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Catalyst used for synthesis of aldehyde or ketone through oxidation of alcohol, and preparation method and application thereof

A catalyst and a technology for synthesizing aldehydes, which are applied in the field of fine chemical technology, can solve the problems of inability to obtain micron-sized silver-copper alloy particles, unsatisfactory catalytic effect and stability, and inability to obtain supported catalysts, and achieve superior catalytic performance. , good activity and stability, a wide range of effects

Active Publication Date: 2015-05-13
HUBEI HONGYUAN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Studies have shown that silver-copper composite catalysts have better low-temperature reactivity in the oxidation of alcohols, but commonly used metal nitrates such as copper nitrate are not oxidative, so silver-copper-embedded silicon nanowire arrays cannot be prepared using the methods mentioned above. supported catalyst
However, conventional two-component catalyst preparation methods such as mixed solution impregnation method, deposition precipitation method, and double impregnation method cannot produce uniform micron-sized silver-copper alloy particles, and the catalytic effect and stability are not ideal.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Take 10g of silicon particles with a particle size of 6-80 mesh, immerse in the mixed solution formed by mixing 1110ml of silver nitrate solution with a concentration of 0.01mol / L and 1250ml of copper nitrate solution with a concentration of 0.01mol / L, and add 2.4ml of a concentration of 40 % hydrogen fluoride solution, 30 o C reflux reaction for 60min under stirring, then raise the temperature to 90°C, close the reflux condensed water, volatilize the remaining hydrogen fluoride and absorb it with lye. Cool down to 10 o C, add 0.7ml of hydrazine hydrate aqueous solution with a weight concentration of 80%, react under stirring for 15min, then raise the temperature to 90°C and continue stirring for 20min, then cool and filter. The solid product obtained at 50 o C drying under nitrogen atmosphere, and then at 300 o Calcined under nitrogen atmosphere for 5h to obtain the product catalyst.

[0024] 3 grams of catalyst (6-20 mesh 0.5g, 20-40 mesh 0.5g, 40-60 mesh 1g, 60-8...

Embodiment 2

[0026] Take 10g of silicon particles with a particle size of 6-80 mesh, immerse in the mixed solution formed by mixing 570ml of silver nitrate solution with a concentration of 0.06mol / L and 50ml of copper nitrate solution with a concentration of 0.06mol / L, add 4.4ml of a concentration of 40 % hydrogen fluoride solution, 60 o C stirred and refluxed for 30 minutes, then raised the temperature to 80°C, closed the reflux condensed water, volatilized the remaining hydrogen fluoride and absorbed it with lye. Cool down to 20 o C, add 0.5ml of hydrazine hydrate aqueous solution with a weight concentration of 40%, react under stirring for 10min, then raise the temperature to 95°C and continue stirring for 15min, then cool and filter. The obtained solid product was at 100 o C drying under argon atmosphere, and then at 600 o Calcined under C argon atmosphere for 1 h to obtain the product catalyst.

[0027] Put 3 grams of catalyst (1g of 6-20 mesh, 1g of 20-40 mesh, 1g of 40-60 mesh i...

Embodiment 3

[0029] Take 10g of silicon particles with a particle size of 6-80 mesh, immerse in the mixed solution formed by mixing 680ml of silver nitrate solution with a concentration of 0.03mol / L and 520ml of copper nitrate solution with a concentration of 0.03mol / L, and add 3.5ml of a concentration of 40 % hydrogen fluoride solution, 50 o C stirred and refluxed for 40min, then raised the temperature to 95°C, closed the reflux condensed water, volatilized the remaining hydrogen fluoride and absorbed it with lye. Cool down to 20 o C, add 0.5ml of hydrazine hydrate aqueous solution with a weight concentration of 50%, react under stirring for 10min, then raise the temperature to 80°C and continue stirring for 30min, then cool and filter. The solid product obtained was at 80 o C drying under a helium atmosphere, and then at 500 o Calcined under C helium atmosphere for 2h to obtain the product catalyst.

[0030] 3 grams of catalyst (6-20 mesh 1g, 20-40 mesh 0.5g, 40-60 mesh 1g, 60-80 mes...

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PUM

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Abstract

The invention discloses a catalyst used for synthesis of aldehyde or ketone through oxidation of alcohol and a preparation method and application thereof, belonging to the technical field of fine chemical engineering. The active center of the catalyst is a micron-order silver copper alloy particle, and a carrier for the catalyst is a nanowire array of a silicon particle. The preparation method comprises the following steps: immersing the silicon particle in a mixed solution of silver nitrate and cupric nitrate in proportion; adding a hydrogen fluoride solution and carrying out an oxidation reduction reaction at a temperature of 30 to 60 DEG C; then heating to a temperature of 80 to 95 DEG C so as to remove residual hydrogen fluoride; cooling to a temperature of 10 to 20 DEG C, and adding a hydrazine hydrate solution for a reduction reaction; then heating to a temperature of 80 to 95 DEG C so as to remove residual hydrazine hydrate and carrying out cooling; and drying and roasting a solid product obtained after solid-liquid separation so as to obtain the catalyst. The catalyst provided in the embodiments in the invention has the advantages of high catalytic activity, uneasy sintering agglomeration, good stability, superior catalytic performance at a temperature in a range of 200 to 600 DEG C and a wide application scope.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, in particular to a catalyst for the oxidation of alcohols to synthesize aldehydes or ketones and its preparation method and application, in particular to a silver-copper catalyst for the oxidation of fatty alcohols and aromatic alcohols to synthesize corresponding aldehydes or ketones The invention relates to a preparation method and application thereof, in particular to a catalyst that can be used to synthesize corresponding aldehydes or ketones such as methanol, ethylene glycol, ethyl lactate and phenethyl alcohol, and a preparation method thereof. Background technique [0002] The selective oxidation of fatty alcohols or aromatic alcohols to corresponding aldehydes or ketones is an important basic reaction in fine chemicals, and the obtained aldehydes or ketones are important organic intermediates for the preparation of spices, drugs and food additives. For example, formaldehyde, the pr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/89C07C45/39C07C45/38C07C47/055C07C49/185C07C47/228C07C67/313C07C69/716
Inventor 邓支华尹国平程思远林建刚汪林涛
Owner HUBEI HONGYUAN PHARMA
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