Device and method for production of o-chloroaniline through continuous catalytic hydrogenation reduction of o-nitro chloro benzene

A technology of o-nitrochlorobenzene and o-chloroaniline, which is applied in the field of o-chloroaniline continuous catalytic hydrogenation reduction to produce o-chloroaniline, can solve the problem of large consumption of catalysts and dechlorination inhibitors, and inconvenient catalyst regeneration and replacement. Convenience, poor catalyst selectivity and other problems, to achieve good heat transfer effect, uniform hydrogenation reaction, high utilization effect

Inactive Publication Date: 2014-10-15
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 method has poor catalyst selectivity, high dechlorination rate, poor product yield, large consumption of catalyst and dechlo

Method used

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  • Device and method for production of o-chloroaniline through continuous catalytic hydrogenation reduction of o-nitro chloro benzene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Example 1: Put ortho-nitrochlorobenzene, platinum-carbon (Pt / C) catalyst with a mass percentage of 1% platinum, and diethylamine dechlorination inhibitor into the hydrogenation reactor to lay out the primer, and use nitrogen to purify the system. The air is replaced cleanly, and then the nitrogen is replaced with hydrogen; then the feed valve is opened, and o-nitrochlorobenzene and dechlorination inhibitors are continuously sent into the hydrogenation reactor, wherein o-nitrochlorobenzene, noble metal catalyst, dechlorination The mass ratio of the inhibitor is 1:0.001:0.001, hydrogen gas is introduced to carry out the hydrogenation reduction reaction, the hydrogenation reaction temperature is 60°C, and the pressure is 0.5MPa; the hydrogenation liquid mixed with the catalyst in the hydrogenation reactor enters first through the circulation pump The heat exchanger removes the heat of reaction to maintain the reaction temperature of the system, and then passes through the c...

Embodiment 2

[0023] Example 2: Put o-nitrochlorobenzene, platinum-carbon (Pt / C) catalyst with 3% mass percentage of platinum, and triethanolamine dechlorination inhibitor into the hydrogenation reactor to arrange the bottom material, and nitrogen in the system The air is replaced cleanly, and then the nitrogen is replaced with hydrogen; then the feed valve is opened, and o-nitrochlorobenzene and dechlorination inhibitor are continuously sent into the hydrogenation reactor, wherein o-nitrochlorobenzene, noble metal catalyst, dechlorination inhibitor The mass ratio of the catalyst is 1:0.003:0.003, and hydrogen gas is introduced to carry out the hydrogenation reduction reaction. The hydrogenation reaction temperature is 80°C and the pressure is 1.0MPa; The heater removes the heat of reaction to maintain the reaction temperature of the system, and then through the cross-flow filter, the catalyst and part of the hydrogenated liquid enter the injector together with fresh o-nitrochlorobenzene and...

Embodiment 3

[0024] Example 3: Put o-nitrochlorobenzene, platinum-carbon (Pt / C) catalyst with 5% mass percentage of platinum, and pyridine dechlorination inhibitor into the hydrogenation reactor to arrange the primer, and use nitrogen to purify the air in the system. The replacement is clean, and then the nitrogen is replaced with hydrogen; then the feed valve is opened, and the o-nitrochlorobenzene and the dechlorination inhibitor are continuously sent into the hydrogenation reactor, wherein the o-nitrochlorobenzene, the noble metal catalyst, the dechlorination inhibitor The mass ratio of the hydrogenation reactor is 1:0.005:0.005, and hydrogen is introduced to carry out the hydrogenation reduction reaction. The hydrogenation reaction temperature is 100°C and the pressure is 1.5MPa; the hydrogenation liquid mixed with the catalyst in the hydrogenation reactor first enters the heat exchange through the circulating pump The device removes the reaction heat to maintain the reaction temperatur...

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Abstract

The invention discloses a device and method for production of o-chloroaniline through continuous catalytic hydrogenation reduction of o-nitro chloro benzene. The method comprises the following steps: o-nitro chloro benzene, a catalyst and a dechlorination inhibitor are put into a hydrogenation reactor, and bottom materials are distributed well; nitrogen and hydrogen are sequentially used for displacing a system completely; a feed valve is opened, the o-nitro chloro benzene and the dechlorination inhibitor are continuously fed into the hydrogenation reactor, wherein the mass ratio of the o-nitro chloro benzene to the catalyst to the dechlorination inhibitor is 1:(0.001-0.005):(0.001-0.005); hydrogen is fed into the hydrogenation reactor for hydrogenation reaction, wherein the reaction temperature is 60-100 DEG C and the pressure is 0.5-1.5 MPa; hydrogenated liquid enters a heat exchanger firstly through a circulating pump and then passes through a cross-flow filter; the catalyst and part of hydrogenated liquid as well as fresh raw materials together enter an ejector for circulation, and the other part of the hydrogenated liquid is extracted out continuously, and o-chloroaniline is obtained after treatment. The device and the method disclosed by the invention have advantages that the production cycle is short, the catalyst selectivity is high, the dechlorination rate is low, the yield is high, the quality is stable, the equipment efficiency is high and continuous production is realized.

Description

technical field [0001] The invention relates to an o-chloroaniline production device and method, in particular to a device and method for producing o-chloroaniline through continuous catalytic hydrogenation reduction of o-nitrochlorobenzene. Background technique [0002] O-chloroaniline is an important organic chemical intermediate, widely used in polyurethane, pesticide, medicine and dye industries. O-chloroaniline is produced by reduction of o-nitrochlorobenzene. Traditional reduction methods include iron powder reduction, alkali sulfide reduction, electrolytic reduction and catalytic hydrogenation reduction. Due to heavy pollution and high energy consumption, the iron powder reduction method and the alkali sulfide reduction method have been included in the list of eliminated processes in my country; the electrolytic reduction method has a large investment in equipment and high energy consumption; the catalytic hydrogenation reduction method has a short process flow and lo...

Claims

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Application Information

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IPC IPC(8): C07C211/52C07C209/36
Inventor 石祖嘉沈学军龚雷章燕军臧维东郭奎
Owner 淮安嘉诚高新化工股份有限公司
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