A preparing method and uses of a hydrogenation catalyst

A hydrogenation catalyst and catalyst technology, applied in the preparation of organic compounds, chemical instruments and methods, preparation of amino hydroxyl compounds, etc., can solve the adverse effects of loss, reduction of aminophenol selectivity, catalyst service life and production cost control, etc. problems, to achieve the effect of low cost, simple process and excellent catalytic performance

Inactive Publication Date: 2017-07-14
南通鼎新催化材料科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, in a strongly acidic reaction medium (usually 15wt.% sulfuric acid aqueous solution), the noble metal may be poisoned and the active components will also be lost, which will have a negative impact on the service life of the catalyst and the control of production costs
[0003] In order to improve the production process under such strong acidic conditions, it has also been proposed to use solid acid instead of liquid sulfuric acid to catalyze th

Method used

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  • A preparing method and uses of a hydrogenation catalyst

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Embodiment 1

[0023] (1) Cerium oxide (CeO 2 ) The carrier is crushed and sieved, and 20-40 meshes are selected, and an equal volume of nickel nitrate aqueous solution is impregnated to obtain a sample with a nickel loading of 6wt.%. Calcined at 450°C for 4 hours to obtain ceria-supported nickel oxide (NiO / CeO 2 );

[0024] (2) Take 1g NiO / CeO 2 Put it into a round-bottomed flask, add 2.0g ethylenediamine, 4.0g carbon tetrachloride and 80mL xylene in sequence, first raise the temperature to 90°C for 4 hours, then raise the temperature to 140°C and continue the reaction for 4 hours, then stop heating and wait to cool to After room temperature, the precipitate was separated by centrifugation and dried, and ground to obtain a powdery product;

[0025] (3) Then calcined at 600°C for 6 hours in a nitrogen atmosphere to obtain a black powder catalyst (CN / Ni / CeO 2 ).

[0026] It is used to catalyze the hydrogenation of nitrobenzene to synthesize p-aminophenol, and the conversion rate of nitro...

Embodiment 12

[0037] (1) Cerium oxide (CeO 2 ) The carrier is crushed and sieved, and 20-40 mesh is selected, and an equal volume of nickel nitrate solution is impregnated to obtain a sample with a nickel loading of 6wt.%. Calcined at 450°C for 4 hours to obtain ceria-supported nickel oxide (NiO / CeO 2 );

[0038] (2) Take 1g NiO / CeO 2 , 0.5g of glucose and 2.0g of urea, ball milled to make them evenly mixed;

[0039] (3) Then calcined at 600°C for 6 hours in a nitrogen atmosphere to obtain a black powder catalyst (CN / Ni / CeO 2 ). It is used to catalyze the hydrogenation of nitrobenzene to synthesize p-aminophenol, and the conversion rate of nitrobenzene is 99%. The p-aminophenol selectivity is 100%.

Embodiment 13

[0041] The method is the same as in Example 12, except that the amount of glucose is 0.2 g, and the obtained catalyst catalyzes the hydrogenation of nitrobenzene to synthesize p-aminophenol, wherein the conversion rate of nitrobenzene is 100%, and the selectivity of p-aminophenol is 43%. .

[0042] Embodiment 13-16 investigated the impact of the catalyst obtained in the mass ratio of different glucose and nitrogen-containing compounds in step (2) to catalyze the hydrogenation of nitrobenzene to synthesize p-aminophenol, see Table 4, and all the other are the same as in Example 12, wherein the nitrogen-containing compounds Any one of urea, melamine, dicyandiamide, pyrrole, polypyrrole, urea-formaldehyde resin and polyvinylpyrrolidone:

[0043] Table 4

[0044]

[0045] Embodiment 17, 18 has investigated the impact of the catalyst catalyzed hydrogenation of nitrobenzene to synthesize p-aminophenol in different nitrogen atmospheres in the step (3) by the treatment temperature...

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Abstract

A preparing method and uses of a hydrogenation catalyst are provided. The method includes (1) loading cerium oxide that is adopted as a carrier with a metal nickel salt, and performing calcination in an air atmosphere to obtain nickel oxide loaded by the cerium oxide; (2) fully mixing the compound obtained in the step (1) with ethanediamine and carbon tetrachloride and refluxing and reacting the mixture in xylene to obtain a nitrogen-containing polymer clad catalyst precursor, or mixing the compound obtained in the step (1) with glucose and a nitrogen-containing compound to obtain a catalyst precursor; and (3) subjecting the catalyst precursor to high-temperature calcination at 500-1000 DEG C in an inert atmosphere to obtain the nitrogen-doped carbon-clad metal nickel hydrogenation catalyst. The catalyst is used for catalyzing hydrogenation of nitrobenzene to synthesize p-aminophenol, and the conversion ratio of the nitrobenzene and selectivity of the p-aminophenol can all reach 100%.

Description

technical field [0001] The invention relates to a preparation method of a catalyst and its use for catalyzing the hydrogenation of nitrobenzene to synthesize p-aminophenol. Background technique [0002] p-Aminophenol is an important organic intermediate widely used in medicine, dyestuff and rubber and other fields. At present, the industrial production process of p-aminophenol is mainly produced in one step by catalyzing the hydrogenation of nitrobenzene in a strong acidic solution. The catalyst used in this process condition is usually a supported noble metal platinum or palladium catalyst, nitro The conversion rate of benzene can reach 90%, and the selectivity of p-aminophenol is about 85%. However, in a strongly acidic reaction medium (usually 15wt.% sulfuric acid aqueous solution), the noble metal may be poisoned and the active components will also be lost, which will have a negative impact on the service life of the catalyst and the control of production costs . [0...

Claims

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Application Information

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IPC IPC(8): B01J27/24C07C213/02C07C215/76
CPCB01J27/24C07C213/02C07C215/76
Inventor 戴晨王涛
Owner 南通鼎新催化材料科技有限公司
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