CN113926481A - CNC/g-C3N4Nanocomposite material, preparation and application thereof - Google Patents
CNC/g-C3N4Nanocomposite material, preparation and application thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 17
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- 239000004202 carbamide Substances 0.000 claims abstract description 19
- 239000002114 nanocomposite Substances 0.000 claims abstract description 14
- 229920002678 cellulose Polymers 0.000 claims abstract description 13
- 239000001913 cellulose Substances 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 12
- 239000002159 nanocrystal Substances 0.000 claims abstract description 5
- 239000002994 raw material Substances 0.000 claims abstract description 5
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- 238000010438 heat treatment Methods 0.000 claims description 9
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- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 5
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- 239000011941 photocatalyst Substances 0.000 claims description 4
- 238000007789 sealing Methods 0.000 claims description 2
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 abstract description 10
- 230000001699 photocatalysis Effects 0.000 abstract description 10
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- 238000012986 modification Methods 0.000 abstract description 2
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- 230000015556 catabolic process Effects 0.000 description 9
- 238000006731 degradation reaction Methods 0.000 description 9
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 7
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- 239000013081 microcrystal Substances 0.000 description 6
- 239000002957 persistent organic pollutant Substances 0.000 description 5
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- 239000000843 powder Substances 0.000 description 3
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- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
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- 238000007146 photocatalysis Methods 0.000 description 1
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- 230000015843 photosynthesis, light reaction Effects 0.000 description 1
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
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- 229910052724 xenon Inorganic materials 0.000 description 1
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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Abstract
The invention relates to CNC/g-C3N4The nano composite material is prepared by carrying out thermal polymerization on raw materials containing urea and cellulose nanocrystals to obtain a three-dimensional nano structure with novel structure, namely CNC/g-C, and preparation and application thereof3N4Compared with the graphite-phase carbon nitride prepared by the traditional method, the photocatalytic material prepared by the method has high-efficiency visible light catalytic performance and good stability. The method has simple operation and good repeatability, effectively improves the photocatalytic performance of the graphite-phase carbon nitride, and further expands the efficient means of modification of the graphite-phase carbon nitride.
Description
Technical Field
The invention belongs to the field of functional composite materials and preparation and application thereof, and particularly relates to CNC/g-C3N4Nanocomposite materials, their preparation and use.
Background
Graphite phase carbon nitride (g-C)3N4) Is a non-toxic semiconductor material with cheap and easily obtained raw materials, and is mixed with other common TiO2And ZnO, etc., which do not contain metal elements, have a narrow band gap (2.7ev), and are chemically stable, and thus, g-C3N4Has great potential in the aspects of solar energy conversion, pollutant degradation and the like. At present g-C3N4Has been widely applied to the fields of fuel cells, photocatalytic degradation, gas storage, carbon dioxide reduction, hydrogen production by photolysis and the like. However, g-C prepared by conventional methods3N4The method has the defects of insufficient light absorption, small specific surface area, fast carrier recombination and the like, thereby greatly reducing the degradation efficiency of organic pollutants. Therefore, scholars at home and abroad can improve g-C by various ways3N4Such as metal doping, non-metal doping, morphology control, and compounding with other materials.
CN110327955A is a preparation method of carbon fiber interpenetrating micro-heterojunction carbon nitride photocatalyst, the synthesis steps are complex, and the preparation period is long. The cellulose nano-microcrystal regulates and controls the morphological structure of the cellulose nano-microcrystal, and g-C3N4The nano material is formed on the surface of the nano-sized microcrystal to form a three-dimensional nano structure, and the nano material has the advantages of novel structure, simple synthesis method and good cycle stability. The regulation direction of the conduction band valence band from graphite to carbon nitride is different, and CN110327955A regulates g-C3N4Reduction property, utilization thereof for O2Reduction to produce H2O2The invention improves the g-C by the nano regulation of the structure3N4The oxidizing ability of the compound is applied to photo-oxidative degradation of organic pollutants.
Disclosure of Invention
The invention aims to solve the technical problem of providing a CNC/g-C3N4The nano composite material, the preparation and the application thereof have the advantages of novel structure of CNC/g-C3N4The nano composite material is of three-dimensional nano structure size, and overcomes the defect of the prior artProcess for the preparation of g-C3N4The method has the defects of insufficient light absorption, small specific surface area, fast carrier recombination and the like, and improves the degradation efficiency of the method on organic pollutants.
The invention relates to CNC/g-C3N4The nano composite material is obtained by thermal polymerization of raw materials containing urea and cellulose nanocrystals.
The invention relates to CNC/g-C3N4A method of preparing a nanocomposite comprising:
adding a cellulose nanocrystalline CNC solution into the molten urea, uniformly stirring, calcining, and cooling to obtain CNC/g-C3N4A nanocomposite material.
The preferred mode of the above preparation method is as follows:
the molten urea is specifically: and (3) putting the urea in a container, sealing the container, and heating the container in an oil bath kettle at 140-150 ℃ to melt the urea.
The concentration of the cellulose nanocrystalline CNC solution is 0.5-2.5 g/L.
The mass ratio of the CNC to the urea is as follows: 1: 2.8X 105～1:1.25×105。
The stirring time is 5-10 min.
The calcining is carried out at the temperature rising speed of 3-10 ℃/min from room temperature to 350-400 ℃, and calcining is carried out for 1-2 h at the temperature; then, the temperature is increased from the set temperature to 550-600 ℃ at the heating rate of 3-10 ℃/min, and the mixture is calcined for 2-3 h at the temperature.
And pouring the mixture into a crucible after uniformly stirring, tightly wrapping the crucible with tinfoil, tightly covering a crucible cover, calcining in a muffle furnace, and opening the cover to cool after the temperature of the muffle furnace is reduced to 200 ℃.
The CNC/g-C of the invention3N4The application of the nano composite material as a photocatalyst.
The cellulose nano-microcrystal regulates and controls the morphological structure of the cellulose nano-microcrystal, and g-C3N4The nanometer material is formed on the surface of the nanometer microcrystal to form three-dimensional nanometer structure size, the structure is novel, the synthesis method is simple, and the method follows the processThe ring stability is good.
The invention improves the g-C by the nano regulation and control of the structure3N4The oxidizing ability of the compound is applied to photo-oxidative degradation of organic pollutants.
The Cellulose Nanocrystal (CNC) is a rigid short rod-shaped crystal with the diameter of 2-20 nm and the length of 100-500 nm. The crystallinity is high, and the nano biomass carbon with higher graphitization degree and larger specific surface area can be prepared by being used as a carbon precursor. g-C3N4On one hand, the hybridization with CNC can utilize the high-quality conductivity of the carbon material to inhibit the recombination of photon-generated carriers; on the other hand, the CNC has larger specific surface area and is simultaneously reacted with g-C in the polymerization process3N4C-O-C bonds are formed between the two, so that the hydrophilicity is improved. The synergy of these factors enables the preparation of CNC/g-C3N4The photocatalytic material has excellent and stable photocatalytic performance and has important application potential in the aspect of environmental purification.
Advantageous effects
1. The invention adopts a one-step polymerization method, and the preparation method is simple and easy to implement, has strong repeatability and does not need subsequent treatment.
2. The product of the invention is subjected to visible light photocatalysis performance test, and the result shows that the CNC/g-C prepared by the invention3N4The degradation rate of the composite photocatalytic material to rhodamine B simulation wastewater reaches more than 95 percent, and g-C prepared under the same condition3N4The degradation rate is only about 45%.
3. CNC/g-C prepared by the method of the invention3N4The composite photocatalytic material can inhibit the recombination of photon-generated carriers. In addition, CNC and g-C3N4The formed C-O-C bond increases the hydrophilicity of the material and is similar to the original g-C3N4Compared with the formula, CNC/g-C3N4The nanocomposite material exhibits stronger adsorption and photocatalytic activity.
Drawings
FIG. 1 is the CNC/g-C produced in example 13N4And g-C prepared in comparative example 13N4Photocatalyst pair RhB degradation efficiency versus graph.
FIG. 2 shows the cycling stability of example 1.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
Raw material sources and specification parameters:
urea (analytical reagent, chemical reagent of national medicine group);
rhodamine B (RhB) analytically pure, Shanghai Tantan technology;
cellulose Nanocrystal (CNC) (50-200 nm in length, 5-20 nm in diameter, molecular weight of 35000 or so, Shanghai Lensi nanotechnology Co., Ltd.)
Example 1
(1) 10.5g of urea was weighed into a 150mL beaker and sealed, and the beaker was placed in a 150 ℃ oil bath and heated.
(2) After the urea is completely melted, 40 mul CNC solution (1g/L) is added, stirred for 5min and mixed evenly.
(3) After the reactants are mixed uniformly, pouring the mixture into a 30mL corundum crucible, tightly wrapping the crucible by using high-temperature-resistant tinfoil, tightly covering the crucible cover, placing the crucible cover in a muffle furnace, performing high-temperature treatment in the air atmosphere, and calcining for 1h at 400 ℃ at room temperature at the heating rate of 5 ℃/min. Then the temperature is increased to 550 ℃ and the mixture is calcined for 3h (the temperature rising rate is 5 ℃/min).
(4) And opening the cover and cooling after the muffle furnace is cooled to 200 ℃, taking out the corundum crucible and opening the sealed tinfoil to obtain light yellow catalyst powder.
Example 2
(1) 21g of urea was weighed into a 150mL beaker and sealed, and the beaker was placed in a 150 ℃ oil bath and heated.
(2) After the urea is completely melted, 80 mul CNC solution (1g/L) is added, stirred for 5min and mixed evenly.
(3) After the reactants are mixed uniformly, pouring the mixture into a 30mL corundum crucible, tightly wrapping the crucible by using high-temperature-resistant tinfoil, tightly covering the crucible cover, placing the crucible cover in a muffle furnace, performing high-temperature treatment in the air atmosphere, and calcining for 1h at 400 ℃ at room temperature at the heating rate of 5 ℃/min. Then the temperature is increased to 600 ℃ and the mixture is calcined for 3h (the temperature rising rate is 5 ℃/min).
(4) And opening the cover and cooling after the muffle furnace is cooled to 200 ℃, taking out the corundum crucible and opening the sealed tinfoil to obtain light yellow catalyst powder.
Comparative example 1
At room temperature, 10.5g of urea is added into a crucible, the crucible is covered with a crucible cover after being sealed by tinfoil, the crucible is transferred into a muffle furnace for heat treatment, and the temperature is raised to 400 ℃ at the temperature rise rate of 5 ℃/min for calcining for 1 h. Then the temperature is raised to 550 ℃ at the speed of 5 ℃/min and the mixture is calcined for 3 h. A yellow powder, namely graphite phase carbon nitride, abbreviated gCN, is obtained.
Taking example 1 as an example, the performance of the test is tested:
the product of example 1 is applied to the explanation of degrading rhodamine B, and specifically comprises the following steps:
respectively weighing 20mg of catalyst and dispersing in 50mL of rhodamine B solution with the initial concentration of 5mg/L, starting a magnetic stirrer, and carrying out dark adsorption for 30min to ensure that the catalyst and the target degradation product reach adsorption and desorption balance. Subsequently, a 500W xenon lamp was turned on, 4mL samples were taken every 30min, filtered through a 0.22 μm microporous filter, and the absorbance of the solution was measured by a UV-3100 type UV-visible spectrophotometer at the maximum absorption wavelength of each substance. The results show that the CNC/g-C prepared by the invention3N4The composite photocatalytic material has a degradation rate of more than 95% for rhodamine B simulation wastewater, and after circulation for 3 times, the degradation rate can still reach more than 85%, and the circulation performance is good. g-C prepared under the same conditions as in comparative example 13N4The degradation rate is only about 45%.
The structure of the invention is different from that of CN110327955A, CN110327955A mainly applies reduction to produce hydrogen peroxide, and the invention obtains a photocatalytic material with novel structure and high catalytic efficiency by regulating and controlling the size of a three-dimensional nano structure, thereby improving the adsorption and oxidation performance of graphite-phase carbon nitride and promoting the graphite-phase carbon nitride to more effectively oxidize and degrade organic pollutants. Both are not comparable in the direction of application.
Claims (9)
1. CNC/g-C3N4The nano composite material is characterized in that the nano composite material is obtained by thermal polymerization of raw materials containing urea and cellulose nanocrystals.
2. CNC/g-C3N4A method of preparing a nanocomposite comprising:
adding a cellulose nanocrystalline CNC solution into the molten urea, uniformly stirring, calcining, and cooling to obtain CNC/g-C3N4A nanocomposite material.
3. The process according to claim 2, characterized in that said molten urea is in particular: and (3) putting the urea in a container, sealing, and placing the container in an oil bath pan for heating, wherein the temperature of the oil bath pan is 140-150 ℃, so that the urea is completely melted.
4. The preparation method according to claim 2, wherein the concentration of the cellulose nanocrystalline CNC solution is 0.5-2 g/L.
5. The preparation method according to claim 2, wherein the mass ratio of CNC to urea is: 1: 2.8X 105～1:1.25×105。
6. The preparation method according to claim 2, wherein the stirring time is 5 to 10 min.
7. The preparation method according to claim 2, wherein the calcination is carried out by heating from room temperature to 350-400 ℃ at a heating rate of 3-10 ℃/min, and calcining for 1-2 h at the temperature; then, the temperature is increased from the set temperature to 550-600 ℃ at the heating rate of 3-10 ℃/min, and the mixture is calcined for 2-3 h at the temperature.
8. The preparation method of claim 2, wherein the mixture is stirred, mixed uniformly, poured into a crucible, tightly wrapped by tinfoil, covered by a crucible cover, calcined in a muffle furnace, and cooled after the temperature of the muffle furnace is reduced to 200 ℃.
9. The CNC/g-C of claim 13N4The application of the nano composite material as a photocatalyst.
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| CN116586096A (en) * | 2023-05-26 | 2023-08-15 | 昆明理工大学 | Carbon nitride modified biochar material and preparation method thereof |
| CN118637568A (en) * | 2024-08-13 | 2024-09-13 | 山东石油化工学院 | Micron-sized carbon nitride and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114988515A (en) * | 2022-04-21 | 2022-09-02 | 南京林业大学 | Method for removing Cr (VI) and g-C adopted by same 3 N 4 Composite foam/cellulose/GO |
| CN116586096A (en) * | 2023-05-26 | 2023-08-15 | 昆明理工大学 | Carbon nitride modified biochar material and preparation method thereof |
| CN118637568A (en) * | 2024-08-13 | 2024-09-13 | 山东石油化工学院 | Micron-sized carbon nitride and preparation method and application thereof |
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