Ruthenium-carbon catalyst, and preparation method and application thereof

A ruthenium-carbon catalyst and catalyst technology, applied in chemical instruments and methods, physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, etc., can solve the problems of large catalyst consumption, high reaction pressure, and high temperature , to achieve the effect of novel preparation method, high conversion rate and high selectivity

Active Publication Date: 2020-01-31
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The object of the present invention is to provide a kind of monometallic supported ruthenium carbon catalyst and preparation method thereof, and it is applied in trimellitic anhydride hydrogenation to prepare 1,2,4-cyclohexane tricarboxylic anhydride reaction, solve existing trimellitic anhydride through catalytic hydrogenation In the process of hydrogen synthesis of 1,2,4-cyclohexanetricarboxylic anhydride, the reaction pressure is high, the temperature is high, the catalyst consumption is large, the cost is high and the yield is low. (100°C~150°C), with a single metal supported ruthenium carbon catalyst with high activity and high selectivity, reducing the cost of synthesizing 1,2,4-cyclohexanetricarboxylic anhydride and increasing its yield

Method used

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  • Ruthenium-carbon catalyst, and preparation method and application thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] (1) Preparation of catalyst

[0029] a. Activated carbon is pretreated to obtain carrier activated carbon

[0030] Get 5g gac, it is submerged in 30ml, 3mol / L nitric acid solution (the nitric acid solution preparation method is: the concentrated nitric acid that commercially available mass fraction is 68% and water are mixed together according to the volume ratio of 1:6.41, configure into a dilute nitric acid solution with a required concentration of 3mol / L, the following examples are the same as above), stirred and impregnated for 12 hours at 30°C, filtered, and the filter cake was washed with deionized water for 10 to 20 times until the pH of the filtrate was 7, and then in a tube furnace in N 2 Under the protection of the atmosphere, calcined at 600°C for 4 hours to obtain 4.5 g of carrier activated carbon;

[0031] b. Preparation of Ru nanoparticles

[0032] Take 5.0005×10 -4 mol RuCl 3 ·3H 2 O was dissolved in 150ml propylene carbonate ester, and ultrasonicat...

Embodiment 2

[0039] (1) Preparation of catalyst

[0040] a. Activated carbon is pretreated to obtain carrier activated carbon

[0041] Take 5g of activated carbon, immerse it in 30ml, 3mol / L nitric acid solution, stir and impregnate at 30°C for 12h, filter, wash the filter cake with deionized water for 10 to 20 times until the pH of the filtrate is 7, and then place it in a tube furnace N 2 Under the protection of the atmosphere, calcined at 600°C for 4 hours to obtain 4.5 g of carrier activated carbon;

[0042] b. Preparation of Ru nanoparticles

[0043] Take 5.0005×10 -4 mol RuCl 3 ·3H 2 O was dissolved in 150ml propylene carbonate ester, and ultrasonicated at a frequency of 25KHz for 60min to obtain a concentration of 3.3333×10 -3 mol / L ruthenium chloride solution, and then the above solution was transferred to a polytetrafluoroethylene-lined stainless steel autoclave, and reduced for 6 hours at 60°C under a hydrogen pressure of 4.0MPa to prepare 150ml of Ru nanoparticle solution....

Embodiment 3

[0049] (1) Preparation of catalyst

[0050] a. Activated carbon is pretreated to obtain carrier activated carbon

[0051] Take 5g of activated carbon, immerse it in 30ml, 3mol / L nitric acid solution, stir and impregnate at 30°C for 12h, filter, wash the filter cake with deionized water for 10 to 20 times until the pH of the filtrate is 7, and then place it in a tube furnace N 2 Under the protection of the atmosphere, calcined at 600°C for 4 hours to obtain 4.5 g of carrier activated carbon;

[0052] b. Preparation of Ru nanoparticles

[0053] Take 5.0005×10 -4 mol RuCl 3 ·3H 2 O was dissolved in 150ml propylene carbonate ester, and ultrasonicated at a frequency of 25KHz for 60min to obtain a concentration of 3.3333×10 -3 mol / L ruthenium chloride solution, and then the above solution was transferred to a polytetrafluoroethylene-lined stainless steel autoclave, and reduced for 6 hours at 80°C under a hydrogen pressure of 4.0MPa to prepare 150ml of Ru nanoparticle solution....

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Abstract

The invention discloses a ruthenium-carbon catalyst, and a preparation method and an application thereof in synthesis of 1,2,4-cyclohexanetricarboxylic anhydride; the ruthenium-carbon catalyst takes metal ruthenium as an active component and takes activated carbon as a carrier, and the mass loading capacity of ruthenium is 0.5-2.5%. The preparation method of the monometal-loaded ruthenium-carbon catalyst is novel; the catalyst is high in catalytic activity, recyclable and reusable, and good in stability; ruthenium particles are small in particle size and uniformly dispersed; a stabilizer is not needed in the preparation process, that is, the reaction can be completed under the condition of high-pressure hydrogen; the reaction process is environment-friendly and pollution-free. Trimelliticanhydride can be hydrogenated in a water phase at a low temperature of 100-150 DEG C and under a low pressure of 4.0 MPa H2, preparation of cyclohexanetricarboxylic anhydride is completed, the cost islow, the conversion rate is as high as 97.5%, the selectivity is as high as 97.6%, the process is simple, the used solvent is water, and the method conforms to the principle of green chemistry.

Description

[0001] (1) Technical field [0002] The invention belongs to the technical field of catalysts, and in particular relates to a single-metal supported ruthenium carbon catalyst and its preparation and application in catalyzing the hydrogenation of trimellitic anhydride to prepare 1,2,4-cyclohexanetricarboxylic anhydride. [0003] (2) Background technology [0004] Ruthenium carbon catalysts have high catalytic activity and are widely used as catalysts for hydrogenation reactions. Therefore, the development and research on ruthenium carbon catalyst has important theoretical significance and industrial application prospect. Common preparation methods of ruthenium catalysts mainly include: impregnation method, ion exchange method, co-precipitation method, etc. There are certain defects in the impregnation method, and the factors affecting the impregnation method include the impregnation method, the strength of adsorption, and the chemical changes that occur during heating and dryin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/46B01J35/02C07D307/89B82Y30/00B82Y40/00
CPCB01J23/462B01J35/023C07D307/89B82Y30/00B82Y40/00Y02P20/584
Inventor 严新焕张荷丰
Owner ZHEJIANG UNIV OF TECH
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