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Location nitration process for chlorobenzene

A technology of chlorobenzene and nitric acid, applied in the preparation of nitro compounds, organic chemistry, etc., can solve the problems of high energy consumption, environmental pollution, etc., and achieve the effects of simple recovery, rich rare earth resources, and good economic benefits

Inactive Publication Date: 2005-07-06
SOUTHEAST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Solve the problem that it is difficult to increase the content of ortho-nitrobenzene in the product by changing the reaction conditions, such as reaction temperature, reactant ratio, reaction time, etc. when directly using nitric acid for nitration at home and abroad; use water-soluble Lewis acid Instead of concentrated sulfuric acid, it solves the problem of heavy use of concentrated sulfuric acid as a catalyst in the traditional mixed acid nitration, which causes serious pollution to the environment and consumes a lot of energy due to the recovery of waste acid in production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0023] Chlorobenzene (3mmol, 0.31ml), 1,2-dichloroethane 5ml and 65% nitric acid (3mmol, 0.29g) were added to the reactor and mixed, and the catalyst La(OSO 2 CF 3 ) 3 (176 mg, 10% mol) was heated to reflux and stirred, the reaction temperature was controlled at 80° C., and the heating was stopped after 10 hours of reaction. The mixture was washed with water and then extracted with chloroform, spin-dried on a rotary evaporator, and passed through a column. Obtained 435 mg of yellow oily liquid with a yield of 92%, and the relative ratio detected by gas chromatography was 1.59.

example 2

[0025] Chlorobenzene (3mmol, 0.31ml), 1,2-dichloroethane 5ml and 65% nitric acid (3mmol, 0.29g) were added to the reactor and mixed, and the catalyst Nd(OSO2 CF 3 ) 3 (177 mg, 10% mol) was heated to reflux and stirred, the reaction temperature was controlled at 80° C., and the heating was stopped after 10 hours of reaction. The mixture was washed with water and then extracted with chloroform, spin-dried on a rotary evaporator, and passed through a column. 435mg of yellow oily liquid was obtained, the yield was 92%, and the ratio of o was 1.56 as detected by gas chromatography.

example 3

[0027] Chlorobenzene (3mmol, 0.31ml), 1,2-dichloroethane 5ml and 65% nitric acid (3mmol, 0.29g) were added to the reactor and mixed, and the catalyst Gd(OSO 2 CF 3 ) 3 (181 mg, 10% mol) was heated to reflux and stirred, the reaction temperature was controlled at 80° C., and the heating was stopped after 10 hours of reaction. The mixture was washed with water and then extracted with chloroform, spin-dried on a rotary evaporator, and passed through a column. Obtained 435 mg of yellow oily liquid with a yield of 92%, and the relative ratio detected by gas chromatography was 1.50.

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Abstract

Chlorobenzene located nitrification method is a method for preparing nitro chlorobenzene of an intermediate in fine chemical industry, especially a method for improving the yield of o-nitro chlorobenzene by using water soluble Lewis acid to catalytically nitrifying chlorobenzene. The provided method comprises: nitric acid, chlorobenzene and water soluble Lewis acid catalyst are put into the 1,2-dichloroethane solvent to react at the temperature of 30C. to 100C. with the mol ratio of 1-3í†1í†0.01-0.15, and the reaction time is 3-30 hours, after cooled to room temperature, the mixture is washed by water, extracted by chloroform, dried in the rotary evaporator, separated by chromatographic column to obtain yellow oily liquid. The water soluble Lewis acid catalyst has the molecular formula as follows: Ln(OSO2CF3)3, wherein Ln is Sc or Y or La family rear earth element, or M(OSO2CF3)4, wherein M is Hf or Zr.

Description

technical field [0001] The present invention is a preparation method of fine chemical intermediate-nitrochlorobenzene, especially a method of using water-soluble Lewis acid to catalyze the nitration of chlorobenzene to increase the yield of o-nitrochlorobenzene, which belongs to chemical preparation The technical field of nitrochlorobenzene. Background technique [0002] O- and p-nitrochlorobenzene are important organic chemical raw materials for the production of dyes, pesticides, medicines, and intermediates for rubber additives. Domestic production of nitrochlorobenzene has been in short supply for many years since 1950, and sometimes even a considerable amount of nitrochlorobenzene is imported from abroad to meet the demand of the domestic market. Due to the urgent market demand, nitrochlorobenzene plants were built or expanded in various places in the early 1990s. At present, there are more than 20 manufacturers with a total production capaci...

Claims

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Application Information

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IPC IPC(8): C07C201/08C07C205/12
Inventor 孙岳明王育乔
Owner SOUTHEAST UNIV
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