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Preparation method of graphite type carbon nitride photocatalytic material

A catalytic material, graphite-based technology, used in chemical instruments and methods, physical/chemical process catalysts, chemical/physical processes, etc., can solve problems such as product agglomeration, low specific surface area, and damage to semiconductor characteristics, and achieve visible light catalytic efficiency. High, broad application prospects, the effect of reducing the compound rate

Inactive Publication Date: 2015-04-08
JIANGSU UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] The problem of environmental pollution has increasingly become a major concern in today's society. In recent years, g-C 3 N 4 As a new type of important organic photocatalytic material, it has attracted wide attention due to the fact that C 3 N 4 Special semiconductor structure (Eg≈2.7eV), good stability, layered structure and easy-to-obtain raw materials are considered to have the potential to catalyze the degradation of organic pollutants; however, a large number of studies have found that high electron-hole recombination rate , low utilization rate of visible light, low specific surface area, low electron transport efficiency and easy agglomeration morphology limit its application in the field of photocatalysis
[0003] Copolymerization of dicyandiamide and barbituric acid, the obtained product has excellent visible light absorption ability, but this experiment only uses a simple heating method, which makes the product appear serious agglomeration phenomenon, which reduces the separation efficiency of photogenerated electron-hole pairs , and excessive barbituric acid will also destroy the semiconductor characteristics; although high temperature calcination is beneficial to improve the crystallinity of the product and improve the separation efficiency of photogenerated electron-hole pairs, but too high temperature is not conducive to the stability of the product, so adopt A suitable heating temperature and heating method is to prepare layered C 3 N 4 In addition, using metal chloride or bromide as the heating medium to calcinate dicyandiamide can obtain carbon-nitrogen polymers with high crystallinity and obvious layered characteristics. 3 N 4 The structural unit is a triazine structure, which is not conducive to its efficient use of visible light; more importantly, the complicated experimental process and harsh conditions in the experiment also make it difficult to transform the experiment into a real production technology

Method used

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  • Preparation method of graphite type carbon nitride photocatalytic material
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  • Preparation method of graphite type carbon nitride photocatalytic material

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preparation example Construction

[0022] A method for preparing a graphite-type carbon nitride photocatalytic material, the preparation method comprising the following steps:

[0023] (1) Thoroughly grind and mix barbituric acid, dicyandiamide, lithium chloride and potassium chloride.

[0024] (2) The mixture is placed in a calcination vessel and calcined under a nitrogen atmosphere.

[0025] (3) Grinding the calcined product, ultrasonication, centrifugation, and drying to obtain the g-C 3 N 4 catalyst.

[0026] The molar ratio of barbituric acid and dipolycyanamide described in step (1) is between 0.04~0.22; The mass ratio of described lithium chloride and potassium chloride is 9:11; The described lithium chloride and chlorine The mass ratio of the total mass of potassium chloride to dipolycyanamide is 5:1.

[0027] The calcination process described in step (2) is: heating to 400°C at a rate of 7°C / min, holding for 6 hours, continuing to heat at the same heating rate to 570°C, and holding for 12 hours...

Embodiment 1

[0031] Example 1: Block g-C 3 N 4 Catalyst preparation

[0032] Take 2g of dicyandiamide and put it into a corundum ark, place it in the middle of a tube furnace, heat it up to 550°C at a heating rate of 2.5°C / min, and keep it at 550°C for 4 hours. The whole process is carried out under the protection of nitrogen. After natural cooling, it was taken out and ground with a mortar to obtain a yellow powder sample.

Embodiment 2

[0033] Embodiment 2: layered modified g-C 3 N 4 preparation of

[0034] Take 2g of dicyandiamide, 0.29g of barbituric acid (the molar ratio of barbituric acid to dicyandiamide is 0.10), 4.5g of lithium chloride, and 5.5g of potassium chloride, and grind them in a mortar for 20 minutes ; Place the mixture in the middle of the tube furnace, heat it to 400°C at a rate of 7°C / min, and keep it at 400°C for 6 hours; continue to heat it to 570°C at a rate of 7°C / min, and keep it at 570°C After 12 hours, the whole process was carried out under the protection of nitrogen. After natural cooling, the block was taken out, ground for 20 minutes, ultrasonicated for 1 hour, rinsed with boiling water at 100°C for 3 times, and centrifuged at a rate of 10,000 rpm for 5 minutes, take out the suspension, and dry it at 80°C for 2 days to obtain the final sample.

[0035] The catalyst prepared by the method of embodiment 1 and 2, after X-ray diffractometer scanning, see figure 1 , the synt...

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Abstract

The invention discloses a preparation method of a graphite type carbon nitride photocatalytic material, belonging to the field of the material preparation and photocatalytic technology. The graphite type carbon nitride photocatalytic material takes dicyandiamide and barbituric acid as co-precursors, adopts lithium chloride and potassium chloride as heating mediums, and is prepared in protective atmosphere through directly burning. The prepared g-C3N4 has excellent visible light absorption ability and the laminated structure characteristics, and has the degradation efficiency up to 83.8% to rhodamine B within 90min under visible light. The preparation method is simple, the raw materials are easily available, the visible light catalytic efficiency is high, and the graphite type carbon nitride photocatalytic material has wide application prospect in the photocatalytic field.

Description

technical field [0001] The invention belongs to the field of visible light catalysis, and in particular relates to a preparation method of a graphite-type carbon nitride photocatalytic material and its application in catalytically degrading pollutants in water under visible light. Background technique [0002] The problem of environmental pollution has increasingly become a major concern in today's society. In recent years, g-C 3 N 4 As a new type of important organic photocatalytic material, it has attracted wide attention due to the fact that C 3 N 4 Special semiconductor structure (Eg≈2.7eV), good stability, layered structure and easy-to-obtain raw materials are considered to have the potential to catalyze the degradation of organic pollutants; however, a large number of studies have found that high electron-hole recombination rate , low utilization rate of visible light, low specific surface area, low electron transport efficiency and easy agglomeration morphology lim...

Claims

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Application Information

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IPC IPC(8): B01J27/24C02F1/30
Inventor 严学华邹涵任杰缪进进吴肖沙大巍戴煜
Owner JIANGSU UNIV
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