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A palladium/graphene catalyst for dehydrogenation of dodecahydroethylcarbazole and preparation method thereof

A technology of dodecahydroethylcarbazole and catalyst, applied in the field of palladium/graphene catalyst and its preparation, to achieve the effects of increased selectivity, low cost and uniform distribution

Active Publication Date: 2019-06-14
安徽秉品新能源科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] At present, the bottleneck of this technology is how to develop high-conversion, high-selectivity and high-efficiency dehydrogenation catalysts to improve the energy conversion efficiency of vehicle-mounted hydrogen fuel cell systems.

Method used

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  • A palladium/graphene catalyst for dehydrogenation of dodecahydroethylcarbazole and preparation method thereof
  • A palladium/graphene catalyst for dehydrogenation of dodecahydroethylcarbazole and preparation method thereof
  • A palladium/graphene catalyst for dehydrogenation of dodecahydroethylcarbazole and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0037] Graphite oxide was prepared by the Hummer method, the product was suction filtered, then washed with distilled water to pH = 6, and dried in a vacuum oven at 60°C for 24 hours; the dried product was added to a ball mill tank containing n-heptane solution, and the ball mill was used for auxiliary pre-stripping for 4 hours , the speed of the ball mill is 500 rpm; weigh 0.5g of graphite oxide powder obtained by ball milling and place it in a conical flask, add 50ml of distilled water and stir for 2h to mix evenly, place the conical flask in a 150w ultrasonic cleaner for 1h, and then use Ultrasonic pulverization with a 600w cell pulverizer for 1 hour to obtain a graphene oxide dispersion.

[0038] Add palladium chloride to the obtained graphene oxide dispersion, add according to the palladium mass fraction of 5wt%, and stir the solution for 12 hours, then add the above solution into a 500ml three-necked flask, add 200ml of ethylene glycol, and react at 120°C for 12h , The w...

Embodiment 2

[0046] Graphite oxide was prepared by the Brodie method, the product was suction-filtered, then washed with distilled water to pH = 5, and dried in a vacuum oven at 60°C for 24 hours; the dried product was added to a ball mill tank containing n-hexane solution, and the ball mill was used for auxiliary pre-stripping for 4 hours. The speed of the ball mill is 800 rpm; weigh 0.5g of the graphite oxide powder obtained by ball milling and place it in a conical flask, add 50ml of distilled water and stir for 2h to mix well, put the conical flask in a 200w ultrasonic cleaning machine for 1h, and then use an 800w The cell pulverizer was ultrasonically pulverized for 1 hour to obtain a graphene oxide dispersion.

[0047] Add palladium chloride to the obtained graphene oxide dispersion, add according to the palladium mass fraction of 3wt%, and stir the solution for 12 hours, then add the above solution into a 500ml three-necked flask, add 250ml of ethylene glycol, and react at 110°C for ...

Embodiment 3

[0049] Graphite oxide was prepared by the Standenmaier method, the product was suction filtered, then washed with distilled water to pH = 3, and dried in a vacuum oven at 60°C for 24 hours; the dried product was added to a ball mill tank containing n-heptane solution, and the ball mill was used for auxiliary pre-stripping for 4 hours , the speed of the ball mill is 1000 rpm; 0.5g of graphite oxide powder obtained by ball milling is weighed and placed in a conical flask, and 50ml of distilled water is added to stir for 2h to mix evenly. Ultrasonic pulverization with a 450w cell pulverizer for 1 hour to obtain a graphene oxide dispersion.

[0050] Add palladium chloride to the obtained graphene oxide dispersion, add according to the palladium mass fraction of 7wt%, stir the solution for 12 hours, add the above solution into a 500ml three-necked flask, add 200ml of ethylene glycol, and react at 110°C for 10h , The whole reaction was protected by argon gas. After the reaction, th...

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Abstract

The invention discloses a preparation method of a palladium / graphene catalyst for dehydrogenation of dodecahydroethyl carbazole which is a product obtained by completely hydrogenating ethyl carbazole. The catalyst comprises, by mass, 70-88% of carbon, 10-25% of oxygen and 1-10% of palladium, and 1-3 carrier graphene sheet layers are formed in the catalyst. The preparation method includes two steps: preparing a graphene oxide dispersion; preparing the palladium / graphene catalyst. Through methods of ball milling aided pre-striping and two-stage ultrasonic striping, the problem that graphene sheet layers prepared by conventional redox methods is solved; the palladium / graphene catalyst prepared by adopting a water-ethylene glycol reducing system is small in grain size and uniform in grain size distribution, so that the defect that active metal is large in grain size and nonuniform in grain size distribution when no dispersant and surfactant are added in conventional preparation methods is overcome. The catalyst is excellent in catalytic performance, so that reaction time is shortened greatly, selectivity of ethyl carbazole which is a final dehydrogenation product is greatly improved to higher than 97%, and total dehydrogenation is higher than 5.74wt%.

Description

technical field [0001] The invention belongs to the technical field of dehydrogenation of dodecahydroethylcarbazole, and in particular relates to a palladium / graphene catalyst for dehydrogenation of dodecahydroethylcarbazole and a preparation method thereof. Background technique [0002] Hydrogen energy, as an ideal clean fuel that may replace fossil fuels, especially in fuel cell vehicles, has been receiving extensive attention and research. A series of research results show that its use in mobile vehicles can significantly reduce emissions of carbon oxides, nitrogen oxides, and sulfur oxides. However, the commercial development of hydrogen energy as a renewable energy is not ideal, mainly due to the technical difficulties in hydrogen storage. At present, the fuel cell hydrogen storage methods that have been commercialized mainly include high-pressure gaseous hydrogen storage and low-temperature liquefied hydrogen storage. These two hydrogen storage methods have obvious di...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/44C07D209/86C01B3/00
CPCB01J23/44C01B3/0015C07D209/86Y02E60/32
Inventor 方涛王斌
Owner 安徽秉品新能源科技有限公司
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