Preparation of supported ruthenium-based hydrogenation catalyst and its application in catalytic hydrogenation of aldehyde-containing compounds

A technology of hydrogenation catalysts and aldehyde-based compounds, which is applied in the field of preparation of supported ruthenium-based hydrogenation catalysts, and can solve problems such as activity and selectivity to be improved, dispersion degree reduction, limited load capacity and stability, etc.

Active Publication Date: 2021-06-08
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, during the catalytic reaction process, due to the effects of high temperature, atmosphere, adsorption and other factors, the dispersion will be further reduced.
Although there are now single-atom catalyst materials, the theoretical dispersion can reach 100%, but it is limited by the loading capacity and stability issues, and is still being explored
[0007] In addition, the activity and selectivity of the existing supported ruthenium-based catalysts still need to be improved
Especially for the hydrogenation of aldehyde-containing compounds with high viscosity to generate corresponding hydroxyl compounds, ruthenium-based catalysts still have not made a breakthrough

Method used

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  • Preparation of supported ruthenium-based hydrogenation catalyst and its application in catalytic hydrogenation of aldehyde-containing compounds
  • Preparation of supported ruthenium-based hydrogenation catalyst and its application in catalytic hydrogenation of aldehyde-containing compounds
  • Preparation of supported ruthenium-based hydrogenation catalyst and its application in catalytic hydrogenation of aldehyde-containing compounds

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] Configure a ruthenium-based hydrogenation catalyst with a ruthenium loading of 5%. The specific process is as follows:

[0047] 1) Add ruthenium, potassium hydroxide and potassium nitrate into the crucible according to the molar ratio of 1:2.1:3.2, and bake at 650°C until melting for 1 hour. Then add appropriate amount of hot water when cooling to 80°C, and stir until all solids are dissolved.

[0048] 2) Pour the above prepared solution into the three-necked flask A, and drop into 15wt% sodium hypochlorite solution through the funnel, the amount of sodium hypochlorite is 1.5 times that of ruthenium. Then heat up to 80°C, stir, react for about 30 minutes, and then slowly add concentrated sulfuric acid solution with an amount 5 times that of ruthenium substance from the funnel, at this time, golden yellow ruthenium tetroxide gas will be generated.

[0049] 3) Weigh the activated carbon (France Arkema CECA (3sw, particle size: 250-300mesh, N 2 -BET:980m 2 g -1 , ash ...

Embodiment 12

[0068] Put 2000g of glucose and 5g of the ruthenium-based hydrogenation catalyst of Example 1 into the high-pressure hydrogenation reactor, seal the reactor, replace the air and fill it with hydrogen to start stirring, at a temperature of 100°C and a hydrogen pressure of 2.0MPa. Catalytic hydrogenation reaction. Before and during the reaction, the pH value of the hydrogenation solution is monitored online in real time to ensure that the pH value of the hydrogenation solution in the kettle is maintained at 7.0 to 7.5, and the real-time adjustment is carried out by linkage with the concentrated tea juice. After no hydrogen absorption, online sampling and analysis, the reactant content in the hydrogenation solution is 0 and the reaction is stopped. The reaction time is 60 minutes, the conversion rate is 100%, and the selectivity is 99.5%.

Embodiment 13

[0070] Put 2000g of glucose and 1g of the ruthenium-based hydrogenation catalyst of Example 6 into the high-pressure hydrogenation reactor, seal the reactor, replace the air, fill it with hydrogen and start stirring, at a temperature of 90°C and a hydrogen pressure of 5.0MPa. Catalytic hydrogenation reaction. Before and during the reaction, the pH value of the hydrogenation solution is monitored online in real time to ensure that the pH value of the hydrogenation solution in the kettle is maintained at 7.2 to 7.5, and the real-time adjustment is carried out by linkage with the concentrated barley leaf juice. After no hydrogen absorption, online sampling and analysis, the reactant content in the hydrogenation solution is 0 and the reaction is stopped. The reaction time is 65 minutes, the conversion rate is 100%, and the selectivity is 99.4%.

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Abstract

The invention provides the preparation of a supported ruthenium-based hydrogenation catalyst and its application in the catalytic hydrogenation reaction of aldehyde-containing compounds. The preparation method is carried out according to the following steps: 1) preparing ruthenium tetroxide gas; 2) pretreating the porous carrier so that the organic matter A is pre-stored in the internal pores of the porous carrier; 3) pouring the pretreated porous carrier into the reaction container , heat up to 80-100°C, vacuumize and degas for 2-5 hours, then turn off the vacuum, let the ruthenium tetroxide gas enter the reaction vessel and mix with the carrier under stirring, continue to stir at constant temperature for 2-5 hours, and then drop to -10--20 ℃, turn off the cooling, let it stand at room temperature, and take out the catalyst precursor; 4) reduce the catalyst precursor by temperature programming in methane / nitrogen to prepare a supported ruthenium-based hydrogenation catalyst. The invention provides the application of the catalyst in the catalytic hydrogenation reaction of aldehyde-containing compounds, which has the characteristics of less catalyst consumption, high conversion rate, good selectivity, fast hydrogenation rate and good stability.

Description

[0001] (1) Technical field [0002] The invention relates to the preparation and application of a hydrogenation catalyst, in particular to a preparation method of a supported ruthenium-based hydrogenation catalyst and its application in catalytic hydrogenation reactions of aldehyde-containing compounds. [0003] (2) Technical background [0004] Supported ruthenium-based catalysts are widely used, such as ammonia synthesis, benzene hydrogenation to cyclohexanone, glucose / xylose and other hydrogenation to sugar alcohols and other fields. Loading the noble metal ruthenium on the carrier can not only increase the specific surface area of ​​the metal particles to improve the catalyst activity and metal utilization rate, but also regulate the interaction between the ruthenium particles and the carrier, adjust the crystal phase and electronic structure of the ruthenium metal particles, and adapt to different Catalytic hydrogenation reaction requirements. [0005] The structural prop...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/46B01J37/16C07C31/26C07C31/18C07C29/132C07C65/03C07C51/367C07C33/22C07C29/141C07C33/20
CPCB01J23/462B01J35/008B01J37/16C07C29/132C07C29/141C07C51/367C07C31/26C07C31/18C07C65/03C07C33/22C07C33/20
Inventor 卢春山聂娟娟刘强强周烨彬张雪洁张群峰丰枫马磊赵佳许孝良郭玲玲吕井辉岑洁李小年
Owner ZHEJIANG UNIV OF TECH
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