Catalyst for liquid phase hydrogenation of chloronitrobenzene and preparation method thereof

A technology of nitrobenzene liquid and catalyst, which is applied in the direction of catalyst activation/preparation, preparation of amino compounds, chemical instruments and methods, etc. It can solve the problems of increased catalyst consumption, backward production process of chlorinated aromatic amines, and increased secondary pollution, etc. , to achieve the effect of simple preparation method, conducive to large-scale production, and reduce catalyst cost

Inactive Publication Date: 2011-06-15
CHINA NAT ACAD NANOTECH & ENG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] However, the production process of chlorinated aromatic amines is relatively backward. At present, iron powder and alkali sulfide reduction methods are mainly used in China. Such a process will produce dozens of tons of high-concentration, difficult-to-treat organic sewage and toxic Sludge, a variety of chlorinated organic compounds can pose serious threats to the environment and ecosystem
[0004] Commonly used catalysts include Raney Ni and supported noble metals (such as Pd/C and Pt/Al2O3, etc.), but this method has the disadvantage of hydrogenolysis and dehalogenation. There are two main methods to prevent hydrogenolysis ...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Embodiment 1: take nickel sulfate hexahydrate 1g and add 50ml deionized water to be mixed with nickel sulfate solution, add 5ml ammoniacal liquor in the solution, stir 1 hour; Under ultrasonic action, 0.4g sodium borohydride is added into 10ml deionized water; The sodium borohydride solution was added dropwise to the nickel-containing solution at room temperature, the reaction proceeded immediately and hydrogen gas was released, after the dropwise addition, when no hydrogen gas was released, it was washed with deionized water, and then the obtained black solid was stored in absolute ethanol.

[0021] The prepared catalyst was used in the liquid-phase hydrodechlorination reaction of chlorobenzene, the reaction conditions were: reaction temperature 70°C, pressure 1.0MPa, using a 100ml reactor, adding 0.4g black precipitate NiB as catalyst and 1.0g chlorobenzene, 40ml of absolute ethanol, the rotation speed is 700rpm, and the reaction time is 1 hour; the final result is tha...

Embodiment 2

[0022] Embodiment 2: take nickel chloride 1g and add 50ml deionized water to be mixed with nickel nickel chloride solution, add 10ml ammoniacal liquor in the solution, stir 1 hour; 0.6g potassium borohydride is joined in 10ml deionized water; Potassium borohydride solution was added dropwise to the nickel-containing solution, the reaction proceeded immediately and hydrogen gas was emitted. After the dropwise addition, when no hydrogen gas was released, it was washed with deionized water, and then the obtained black solid was stored in absolute ethanol.

[0023] The prepared catalyst was used in the liquid-phase hydrodechlorination reaction of chlorobenzene, the reaction conditions were: reaction temperature 75°C, pressure 0.9MPa, using a 200ml reactor, adding 0.8g black precipitate NiB as catalyst and 2.0g chlorobenzene, 80ml of absolute ethanol, the rotating speed is 800rpm, and the reaction time is 1.5 hours; the final result shows that the conversion rate of the catalyst chl...

Embodiment 3

[0024] Embodiment 3: take nickel nitrate hexahydrate 1g and add 50ml deionized water to be mixed with nickel nitrate solution, add 10ml ammoniacal liquor in the solution, stir 1 hour; 0.4g sodium borohydride is joined in 10ml deionized water; The sodium hydride solution was added dropwise to the nickel-containing solution, and the reaction proceeded immediately and hydrogen gas was emitted. After the dropwise addition, when no hydrogen gas was released, it was washed with deionized water, and then the obtained black solid was stored in absolute ethanol.

[0025] The prepared catalyst was used in the liquid-phase hydrodechlorination reaction of chlorobenzene, the reaction conditions were: reaction temperature 80°C, pressure 1.2MPa, using a 500ml reactor, adding 2.0g black precipitate NiB as catalyst and 5.0g chlorobenzene, 200ml of absolute ethanol, the rotation speed is 900rpm, and the reaction time is 2 hours; the final result is that the conversion rate of chloronitrobenzene ...

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PUM

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Abstract

The invention discloses a catalyst for liquid phase hydrogenation of chloronitrobenzene and a preparation method thereof. The invention is characterized in that the catalyst consists of amorphous alloy NiB, wherein the mass percentage of Ni is 10 to 80 percent and the mass percentage of B is 20 to 90 percent. The preparation method is an ultrasonic wave-assisted liquid phase reduction method, and comprises the following steps: (1) preparing solution; (2) forming a precipitate; and (3) washing precipitate and storing. The invention has the advantages that: the catalyst has high activity and selectivity; and when the catalyst is used, the chloronitrobenzene conversion rate is over 99 percent and the dechloridation rate is below 4 percent.

Description

(1) Technical field: [0001] The invention relates to a catalyst, in particular to a catalyst for liquid-phase hydrogenation of chloronitrobenzene and a preparation method thereof. (two) background technology: [0002] Chlorinated organic compounds are products in which one or several hydrogen atoms in aliphatic hydrocarbons, aromatic hydrocarbons and their derivatives are replaced by chlorine atoms. A variety of chlorinated hydrocarbons are used as basic raw materials or intermediates for various organic synthesis, and are widely used in industries such as organic chemicals, pesticides, medicines, dyes, etc., thus making the production of chlorinated hydrocarbons very important in the organic chemical industry. Part. [0003] However, the production process of chlorinated aromatic amines is relatively backward. At present, iron powder and alkali sulfide reduction methods are mainly used in China. Such a process will produce dozens of tons of high-concentration, difficult-to...

Claims

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Application Information

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IPC IPC(8): B01J23/755B01J21/02B01J37/16C07C211/52C07C209/36
Inventor 张东
Owner CHINA NAT ACAD NANOTECH & ENG
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