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A kind of PD/C catalyst and preparation method for TMBQ hydrogenation production TMHQ

A catalyst and activated carbon technology, which is applied in the field of Pd/C catalyst and its preparation, can solve the problems of low catalytic activity, low dispersion of precious metal Pd, and high dispersion, and achieve high catalytic activity, increased reduction potential, and high dispersion.

Inactive Publication Date: 2011-12-28
ZHEJIANG NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The present invention aims at the low dispersion of precious metal Pd existing in the existing Pd / C catalyst, and the deficiency that the catalytic activity is not high in the process of catalyzing TMBQ hydrogenation to synthesize TMHQ, and provides a kind of precious metal Pd with high dispersion, which is catalytic in TMBQ In the process of hydrogenation to produce TMHQ, it not only has high selectivity, but also has high catalytic activity in TMBQ catalytic hydrogenation reaction for TMBQ (2,3,5-trimethylbenzoquinone) hydrogenation to produce TMHQ (2,3, 5-trimethylhydroquinone) Pd / C catalyst and preparation method

Method used

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  • A kind of PD/C catalyst and preparation method for TMBQ hydrogenation production TMHQ
  • A kind of PD/C catalyst and preparation method for TMBQ hydrogenation production TMHQ
  • A kind of PD/C catalyst and preparation method for TMBQ hydrogenation production TMHQ

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Effect test

Embodiment 1

[0039] 20g powder, specific surface area greater than 1000m 2 The coconut shell-type activated carbon with a concentration of 5wt.% was refluxed in a water bath at 60°C for 2h with a concentration of 5wt.%, then repeatedly washed with deionized water to neutrality, and then air-dried at 80°C for 4h for later use.

[0040] Preparation of Pd source impregnation solution, weigh about 3g of PdCl 2 The solid was added to 7.29ml of concentrated hydrochloric acid, and after being completely dissolved, it was diluted with deionized water to a 50ml volumetric flask for later use.

[0041] Take 3 g of pretreated activated carbon and add 10 ml of sodium carbonate with a concentration of 0.9 mol / L to pre-soak the activated carbon for 0.5 h. According to the loading of Pd is 5.0wt.%, pipette PdCl 2 About 14ml of the solution was added to pre-soaked activated carbon and soaked for 6h, and then placed in an oven at 50°C overnight, in 10vol.%H 2 / Ar (total flow rate: 30ml / min) atmosphere a...

Embodiment 2

[0045] 20g powder, specific surface area greater than 1000m 2 The activated carbon per g was refluxed with 5wt.% nitric acid in a water bath at 60°C for 2h, then repeatedly washed with deionized water until neutral, and then air-dried at 80°C for 4h for later use.

[0046] Preparation of Pd source impregnation solution, weigh about 3g of PdCl 2 The solid was added to 7.29ml of concentrated hydrochloric acid, and after being completely dissolved, it was diluted with deionized water to a 50ml volumetric flask for later use.

[0047] Take 3 g of pretreated activated carbon and add 10 ml of oxalic acid with a concentration of 0.1 mol / L to pre-soak the activated carbon for 0.5 h. According to the loading of Pd is 5.0wt%, pipette PdCl 2 About 14ml of the solution was added to pre-soaked activated carbon and soaked for 6h, and then placed in an oven at 50°C overnight, in 10vol.%H 2 / Ar (total flow rate: 30ml / min) atmosphere at 200°C for 2h to obtain the catalyst, and the dispersio...

Embodiment 3

[0051] 20g powder, specific surface area greater than 1000m 2 The coconut shell-type activated carbon with a concentration of 10wt.% was refluxed in a water bath at 60°C for 2h with a concentration of 10wt.%, then repeatedly washed with deionized water to neutrality, and then air-dried at 80°C for 4h for later use.

[0052] Preparation of Pd source impregnation solution, weigh about 3g of PdCl 2 The solid was added to 7.29ml of concentrated hydrochloric acid, and after being completely dissolved, it was diluted with deionized water to a 50ml volumetric flask for later use.

[0053] Take 3 g of pretreated activated carbon and add 10 ml of oxalic acid with a concentration of 0.1 mol / L to pre-soak the activated carbon for 0.5 h. According to the loading of Pd is 5.0wt%, pipette PdCl 2 About 14ml of the solution was added to pre-soaked activated carbon and soaked for 6h, and then placed in an oven at 50°C overnight, in 10vol.%H 2 / Ar (total flow rate: 30ml / min) atmosphere at 20...

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Abstract

The invention relates to a Pd / C catalyst for producing 2,3,5-trimethylhydroquinone (TMHQ) by virtue of hydrogenation of 2,3,5-trimethylbenzoquinone (TMBQ) and a preparation method thereof. In the Pd / C catalyst provided by the invention, a noble metal Pd supported on a carrier activated carbon exists in a nano particle form, the dispersion degree of Pd is not less than 30%, and the carrier activated carbon has micropores and mesopores. The preparation method comprises the following steps: (1) carrying out acid treatment on the carrier activated carbon, and adding an acid solution in activated carbon for carrying out water bath reflux treatment; (2) washing activated carbon treated by the acid with deionized water to be neutral, and drying so as to obtain the activated carbon carrier; (3) infiltrating the activated carbon carrier with an infiltration liquid in advance; (4) slowly dropwise adding a 0.01-0.3mol / L Pd source solution in the activated carbon carrier which is infiltrated in advance, so that Pd is supported on the activated carbon, thus a catalyst precursor is obtained; and (5) drying the catalyst precursor and then treating the dried catalyst precursor by a reduction method so as to obtain the Pd / C catalyst for producing TMHQ by virtue of hydrogenation of TMBQ. The Pd / C catalyst provided by the invention has the characteristics of being simple and efficient, and having high catalysis property in BTOP (benzene to phenol) reaction.

Description

technical field [0001] The invention relates to a supported noble metal catalyst for liquid-phase catalytic hydrogenation and a preparation method thereof, in particular to a method for hydrogenation of TMBQ (2,3,5-trimethylbenzoquinone) to produce TMHQ (2 , 3,5-trimethylhydroquinone) Pd / C catalyst and preparation method. Background technique [0002] Vitamin E (VE) is not only used as an additive in medicine, health products, food, and cosmetics, but also as an industrial antioxidant. It has become a hot product that has attracted much attention in recent years. The demand for VE in the domestic and foreign markets has increased sharply, and the price has continued to rise. Therefore, timely production and expansion of VE production will bring better economic benefits. [0003] TMHQ (2,3,5-trimethylhydroquinone) is a white powdery organic substance, an important intermediate for the synthesis of vitamin E, which reacts with isophytol to synthesize VE. However, the product...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/44B01J35/10C07C50/02C07C46/00
Inventor 朱伟东张富民吴利钟依均
Owner ZHEJIANG NORMAL UNIVERSITY
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