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Nanometer palladium catalyst for hydrogenation of anthraquinone and preparation method thereof

The technology of nano-palladium and catalyst is applied in the field of nano-palladium catalyst for hydrogenation of anthraquinone and the field of preparation, which can solve the problems of low hydrogenation efficiency, large amount of palladium and the like, and achieves environmental protection in preparation process, mild conditions, and stable performance for repeated reuse. Effect

Inactive Publication Date: 2010-08-18
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a kind of nano-palladium for anthraquinone hydrogenation using natural plants as reducing agent and carrier for the problems of low hydrogenation efficiency of supported palladium catalysts prepared by conventional chemical methods and large amount of palladium. Catalyst and preparation method

Method used

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  • Nanometer palladium catalyst for hydrogenation of anthraquinone and preparation method thereof
  • Nanometer palladium catalyst for hydrogenation of anthraquinone and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Take 3g of Gardenia (the dry weight of Gardenia and deionized water is 1:40) soak in 120ml of water at 100°C for 10min, take 0.1g of palladium chloride and make a 0.5mmol / L solution with the above extract of Gardenia, at 80°C After acting in a water bath for 36 hours and evaporating to dryness at 60° C. in vacuum, a gardenia in situ reduction-supported nanocatalyst was obtained, and the palladium loading relative to the gardenia extract was 1.2% by weight. Take 30mg of catalyst and put it into a fluidized bed reactor with 10ml of ethanol and 15ml of anthraquinone working solution, hydrogenate at 65°C for 1.75h, hydrogen flow rate is 30ml / min, oxidation is 45min, air flow rate is 30ml / min, hydrogenation efficiency is 9.3g / min L.

[0027] The XRD spectrum of the nano-palladium catalyst supported on the gardenia is shown in figure 1 , the diffraction peaks from left to right correspond to (111), (200), (220) and (311) palladium crystal planes, respectively. The electron ...

Embodiment 2

[0029] Take 2g of Gardenia (the dry weight of Gardenia and deionized water is 1:50) soak in 100ml of water at 90°C for 10min, take 0.1g of palladium chloride and use the above-mentioned Gardenia extract to make a 1 mmol / L solution, and put it in a water bath at 90°C After being neutralized for 24 hours and evaporated to dryness under vacuum at 60° C., a gardenia in situ reduction-supported nanocatalyst was obtained, and the palladium loading was 2.4% relative to the mass percentage of the gardenia extract. Take 30mg of catalyst and add it to a fluidized bed reactor with 10ml of ethanol and 10ml of anthraquinone working solution, hydrogenate at 50°C for 1.5h, hydrogen flow rate is 40ml / min, oxidation is 45min, air flow rate is 50ml / min, hydrogenation efficiency is 12.8g / L.

Embodiment 3

[0031] Take 5g of Gardenia (the dry weight of Gardenia and deionized water is 1:20) soak in 100ml of water at 100°C for 10min, take 0.1g of palladium chloride and make a 0.5mmol / L solution with the above extract of Gardenia, 60°C After acting in a water bath for 48 hours, and evaporating and drying in a vacuum at 60° C., a gardenia in situ reduction-supported nanocatalyst was obtained, and the palladium loading was 1.2% relative to the mass percentage of the gardenia extract. Take 25mg of catalyst and put it into a fluidized bed reactor with 10ml of ethanol and 10ml of anthraquinone working solution, hydrogenate at 65°C for 1h, hydrogen flow rate is 40ml / min, oxidation is 30min, air flow rate is 30ml / min, hydrogenation efficiency is 9.0g / min L.

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Abstract

The invention relates to a nanometer palladium catalyst for hydrogenation of anthraquinone and a preparation method thereof, relating to a palladium catalyst. The invention provides the nanometer palladium catalyst for the hydrogenation of anthraquinone and the preparation method thereof, wherein natural plants are taken as a reducing agent and a carrier. The nanometer palladium catalyst is prepared by dispersing nanometer palladium granules on a Cape jasmine carrier, and based on weight percent, the loaded palladium accounts for 1.2-3.6 percent of Cape jasmine, and the size of the nanometer palladium granules is 3-10 nm. Cape jasmine lixivium is prepared by dipping Cape jasmine in water, and the nanometer palladium catalyst is prepared by preparing palladium chloride into palladium chloride and Cape jasmine mixing solution by using the Cape jasmine lixivium, reducing and drying to obtain the nanometer palladium catalyst loaded on the Cape jasmine, i.e. the nanometer palladium catalyst for the hydrogenation of anthraquinone.

Description

technical field [0001] The invention relates to a palladium catalyst, in particular to a nano-palladium catalyst for anthraquinone hydrogenation which is reduced by natural plants and a preparation method. Background technique [0002] Hydrogen peroxide is a green chemical, widely used in papermaking, electronics, textile, medicine, environmental protection and other industries. There are many methods for producing hydrogen peroxide, among which the anthraquinone method accounts for more than 95% of the total capacity of industrial production of hydrogen peroxide. Anthraquinone hydrogenation is the most important process step of anthraquinone method. Supported palladium catalyst is currently the most effective catalyst for anthraquinone hydrogenation. Since palladium is a rare metal, the activity of the catalyst and the loading of palladium become the key factors affecting the production cost of hydrogen peroxide. In recent years, many new preparation methods of palladium...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/44B01J32/00B01J37/16C01B15/023
Inventor 李清彪张茜贾立山
Owner XIAMEN UNIV
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