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Highly active ruthenium-carbon catalyst modified by transition metal atoms and preparation method thereof

A technology of ruthenium-carbon catalyst and transition metal, which is applied in the field of high-activity ruthenium-carbon catalyst and its preparation, can solve problems such as failure to meet reaction requirements, high cost, and insufficient activity, and achieve excellent catalytic effect, increased yield, and improved catalytic performance. active effect

Inactive Publication Date: 2017-04-26
PANJIN GELIN KAIMO TECH CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the activity of ruthenium-on-carbon catalysts can be improved to a certain extent by adjusting the process parameters such as the type of ruthenium precursor, the support structure and the reduction method, it is still difficult to meet the market demand for the catalytic activity of the product.
Many hydrogenation reactions cannot be realized with existing ruthenium-carbon catalysts. The main reason is that the existing ruthenium-carbon catalysts are not active enough to meet the reaction requirements.
For example, the current production of key intermediates of gliclazide still uses the borohydride reduction method, which is not only polluting but also costly
If the hydrogenation method can be realized by hydrogen reduction, it will not only have high atom economy, but also the cost will be greatly reduced
However, due to the insufficient activity of the existing ruthenium-on-carbon catalysts, it is difficult to realize its hydrogenation reaction

Method used

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  • Highly active ruthenium-carbon catalyst modified by transition metal atoms and preparation method thereof
  • Highly active ruthenium-carbon catalyst modified by transition metal atoms and preparation method thereof
  • Highly active ruthenium-carbon catalyst modified by transition metal atoms and preparation method thereof

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preparation example Construction

[0032] The preparation method of modified ruthenium carbon catalyst of the present invention comprises the steps:

[0033] (1) active carbon carrier and ruthenium solution are mixed and adsorbed;

[0034] (2) Add a certain amount of transition metal salt solution, and continue to stir and adsorb for 1 to 3 hours;

[0035] (3) adding a reducing agent solution for reduction for 1 to 3 hours;

[0036] (4) After the reaction is finished, filter with suction, wash with deionized water until nearly neutral, and dry to obtain a ruthenium-carbon catalyst modified by a transition metal atom.

[0037] Wherein, in step (1), the ruthenium solution is a soluble ruthenium solution, such as ruthenium chloride, ruthenium sulfate, ruthenium nitrite trinitrate or ruthenium acetate solution. A corresponding amount of ruthenium solution is prepared according to the mass percentage of ruthenium atoms in the catalyst being 3wt%-10wt%.

[0038] In step (2), the transition metal salt solution is p...

Embodiment 1

[0044] Preparation of molybdenum atom modified ruthenium carbon catalyst

[0045] Weigh 47.26g of activated carbon powder and disperse it in 200mL of deionized water; weigh 6.723g of ruthenium chloride trihydrate and dissolve it in 100mL of deionized water; under stirring conditions, mix the two and absorb for 1 hour; weigh 1.911g of molybdic acid Ammonium solid ((NH 4 ) 6 Mo 7 o 24 4H 2(0), be dissolved in 50mL deionized water, gradually add in the above-mentioned gac solution under stirring condition; After stirring and absorbing for 1 hour, add sodium borohydride aqueous solution (1.2g sodium borohydride is dissolved in 100mL deionized water) gradually, react 1 at room temperature Hours later, filter with suction, wash 5 times with deionized water to near neutrality, and dry in an oven at 80° C. for 12 hours to obtain a molybdenum atom-modified ruthenium carbon catalyst, wherein the mass percentage of ruthenium is 5 wt%, and the mass percentage of molybdenum The conten...

Embodiment 2

[0048] Preparation of Tungsten Atom Modified Ruthenium Carbon Catalyst

[0049] Weigh 47.26g of activated carbon powder and disperse it in 200mL of deionized water; weigh 6.723g of ruthenium chloride trihydrate and dissolve it in 100mL of deionized water; mix the two under stirring conditions and absorb for 1 hour; weigh 1g of tungsten chloride Solid (WCl 6 ), dissolved in 50mL deionized water, and gradually added to the above activated carbon solution under stirring; after stirring and absorbing for 1 hour, gradually added sodium formate aqueous solution (2g sodium formate dissolved in 100mL deionized water), reacted at 80°C for 1 hour, and suction filtered , washed 5 times with deionized water to near neutrality, and dried in an oven at 80°C for 12 hours to obtain a ruthenium-carbon catalyst modified by tungsten atoms, wherein the mass percentage of ruthenium is 5 wt%, and the mass percentage of tungsten is 0.9 wt%. (Based on the total mass of the catalyst).

[0050] fig...

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Abstract

The invention relates to a ruthenium-carbon catalyst. The ruthenium-carbon catalyst comprises an activated carbon carrier on which ruthenium nanoparticles and transition metal nanoparticles are loaded. According to the invention, transition metal atoms of molybdenum, tungsten, vanadium, rhenium or cobalt and the like are added, so that a modified ruthenium-carbon catalyst is prepared, and then the catalytic activity of the modified ruthenium-carbon catalyst is greatly improved and an activity restrictive bottleneck of the traditional ruthenium-carbon catalyst is broken. The modified ruthenium-carbon catalyst prepared by the invention takes difficult activation reactions of amino acid reduction, imide reduction and the like as evaluation reactions, and shows higher catalytic activity compared with a commercial ruthenium-carbon catalyst under same reaction conditions, and the yield of the modified ruthenium-carbon catalyst is improved by about 50% to 2 times to realize a green and high-efficient catalytic reaction process.

Description

technical field [0001] The invention relates to a highly active ruthenium-carbon catalyst modified by transition metal atoms and a preparation method thereof, belonging to the technical field of organic synthesis. Background technique [0002] Ruthenium carbon catalysts are an important class of chemical reaction catalysts, which are widely used in hydrogenation reactions in fine chemical, pharmaceutical and other industries. They are specifically used to catalyze many reactions such as hydrogenation of glucose to sorbitol, hydrogenation of amino acids to amino alcohols, etc. . [0003] In recent years, with the strict requirements of the environmental protection law, the traditional reduction route with large pollution and high cost will gradually be eliminated; on the other hand, the market demand for ruthenium carbon catalyst product quality continues to increase, requiring higher purity ruthenium carbon catalyst products. Based on these two requirements, the developmen...

Claims

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Application Information

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IPC IPC(8): B01J23/648B01J23/652B01J23/656B01J23/89C07C213/00C07C215/08C07D209/52
CPCB01J23/6482B01J23/6525B01J23/6527B01J23/6567B01J23/8913C07C213/00C07D209/52C07C215/08
Inventor 宫宁瑞
Owner PANJIN GELIN KAIMO TECH CO LTD
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