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Phosphorus-doped porous graphene and its preparation method and method for catalyzing the oxidation of benzylamine

A technology of porous graphene and catalyst catalyzing benzylamine, applied in graphene, chemical instruments and methods, catalyst activation/preparation and other directions, can solve the problems of complicated preparation process and long period of porous graphene, and achieve stable physical and chemical properties, The effect of low cost and simple preparation process

Active Publication Date: 2019-02-22
CHINA UNIV OF PETROLEUM (BEIJING)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The preparation process of these porous graphene is relatively cumbersome and the cycle is long

Method used

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  • Phosphorus-doped porous graphene and its preparation method and method for catalyzing the oxidation of benzylamine
  • Phosphorus-doped porous graphene and its preparation method and method for catalyzing the oxidation of benzylamine
  • Phosphorus-doped porous graphene and its preparation method and method for catalyzing the oxidation of benzylamine

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Embodiment 1

[0053] This embodiment provides a kind of phosphorus-doped porous graphene, which is prepared through the following steps, such as figure 1 Shown:

[0054] (1) Reflux and boil the magnesium oxide powder in water and keep it for 8 hours, cool and filter, and dry at 80°C for 12 hours, then place it in a muffle furnace and raise the temperature to 500°C at a rate of 10°C / min in an air atmosphere. ℃ roasting for 2 hours to obtain porous flake hexagonal magnesium oxide with a specific surface area of ​​195m 2 / g, the two-dimensional film size is about 300nm;

[0055] (2) Add 0.5g of 4,5-bisdiphenylphosphine-9,9-dimethylxanthene into 30mL of ethanol, and ultrasonically disperse for 0.5 hours, and the ultrasonic power is 80kHz to obtain Source dispersion;

[0056] (3) The porous sheet-shaped hexagonal magnesia that 0.5g step (1) obtains is joined in the dispersion liquid that contains organic carbon, phosphorus source that step (2) obtains, with the rotating speed magnetic stirrin...

Embodiment 2

[0069] This embodiment provides a kind of phosphorus-doped porous graphene, which is prepared through the following steps, such as figure 1 Shown:

[0070] (1) Reflux and boil the magnesium oxide powder in water and keep it for 8 hours, cool, filter and dry at 90°C for 10 hours, then place it in a muffle furnace and raise the temperature to 800°C at a rate of 10°C / min in an air atmosphere. ℃ roasting for 2 hours to obtain porous flake hexagonal magnesium oxide with a specific surface area of ​​197m 2 / g, the two-dimensional film size is about 300nm;

[0071] (2) Add 1g of 2-dicyclohexylphosphine-2',4',6'-triisopropylbiphenyl into 30mL of ethanol, ultrasonically disperse for 0.5 hours, and the ultrasonic power is 80kHz to obtain organic carbon, Dispersion of phosphorus source;

[0072] (3) The porous sheet-shaped hexagonal magnesia that 0.5g step (1) obtains is joined in the dispersion liquid that contains organic carbon, phosphorus source that step (2) obtains, with the rot...

Embodiment 3

[0084] This embodiment provides a kind of phosphorus-doped porous graphene, which is prepared through the following steps, such as figure 1 Shown:

[0085] (1) Boil the magnesium oxide powder in water for reflux and keep it for 10 hours, cool and filter it, then dry it at 80°C for 10 hours, then place it in a muffle furnace and raise the temperature to 300°C at a rate of 10°C / min in an air atmosphere. ℃ roasting for 2 hours to obtain porous flake hexagonal magnesium oxide with a specific surface area of ​​190m 2 / g, the two-dimensional film size is about 200nm;

[0086] (2) Add 2g of triphenylphosphine into 30mL of ethanol, ultrasonically disperse for 0.5 hours, and the ultrasonic power is 80kHz, to obtain a dispersion containing organic carbon and phosphorus sources;

[0087] (3) The porous flaky hexagonal magnesia that 0.5g step (1) obtains is joined in the dispersion liquid that contains organic carbon, phosphorus source that step (2) obtains, with the rotating speed magn...

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Abstract

The invention provides a phosphorus-doped porous graphene, a preparation method thereof and a method for catalyzing the oxidation of benzylamine. The phosphorus-doped porous graphene is prepared by the following method: mixing the template agent with a dispersion containing organic carbon and phosphorus source, removing the solvent in the mixed solution, and placing the obtained mixture under the protection of inert gas at 200-700°C. Calculate for 2 to 5 hours, and then use pickling to remove the template agent to obtain phosphorus-doped porous graphene. The method for catalyzing the oxidation of benzylamine includes the following steps: using the phosphorus-doped porous graphene of the present invention or a mixture of template agent and phosphorus-doped porous graphene as a catalyst, reacting with benzylamine under the action of an oxidant to obtain N-benzylidene amine. The present invention uses a template agent to control the morphology, uses organic compounds containing carbon and phosphorus as both carbon and phosphorus sources, and directly synthesizes phosphorus-doped porous graphene by a roasting method. It is fast, convenient, can be synthesized in one step, and is easy to be synthesized on a large scale. Production and other advantages.

Description

technical field [0001] The invention relates to a phosphorus-doped porous graphene and a preparation method thereof, a mixture of a template agent and phosphorus-doped porous graphene, and a composite material using the phosphorus-doped porous graphene or the template agent and phosphorus-doped porous graphene The invention relates to a method for catalyzing the oxidation reaction of benzylamine as a catalyst, and belongs to the technical field of graphene materials. Background technique [0002] N-benzylamine is widely used in chemical industry and biochemistry, etc. The synthesis of N-benzylamine is generally based on the oxidation of benzylamine. However, the current oxidation process of benzylamine requires the use of metal-organic complexes that are difficult to separate and recycle as catalysts, and may also require higher reaction temperatures or use solvents that are toxic to the environment. Therefore, it is still a great challenge to develop an efficient and green...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/14B01J27/20C01B32/184C07C249/02C07C251/24
CPCC07C249/02B01J27/14B01J27/20B01J37/084C01P2002/72C01P2004/04C01P2004/03B01J35/618B01J35/647C07C251/24
Inventor 杨帆范晓旭李永峰
Owner CHINA UNIV OF PETROLEUM (BEIJING)