Preparation method of supported nickel-based catalyst for synthesizing chloroaniline through selective hydrogenation of chloronitrobenzene

A chloronitrobenzene, nickel-based catalyst technology, applied in the preparation of amino compounds, the preparation of organic compounds, metal/metal oxide/metal hydroxide catalysts and other directions, can solve the problem of expensive, difficult to recover, easy to deactivate and other problems, to achieve the effects of low production cost, low dechlorination performance and simple preparation process

Inactive Publication Date: 2017-03-29
NORTHWEST UNIV(CN)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] Some problems existing in these synthesis methods at present: Although noble metals such as Pt and Pd have high hydrogenation activity and are beneficial to the hydrogenation reaction of chloronitrobenzene, they are expensive, difficult to recycle and easy to deactivate, which is not conducive to industrial application. Non-precious metal catalysts have good catalytic activity and low cost, and have good industrial application value

Method used

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  • Preparation method of supported nickel-based catalyst for synthesizing chloroaniline through selective hydrogenation of chloronitrobenzene
  • Preparation method of supported nickel-based catalyst for synthesizing chloroaniline through selective hydrogenation of chloronitrobenzene
  • Preparation method of supported nickel-based catalyst for synthesizing chloroaniline through selective hydrogenation of chloronitrobenzene

Examples

Experimental program
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Effect test

Embodiment 1

[0032] The preparation method of the supported nickel catalyst for the selective catalytic hydrogenation of chloronitrobenzene comprises the following steps:

[0033] (1) First, γ-Al 2 o 3 Roast at 500°C for 5h;

[0034] (2) Weigh 2g of γ-Al after roasting 2 o 3 and 0.9908g nickel nitrate (Ni(NO 3 ) 2 ·6H 2 O) Add it to 50mL of ethylene glycol, raise the temperature to 90°C under stirring, keep it for 30min, then add 0.2mol / L Na2 CO 3 The aqueous solution was brought to pH=9-10 to obtain a suspension.

[0035] The suspension was aged at 25°C for 2 hours, filtered and washed until the filtrate was neutral, then dried at 120°C for 12 hours, and ground through a 100-mesh sieve to obtain a solid powder;

[0036] (3) Calcining the obtained solid powder in air at 400° C. for 4 hours to obtain a catalyst precursor.

[0037] (4) Place the obtained catalyst precursor in a tubular heating furnace and reduce it under a high-purity hydrogen atmosphere with a flow rate of 20mL / min...

Embodiment 2

[0041] Steps (1)-(2) are the same as in Example 1.

[0042] (3) Calcining the obtained solid powder at 500° C. for 4 hours to obtain a catalyst precursor.

[0043] (4) Place the obtained catalyst precursor in a tubular heating furnace and reduce it under a high-purity hydrogen atmosphere with a flow rate of 20mL / min. The reduction temperature is 300°C and the reduction time is 1h. A supported nickel catalyst for the selective hydrogenation of benzene, designated Cat-2.

[0044] The evaluation of the above-mentioned catalysts is the application of the catalysts:

[0045] Under the conditions of 100°C, hydrogen pressure 2.0Mpa, 1.0000g o-chloronitrobenzene, 0.4000g Cat-2 catalyst, and 20mL absolute ethanol, react for 120min to obtain o-chloroaniline. The reaction results are shown in Table 1.

[0046] figure 1 (a) is NiO / γ-Al after calcination at 500°C for 4 hours (i.e. Example 2) 2 o 3 SEM spectra of catalyst precursors. Observing the SEM image of the sample, it can be s...

Embodiment 3

[0049] Steps (1)-(2) are the same as in Example 1.

[0050] (3) Calcining the obtained solid powder at 600° C. for 4 hours to obtain a catalyst precursor.

[0051] (4) Place the obtained catalyst precursor in a tubular heating furnace and reduce it under a high-purity hydrogen atmosphere with a flow rate of 20mL / min. The reduction temperature is 300°C and the reduction time is 1h. A supported nickel catalyst for the selective hydrogenation of benzene, designated Cat-3.

[0052] The evaluation of the above-mentioned catalysts is the application of the catalysts:

[0053] Under the conditions of 100°C, hydrogen pressure 2.0Mpa, 1.0000g o-chloronitrobenzene, 0.4000g Cat-3 catalyst, and 20mL absolute ethanol, react for 120min to obtain o-chloroaniline. The reaction results are shown in Table 1.

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Abstract

The invention discloses a preparation method of a supported nickel-based catalyst for synthesizing chloroaniline through selective hydrogenation of chloronitrobenzene. The preparation method comprises the following steps: firstly roasting a carrier, adding the roasted carrier and nickel salt into a solvent for mixing, heating the mixture while stirring, and then dropping a precipitator till the pH value is equal to 6 to 12 to obtain a suspension; carrying out static aging on the suspension obtained in the step (1), filtering and washing the suspension till the filtrate is neutral, drying the filtrate, and roasting in air at the temperature of 200 to 800 DEG C for 2 to 6 hours to obtain a catalyst precursor; and reducing the catalyst precursor under a condition of feeding H2 and N2 mixed gas or feeding H2 at the reducing temperature of 200 to 800 DEG C for 0.5 to 4 hours to obtain the supported nickel-based catalyst for synthesizing chloroaniline through selective hydrogenation of chloronitrobenzene. The catalyst has the advantages of low production cost, simple preparation process, short preparation period and little pollution, is high in reaction performance for synthesizing chloroaniline through selective hydrogenation of chloronitrobenzene, and is low in dechlorination performance.

Description

technical field [0001] The present invention relates to a catalyst, in particular to a method for preparing a supported nickel-based catalyst for the selective hydrogenation of chloronitrobenzene to synthesize chloroaniline. The catalyst is particularly suitable for the hydrogenation of chloronitrobenzene to synthesize chloroaniline Reaction. Background technique [0002] Chloroaniline, the hydrogenation product of chloronitrobenzene, is an important organic intermediate, which plays an important role in the synthesis of fine chemical products such as medicine, pesticide, dye, and pigment. There are many industrial processes for synthesizing chloroanilines, but the vast majority of chloroanilines are produced through the reduction of chloronitrobenzene, which makes the reduction of chloronitrobenzene to prepare chloroanilines an important organic synthesis unit reaction. At present, several methods such as iron powder reduction, alkali sulfide or hydrazine hydrate reduction...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/755C07C209/36C07C211/52
CPCB01J23/755C07C209/365C07C211/52
Inventor 李爽吴彤彤王鹏星
Owner NORTHWEST UNIV(CN)
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