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Preparation of Supported Ruthenium-Based Hydrogenation Catalyst and Its Application in Catalytic Hydrogenation of Butenedioic Anhydride

A hydrogenation catalyst and a supported technology are applied in the field of preparation of a supported ruthenium-based hydrogenation catalyst, which can solve the problems that the ruthenium-based catalyst has not made a great breakthrough, and the activity and selectivity need to be improved, and achieve high stability and cost. Low, reduced effect on mass transfer

Active Publication Date: 2021-06-04
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In conclusion, the activity and selectivity of existing ruthenium-based hydrogenation catalysts still need to be improved
Especially for the catalytic hydrogenation of butenedioic anhydride, ruthenium-based catalysts still have not made a major breakthrough

Method used

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  • Preparation of Supported Ruthenium-Based Hydrogenation Catalyst and Its Application in Catalytic Hydrogenation of Butenedioic Anhydride
  • Preparation of Supported Ruthenium-Based Hydrogenation Catalyst and Its Application in Catalytic Hydrogenation of Butenedioic Anhydride
  • Preparation of Supported Ruthenium-Based Hydrogenation Catalyst and Its Application in Catalytic Hydrogenation of Butenedioic Anhydride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] A ruthenium-based hydrogenation catalyst having a ruthenium load is configured. The specific process is as follows:

[0045] 1) The ratio of ruthenium, potassium hydroxide and potassium hydroxide and potassium hydroxide were added to the crucible in the ratio of 1: 2.1: 3.2, and fired at 650 ° C to melt 1 h. Then it was added to 80 ° C to add an appropriate amount of hot water, stir until all solids dissolved.

[0046] 2) Pour the solution prepared in the three flask A and dropped into 15 wt% sodium hypochlorite solution by the funnel, and the amount of sodium hypochlorite is 1.5 times the amount of ruthenium. Then the temperature is warmed to 80 ° C, stirred, and the reaction is slowly added from the funnel from the funnel from the funnel for about 30 minutes. At this time, there will be a golden quadruple hydrazine gas.

[0047] 3) Weigh activated carbon corresponding to 5% load (France Arkema Ceca (3SW, Particle Size: 250-300MESH, N) 2 -BET: 980M 2 G -1 ASH Content: <3%)...

Embodiment 12

[0066] 100 g of butene hydrogenlide, 200 ml DMF and 5G Example 1 was put into high pressure hydrogenation reactor, and the reaction kettle was sealed. After replacing the air, the hydrogen was charged and stirred, at a temperature of 120 ° C, hydrogen pressure Catalytic hydrogenation reaction was carried out under the conditions of 1.0 MPa. Pre-reactions and in progress, in real time, the hydrogen-hydrogen-mixed pH is monitored online, ensuring that the hydrogen solution in the kettle is maintained at 7.5 to 8.0, and real-time regulation is carried out by the concentrated juice of the tea. After the hydrogen is not suction, the in-line sampling analysis, the reactant in the hydrogenation liquid is stopped and the reaction is stopped to obtain butoth dihydrane. The reaction time was 30 minutes, the conversion rate was 100%, and the selectivity was 99.1%.

Embodiment 13

[0068] 100 g of butene hydrogen-hydrogenation catalysts of 100 g of butene chloric anhydride, 100 mL DMF and 1G Example 6 were put into high pressure hydrogenation reactor, and the reactor was sealed. After the air was replaced, the hydrogen was charged, and the temperature was 90 ° C, the hydrogen pressure was Catalytic hydrogenation reaction was carried out under 2.0 MPa conditions. Pre-reactions and in progress, real-time online pH, ensure that the hydrogen solution in the kettle is maintained at 7.5 to 8.0, and real-time regulation is carried out by linkage of Ruoya lobes. After the hydrogen is not suction, the in-line sampling analysis, the reactant in the hydrogenation liquid is stopped and the reaction is stopped to obtain butoth dihydrane. The reaction time was 35 minutes, the conversion rate was 100%, and the selectivity was 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 butenedioic anhydride. 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 close 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 lower to ≤0°C and high At -10°C, turn off the cooling, let it stand at room temperature, and take out the catalyst precursor; 4) The catalyst precursor is reduced by temperature programming in ethylene / nitrogen to prepare a supported ruthenium-based hydrogenation catalyst. The invention provides the application of the catalyst in the catalytic hydrogenation reaction of butenedioic anhydride, 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 present invention relates to a hydrogenation catalyst and a preparation and application thereof, in particular to a method for preparing a load type ruthenium hydrogenation catalyst and a use of catalytic hydrogenation in butene diacid anhydride. [0003] (2) Technology background [0004] The load ruthenium-based catalyst is widely used, such as ammonia synthesis, benzene hydrocarhexanone, glucose / xylose, and the like. The noble metal ruthenium is loaded on the carrier, not only can increase the metal particles than the surface area to improve the catalyst activity and metal utilization, but also regulate the interaction of ruthenium particles and the carrier, and modulate the crystal phase and electronic structure of ruthenium metal particles, and adapt to different Catalytic Hydrogenation Reaction. The structural properties of the catalyst material are often associated with the catalyst preparation process. Preparation method of load type...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/46B01J37/16B01J31/02C07D307/60
CPCB01J23/462B01J31/0202B01J31/0204B01J31/0207B01J37/16C07D307/60
Inventor 卢春山张雪洁聂娟娟刘强强周烨彬马磊丰枫张群峰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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