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Metal single atom loaded carbon-nitrogen polymer catalyst and preparation method thereof

A technology for polymers and catalysts, which is applied in the field of metal single-atom-supported carbon-nitrogen polymer catalysts and its preparation. The effect of large amount and stable structure

Active Publication Date: 2021-02-12
INST OF EARTH ENVIRONMENT CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] However, as the size decreases, the surface energy of metal particles will increase sharply, and they will spontaneously aggregate into larger metal particles
Although various "top-down" or "bottom-up" metal single atom loading methods have been reported in many literatures, none of the methods can accurately load single atoms around the active site.
Therefore, it is extremely difficult to accurately load a large amount of metal single atoms around the active site of P-CN, and no one has reported

Method used

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  • Metal single atom loaded carbon-nitrogen polymer catalyst and preparation method thereof
  • Metal single atom loaded carbon-nitrogen polymer catalyst and preparation method thereof
  • Metal single atom loaded carbon-nitrogen polymer catalyst and preparation method thereof

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preparation example Construction

[0035] The preparation method of the metal single atom supported carbon nitrogen polymer catalyst provided by the invention comprises the following steps:

[0036] (1) Put 1-10g of nitrogen-containing precursor into a 10-100mL alumina crucible with a cover, then put it into a muffle furnace, and raise the temperature from room temperature to 520-580°C at a rate of 1-5°C, And calcined at this temperature for 2-5h.

[0037] Wherein, the nitrogen-containing precursor is one or more of urea, melamine and cyanuric acid, when two of urea, melamine and cyanuric acid are used, the two are mixed according to the mass ratio of 1:1 , when three kinds are used, the three kinds are mixed according to the mass ratio of 1:1:1.

[0038] (2) Grinding the block solid obtained after calcination to below 200 mesh to obtain a carbon nitrogen polymer, which is denoted as P-CN.

[0039] (3) Take 0.1-0.5g P-CN and add it to a 30-100mL reaction kettle, add 20-70mL deionized water, and conduct a hydr...

Embodiment 1

[0057] (1) Put 5g of melamine into a 100mL alumina crucible with a cover, and calcinate in a muffle furnace for 3h, with a heating rate of 5°C and a calcining temperature of 550°C.

[0058] (2) Grinding the massive solid obtained after the former is calcined to below 200 mesh to obtain P-CN.

[0059] (3) Take 0.3g of the P-CN prepared by the former and add it to a 100mL reactor, add 70mL of deionized water, and conduct a hydrothermal treatment in an oven at 180°C for 12 hours. After the reaction is completed, the solution is centrifuged, and absolute ethanol and deionized water are alternately Wash 3 times, dry at 80°C for 12 hours, and grind to below 200 mesh to obtain a carbon-nitrogen polymer containing a large number of hydroxyl groups, which is denoted as P-CN-OH.

[0060] (4) Put 0.3g of the P-CN-OH prepared by the former into a 200mL beaker, add 40mL of deionized water, and ultrasonically treat it with a power of 200W for 30min to disperse the P-CN-OH evenly in water. ...

Embodiment 2

[0070] (1) Put 5g of melamine into a 100mL alumina crucible with a cover, and calcinate in a muffle furnace for 3h, with a heating rate of 5°C and a calcining temperature of 550°C.

[0071] (2) Grinding the massive solid obtained after the former is calcined to below 200 mesh to obtain P-CN.

[0072] Take 0.3g of P-CN and add it to a 100mL reactor, add 70mL of deionized water, and conduct a hydrothermal treatment in an oven at 180°C for 12 hours. Dry at ℃ for 12 hours, and grind to below 200 mesh to obtain a carbon-nitrogen polymer containing a large number of hydroxyl groups, which is recorded as P-CN-OH.

[0073] (3) Put 0.3g of P-CN-OH into a 200mL beaker, add 40mL of deionized water, and sonicate with a power of 200W for 30min to disperse P-CN-OH in water evenly.

[0074] (4) Add 10mL of 0.1mol / L CuCl to the solution obtained from the former 2 The solution was stirred at 500 r / min at room temperature and protected from light for 10 hours. After the stirring was completed...

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Abstract

The invention relates to a metal single atom loaded carbon-nitrogen polymer catalyst and a preparation method thereof. The preparation method comprises the following steps: mixing a carbon-nitrogen polymer with water, and carrying out hydrothermal treatment at 150-200 DEG C for 10-15 hours to obtain a hydroxyl-containing carbon-nitrogen polymer; mixing a hydroxyl-containing carbon-nitrogen polymerwith water, carrying out ultrasonic treatment, adding a metal source solution, performing stirring for 8-24 hours in a dark place, performing separating, drying, and calcining to obtain the metal monatomic supported carbon-nitrogen polymer catalyst. The preparation method of the metal single atom loaded carbon-nitrogen polymer is simple, high in universality and accurate and controllable in single atom position loading position, and the prepared metal single atom loaded carbon-nitrogen polymer catalyst is high in loading capacity, rapid in in-plane charge transmission, excellent in photocatalytic performance and high in stability.

Description

technical field [0001] The invention belongs to the field of composite material preparation, and in particular relates to a metal single atom supported carbon nitrogen polymer catalyst and a preparation method thereof. Background technique [0002] Polymer carbon nitrogen (P-CN) is one of the oldest materials reported in the literature, composed of the abundant carbon and nitrogen elements in the earth's crust. P-CN is non-toxic and harmless, with low production cost and visible light response (energy band width around 2.7eV). As a photocatalyst, it has received extensive attention and research from the scientific community. However, the charge transport in the plane is slow and disordered, so that the photoexcited electrons cannot be effectively and accurately transported to the active sites of the catalytic reaction to complete the photocatalytic reaction, which greatly limits its application in the field of photocatalysis. Find a way to directly transport the excited sta...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24B01J35/00B01J37/08B01J37/10
CPCB01J37/082B01J37/10B01J37/08B01J27/24B01J35/391B01J35/39
Inventor 黄宇石先进
Owner INST OF EARTH ENVIRONMENT CHINESE ACAD OF SCI
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