Preparation of supported ruthenium-based hydrogenation catalyst and its application in catalytic hydrogenation of dimethyl terephthalate

A hydrogenation catalyst and supported technology, which is applied in the field of hydrogenation catalyst and its preparation and application, can solve the problems of no breakthrough, activity and selectivity to be improved, and achieve the effect of easy operation, low cost and high selectivity

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

[0005] In conclusion, the activity and selectivity of existing ruthenium-based hydrogenation catalysts still need to be improved
Especially for the hydrogenation of dimethyl terephthalate to methyl 1,4-cyclohexyldicarboxylate, 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 dimethyl terephthalate
  • Preparation of supported ruthenium-based hydrogenation catalyst and its application in catalytic hydrogenation of dimethyl terephthalate
  • Preparation of supported ruthenium-based hydrogenation catalyst and its application in catalytic hydrogenation of dimethyl terephthalate

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 terephthalate, 200 ml of THF and 5G Example 1 was put into high pressure hydrogenation reactor, and the reaction kettle was sealed, and the air was charged and stirred and stirred, at a temperature of 100 ° C, The hydrogen pressure is carried out under conditions of 4.0 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 reactant is stopped in the hydrogenation content of 0 after the hydrogenation solution, resulting in 1,4-cyclohexyl methylene methyl methyl. The reaction time is 3 h, the conversion rate is 100%, and the selectivity is 99.4%.

Embodiment 13

[0068] 100 g of terephthalate, 100 ml of THF and 1G Example 6 was put into high pressure hydrogenation reactor, and the reactor was sealed, and the air was charged into hydrogen and stirred at the temperature of 120 ° C, Catalytic hydrogenation is carried out under conditions of 6.0 MPa of hydrogen pressure. 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 reactant is stopped in the hydrogenation content of 0 after the hydrogenation solution, resulting in 1,4-cyclohexyl methylene methyl methyl. The reaction time is 4 h, 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 of dimethyl terephthalate. 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 stirring at constant temperature for 2-5 hours, and then lower it to 0-5°C, Turn off the cooling, let it stand at room temperature, and take out the catalyst precursor; 4) program the temperature reduction of the catalyst precursor 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 dimethyl terephthalate, 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 of preparing a load-type ruthenium-based hydrogenation catalyst and a use of terephthalate catalytic hydrogenation reaction. [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 typ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/46B01J35/02C07C67/303C07C69/75
Inventor 卢春山刘强强聂娟娟张雪洁周烨彬赵佳丰枫马磊张群峰郭玲玲许孝良吕井辉岑洁李小年
Owner ZHEJIANG UNIV OF TECH
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