 2-fluoro-5-chloronitrobenzene and potassium chloride, remove potassium chloride by filtration, and then obtain 3-chloro-4-fluoronitrobenzene through rectification and 2-fluoro-5 chloronitrobenzene mixture;

[0033] (2), raise the temperature of the kettle to 200-220 ° C, feed chlorine gas, and continuously add the mixture of 2-fluoro-5-chloronitrobenzene and 3-chloro-4-fluoronitrobenzene that was prepared in the previous step, drop The acceleration is equivalent to the evaporation rate, and the bottom liquid in the reactor is recycled, and more than 80% of the crude product of 2,4-dichlorofluorobenzene is evaporated, and the crude product is rectified, and the frac...

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Abstract

The invention discloses a method for separating and comprehensively utilizing nitrobenzene chlorides, which comprises the separation and comprehensive utilization of monochloride and the comprehensive utilization of dichloride, wherein the monochloride is subjected to fluorine substituted reaction to separate m-nitrochlorobenzene, o-fluoronitrobenzene and dinitro-fluorobenzene, and the o-fluoronitrobenzene and the dinitro-fluorobenzene are taken as products for sale, or a mixture is subjected to chlorination to generate 2,4-dichlor fluorbenzene with higher economic value; and the dichloride is subjected to chlorination to generate the 2,4-dichlor fluorbenzene with higher economic value. The method improves the yield of the m-nitrochlorobenzene on the one hand, and utilizes the resources with low economic value to produce the product with higher economic value by steps of reasonable chemical reaction and separation, brings economic benefit to enterprises and solves environmental pollution problem on the other hand.

Description

technical field [0001] The invention relates to a separation and comprehensive utilization method of a mixture, in particular to a separation and comprehensive utilization method of nitrobenzene chloride. Background technique [0002] Domestic production of m-nitrochlorobenzene is made from nitrobenzene and chlorine gas in the presence of catalysts. The conversion rate of nitrobenzene is 40%, and the selectivity of m-nitrochlorobenzene is 72.6%. The chlorination solution contains 60% nitrobenzene, 29% m-nitrochlorobenzene, and 4% p-nitrochlorobenzene. Benzene, 6.3% o-nitrochlorobenzene and 1.6% dichloronitrobenzene. Nitrobenzene, m-nitrochlorobenzene, nitrobenzene monochloride and nitrobenzene dichloride are separated from the chlorinated solution through processes such as water washing, neutralization, and rectification. Nitrobenzene monochloride and dichloride are collectively referred to as nitrobenzene chloride; nitrobenzene monochloride refers to a mixture of three is...

Claims

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Application Information

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IPC IPC(8): C07C205/12C07C201/16C07C201/12C07C25/13C07C17/093
Inventor 王士玉
Owner 淮安嘉诚高新化工股份有限公司
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