Method for preparing o-chloroaniline by adopting microchannel reaction device

A technology of micro-channel reaction and micro-channel reactor, which is applied in the preparation of amino compounds, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems of decreased reaction selectivity, large amount of catalyst, catalyst poisoning, etc., to reduce errors , Efficiency improvement, full contact effect

Active Publication Date: 2014-03-26
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003]CN1660774A uses catalysts such as Ru/C, amorphous NiB, Ni-Fe-B, Ni-Co-B, etc., and the amount of catalyst is 10-20% of the amount of raw materials , using ethanol as a solvent, the hydrogen obtained by cracking with alcohol is used for hydrogenation reaction, but the amount of catalyst required for the reaction in this patent is very large,...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Methanol and palladium-carbon catalyst are pumped into the reaction system via a slurry pump, hydrogen is fed and the pressure required for the reaction is adjusted to 0.7MPa, and the temperature of the constant temperature system is adjusted to the reaction temperature of 70°C, the o-nitrochlorobenzene is 0.0254mol / min Feed, the hydrogen flow rate is 1SL / min, the reaction time is 3.2s, after the reaction, sampling and analysis, the selectivity is 62%.

Embodiment 2

[0019] Methanol and skeletal nickel catalyst are pumped into the reaction system through a slurry pump, hydrogen is fed and the pressure required for the reaction is adjusted to 0.7MPa, the temperature of the constant temperature system is adjusted to the reaction temperature of 90°C, the o-nitrochlorobenzene is 0.0223mol / min Feed, the hydrogen flow rate is 1SL / min, the reaction time is 3.2s, after the reaction, sampling and analysis, the selectivity is 66%.

Embodiment 3

[0021] Methanol and palladium-carbon catalyst are pumped into the reaction system through a slurry pump, hydrogen is fed and the pressure required for the reaction is adjusted to 0.7MPa, and the temperature of the constant temperature system is adjusted to the reaction temperature of 110°C, and the o-nitrochlorobenzene is at 0.0180mol / min Feeding, the hydrogen flow rate is 0.4SL / min, the reaction time is 8.0s, after the reaction, sampling and analysis, the selectivity is 68%.

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Abstract

The invention belongs to the technical field of fine chemical engineering, and relates to a method for preparing o-chloroaniline by adopting liquid-phase catalytic hydrogenation of o-nitrochlorobenzene. A microchannel reaction device is adopted in reaction, and ortho-nitrochlorobenzene, a solvent and a catalyst react with hydrogen by adopting a slurry feeding mode at 50-150 DEGC under the pressure of 0.5-1.2MPa, so as to obtain the o-chloroaniline. The preparation technology of the o-chloroaniline has the advantages that feed is continuous, the reaction condition is flexible to change, mass transfer effect is good, a reactant fully contacts with a catalyst, the side reaction is reduced, and the like.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, and relates to a new preparation method of o-chloroaniline, in particular to a preparation method of o-chloroaniline using a microchannel reaction device. Background technique [0002] O-chloroaniline is an important organic chemical raw material and intermediate, which occupies an important position in the chemical and industrial production of dyes, pesticides, medicines, rubber additives, synthetic resins, spices, photographic medicines, etc. Its production is the synthesis of fine chemicals It is an important field, and its synthesis method has also become a research hotspot this year. At present, domestic manufacturers mainly use the hydrogenation method, but new patents have been published on the research on its synthesis method. [0003] CN1660774A Catalysts such as Ru / C, amorphous NiB, Ni-Fe-B, Ni-Co-B, catalyst consumption is 10-20% of raw material consumption, with ethanol as sol...

Claims

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Application Information

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IPC IPC(8): C07C211/52C07C209/36
Inventor 张帆黄伟管庆宝
Owner CHINA PETROLEUM & CHEM CORP
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