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High-selectivity catalyst for preparing phthalide by hydrogenation of phthalic anhydride

A highly selective, catalyst technology, used in metal/metal oxide/metal hydroxide catalysts, physical/chemical process catalysts, organic chemistry, etc., can solve the limitation of active ingredient loading, poor stability, and difficult preparation It solves the problems of high dispersibility and high loading of catalysts, and achieves the effects of high selectivity, easy availability of raw materials, and good industrial application prospects.

Active Publication Date: 2013-12-11
成都大研科技产业发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation method of the catalyst adopts the impregnation method, which has poor stability, and the active component Ni nanoparticles are easy to agglomerate on the surface of the carrier.
In addition, the impregnation method is used to prepare supported nickel-based catalysts, and the loading amount of active components is limited to a certain extent, so it is difficult to prepare highly dispersed and high-loading catalysts.

Method used

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  • High-selectivity catalyst for preparing phthalide by hydrogenation of phthalic anhydride
  • High-selectivity catalyst for preparing phthalide by hydrogenation of phthalic anhydride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Example 1: Ni / Al 2 o 3 Catalyst preparation

[0020] Co-precipitation method was used to prepare 0.75mol / L Ni(NO 3 ) 2 ·6H 2 O and 0.25mol / L Al(NO 3 ) 3 9H 2 O solution A50mL, prepared to contain 0.80mol / L Na 2 CO 3 and 1.20mol / L NaOH alkali solution B50mL, at 65°C, add solution A evenly dropwise into solution B, maintain the pH of the reaction system at 9-10, stir vigorously, and co-precipitate. After the titration is completed, continue to stir and age, and finally filter, wash, and dry to obtain a nickel-containing hydrotalcite precursor. The obtained nickel-containing hydrotalcite precursor is calcined at 500°C and reduced at 400°C for 2 hours to obtain Ni / Al 2 o 3 catalyst. figure 1 Ni / Al is obtained by roasting the nickel-containing hydrotalcite material as the precursor 2 o 3 X-ray diffraction pattern of the catalyst.

Embodiment 2

[0021] Embodiment 2: the preparation of Co / ZnO catalyst

[0022] Co-precipitation method was used to prepare 0.75mol / L Co(NO 3 ) 2 ·6H 2 O and 0.25mol / L Zn(NO 3 ) 3 ·6H 2 O solution A50mL, prepared to contain 0.80mol / L Na 2 CO 3 and 1.20mol / L NaOH alkali solution B50mL, at 65°C, add solution A evenly dropwise into solution B, maintain the pH of the reaction system at 9-10, stir vigorously, and co-precipitate. After the titration is completed, continue to stir and age, and finally filter, wash, and dry to obtain a nickel-containing hydrotalcite precursor. The obtained nickel-containing hydrotalcite precursor is calcined at 500°C and reduced at 400°C for 2 hours to obtain a Co / ZnO catalyst.

Embodiment 3

[0023] Example 3: NiAu / Al 2 o 3 Catalyst preparation

[0024] Co-precipitation method was used to prepare 0.70mol / L Ni(NO 3 ) 2 ·6H 2 O, 0.05mol / L chloroauric acid and 0.25mol / L Al(NO 3 ) 3 9H 2 O solution A50mL, prepared to contain 0.80mol / L Na 2 CO 3and 1.20mol / L NaOH alkali solution B50mL, at 65°C, add solution A evenly dropwise into solution B, maintain the pH of the reaction system at 9-10, stir vigorously, and co-precipitate. After the titration is completed, continue to stir and age, and finally filter, wash, and dry to obtain a nickel-gold-containing hydrotalcite-like precursor. The obtained nickel-gold-containing hydrotalcite-like precursor was calcined at 500°C and reduced at 400°C for 2 hours to obtain NiAu / Al 2 o 3 catalyst.

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Abstract

The invention relates to a high-selectivity catalyst for preparing phthalide by hydrogenation of phthalic anhydride, which is a supported monometallic and bimetallic catalyst prepared by taking a hydrotalcite or hydrotalcite-like material as a precursor as well as preparation and application thereof. The composition of the catalyst is MM' / S, wherein the supported amount of metal M (Ni, Co, Fe, Cu, Mo and W) is 5-70%, the supported amount of metal M' (Au, La and Mg) is not higher than 30%, and S is an oxide of Al, Zn, Nb, Fe, Zr, Cr and Ti. The catalyst disclosed by the invention is applicable to kettle-type (intermittent or continuous) stirring reaction and is also applicable to continuous fixed-bed hydrogenation reaction, the selected solvent is gamma-butyrolactone, the activity for phthalic anhydride hydrogenation is high, the selectivity of phthalide is high, the phthalic anhydride conversion ratio can reach 99%, and the phthalide selectivity can reach 98%. The catalyst has high activity, high selectivity and high stability, raw materials are easily obtained, and the process is simple, so that the catalyst has a good industrial prospect.

Description

technical field [0001] The invention relates to a catalyst for preparing phthalide through hydrogenation of phthalic anhydride with high selectivity, in particular to a supported monometallic and bimetallic catalyst prepared by taking hydrotalcite or hydrotalcite-like material as a precursor, and its preparation and application. The catalyst described in the present invention can be applied to tank-type (intermittent or continuous) stirring reaction, and is also suitable for continuous fixed-bed hydrogenation reaction. The selected solvent is γ-butyrolactone, which has high activity for hydrogenation of phthalic anhydride and The target product phthalide has high selectivity and high stability, easy to obtain raw materials, simple process and good industrial application prospect. Background technique [0002] Phthalide (o-hydroxymethylbenzoic acid lactone) is an important fine chemical intermediate, mainly used in the production of dye intermediates 1,4-dichloroanthraquinone...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/755B01J23/80B01J23/89C07D307/88
Inventor 梁长海陈霄靳少华
Owner 成都大研科技产业发展有限公司
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