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Phosphorus-doped porous graphene, preparation method thereof and method for catalyzing oxidation of benzylamine

A technology of porous graphene and magnesium oxide, applied in chemical instruments and methods, preparation of imino compounds, catalyst activation/preparation, etc., can solve the problems of cumbersome preparation process and long period of porous graphene, and achieve easy mass production, Low cost and effect of increasing reactivity

Active Publication Date: 2016-12-21
CHINA UNIV OF PETROLEUM (BEIJING)
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  • 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, preparation method thereof and method for catalyzing oxidation of benzylamine
  • Phosphorus-doped porous graphene, preparation method thereof and method for catalyzing oxidation of benzylamine
  • Phosphorus-doped porous graphene, preparation method thereof and method for catalyzing 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 phosphorus-doped porous graphene, a preparation method thereof and a method for catalyzing oxidation of benzylamine. The phosphorus-doped porous grapheme is prepared from the steps that templating agent and a dispersion containing organic carbon and a phosphorus source are mixed, solvent in the mixed solution is removed to obtain a mixture, the obtained mixture is calcined for 2-5 hours at the temperature of 200-700DEG C under an inert atmosphere protection, then the templating agent is removed by means of acid washing to obtain the phosphorus-doped porous graphene. The method for catalyzing oxidation of benzylamine comprises the following steps that the phosphorus-doped porous graphene or the mixture of the templating agent and the phosphorus-doped porous graphene are used as a catalyst and are reacted with benzylamine under the action of oxidizing agent to obtain N-benzylidenebutyramide. According to the phosphorus-doped porous graphene, the preparation method thereof and the method for catalyzing oxidation of benzylamine, the templating agent is used for controlling the morphology, meanwhile, the organic compounds containing carbon and phosphorus are used as a carbon source and a phosphorus source, and the phosphorus-doped porous graphene is synthesized directly by means of calcination, therefore, the preparation method has the advantages of being quick, convenient and fast, and being capable of being synthesized in one step, prone to large-scale production and so on.

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 Applications(China)
IPC IPC(8): B01J27/14B01J27/20C01B31/04C07C249/02C07C251/24
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)
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