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Continuous liquid-phase catalytic hydrogenation reduction method for production of o-chloroaniline

An o-chloroaniline, liquid-phase catalysis technology, applied in chemical instruments and methods, chemical recovery, organic chemistry, etc., to achieve the effects of short process, enhanced mass transfer, and simple equipment

Inactive Publication Date: 2013-10-23
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

[0003] The purpose of the present invention is to: provide a continuous liquid-phase catalytic hydrogenation reduction method for producing o-chloroaniline, so as to solve many defects in the intermittent hydrogenation reduction process

Method used

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  • Continuous liquid-phase catalytic hydrogenation reduction method for production of o-chloroaniline

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Embodiment 1: produce o-chloroaniline according to the following steps

[0014] (1) Check the airtightness of the production device, make preparations before starting up, and lay the bottom material; then put a certain amount of Raney nickel catalyst into each hydrogenation tank to ensure that the hydrogenation tank is adjacent to nitrochloride The weight ratio of benzene to the catalyst reaches 3%, and then replaced with nitrogen and hydrogen in sequence;

[0015] (2) Start the material delivery pump, continuously send o-nitrochlorobenzene, methanol and additives into the 1# hydrogenation tank, and control the flow of each material; then continuously feed hydrogen, under the conditions of 50 ° C and 1.0 MPa Carry out hydrogenation reaction; part of the reaction materials in the 1# hydrogenation tank is circulated between the heat exchange mixer, injector and 1# hydrogenation tank through the 1# circulation pump, so that o-nitrochlorobenzene can be fully converted into ...

Embodiment 2

[0016] Embodiment 2: produce o-chloroaniline according to the following steps

[0017] (1) Check the airtightness of the production device, make preparations before starting up, and lay the bottom material; then put a certain amount of Raney nickel catalyst into each hydrogenation tank to ensure that the hydrogenation tank is adjacent to nitrochloride The weight ratio of benzene to the catalyst reaches 3%, and then replaced with nitrogen and hydrogen in sequence;

[0018] (2) Start the material delivery pump, continuously send o-nitrochlorobenzene, methanol and additives into the 1# hydrogenation tank, and control the flow of each material; then continuously feed hydrogen, under the conditions of 60°C and 1.0MPa Carry out hydrogenation reaction; part of the reaction materials in the 1# hydrogenation tank is circulated between the heat exchange mixer, injector and 1# hydrogenation tank through the 1# circulation pump, so that o-nitrochlorobenzene can be fully converted into o-c...

Embodiment 3

[0019] Embodiment 3: produce o-chloroaniline according to the following steps

[0020] (1) Check the airtightness of the production device, make preparations before starting up, and lay the bottom material; then put a certain amount of Raney nickel catalyst into each hydrogenation tank to ensure that the hydrogenation tank is adjacent to nitrochloride The weight ratio of benzene to the catalyst reaches 3%, and then replaced with nitrogen and hydrogen in sequence;

[0021] (2) Start the material delivery pump, continuously send o-nitrochlorobenzene, methanol and additives into the 1# hydrogenation tank, and control the flow of each material; then continuously feed hydrogen, under the conditions of 70 ° C and 1.0 MPa Carry out hydrogenation reaction; part of the reaction materials in the 1# hydrogenation tank is circulated between the heat exchange mixer, injector and 1# hydrogenation tank through the 1# circulation pump, so that o-nitrochlorobenzene can be fully converted into ...

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Abstract

The invention discloses a continuous liquid-phase catalytic hydrogenation reduction method for production of o-chloroaniline. The method is characterized in that (1) multi-kettle cascade reaction is adopted during the hydrogenation reaction process, a No.1 hydrogenation kettle is provided with a heat exchange mixer and an injector, part of reaction materials circulate among the heat exchange mixer, the injector and the No.1 hydrogenation kettle through a circulating pump so as to fully convert o-nitrochlorobenzene to o-chloroaniline; and (2) a cyclone hydraulic separator is installed at the back of each hydrogenation reaction vessel to separate a catalyst in a hydrogenation liquid, and the separated catalyst returns to a corresponding hydrogenation kettle through the circulating pump for recycling. The process flow of the method is short; equipment used is simple; and defects of large investment of batch production, low utilization rate of equipment, large labor intensity, short service life of the catalyst, large loss of hydrogen and solvents, large fatigue strength of hydrogenation equipment and short service life are solved.

Description

technical field [0001] The invention relates to a method for producing o-chloroaniline, in particular to a method for producing o-chloroaniline through continuous liquid-phase catalytic hydrogenation reduction. Background technique [0002] O-chloroaniline is an important organic chemical intermediate, widely used in polyurethane, pesticide, medicine and dye industries. At present, the production of o-chloroaniline mostly adopts a batch-type hydrogenation reduction process, that is, o-nitrochlorobenzene is used as a raw material, methanol is used as a solvent, and the reaction temperature and pressure are controlled in the presence of a Raney nickel catalyst and an auxiliary agent. O-chloroaniline products can be obtained by hydrogenation reduction. In the intermittent hydrogenation reduction process, every batch of material produced must undergo pressure testing, replacement, reaction and then return to the original state. This repeated intermittent production requires lar...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/52C07C209/36
CPCY02P20/584
Inventor 石祖嘉章燕军徐登建沈学军王凤珠
Owner 淮安嘉诚高新化工股份有限公司
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