CN113926481B - CNC/g-C3N4Nanocomposite, preparation and use thereof - Google Patents
CNC/g-C3N4Nanocomposite, preparation and use thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title abstract description 11
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000004202 carbamide Substances 0.000 claims abstract description 19
- 239000002114 nanocomposite Substances 0.000 claims abstract description 16
- 229920002678 cellulose Polymers 0.000 claims abstract description 12
- 239000001913 cellulose Substances 0.000 claims abstract description 12
- 239000002159 nanocrystal Substances 0.000 claims abstract description 4
- 238000012719 thermal polymerization Methods 0.000 claims abstract description 3
- 238000001354 calcination Methods 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 8
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 239000011941 photocatalyst Substances 0.000 claims description 4
- 238000007789 sealing Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 21
- 230000001699 photocatalysis Effects 0.000 abstract description 11
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 abstract description 8
- 239000002086 nanomaterial Substances 0.000 abstract description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 4
- 229910002804 graphite Inorganic materials 0.000 abstract description 4
- 239000010439 graphite Substances 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 4
- 238000007146 photocatalysis Methods 0.000 abstract description 2
- 230000015556 catabolic process Effects 0.000 description 11
- 238000006731 degradation reaction Methods 0.000 description 11
- 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
- 229940043267 rhodamine b Drugs 0.000 description 7
- 239000002131 composite material Substances 0.000 description 5
- 239000013081 microcrystal Substances 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 4
- 229910052593 corundum Inorganic materials 0.000 description 4
- 239000010431 corundum Substances 0.000 description 4
- 239000002957 persistent organic pollutant Substances 0.000 description 4
- 230000006798 recombination Effects 0.000 description 4
- 238000005215 recombination Methods 0.000 description 4
- 238000001179 sorption measurement Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000002028 Biomass Substances 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 239000000969 carrier Substances 0.000 description 2
- 239000003610 charcoal Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000031700 light absorption Effects 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 230000000877 morphologic effect Effects 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000001308 synthesis method Methods 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229920001046 Nanocellulose Polymers 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 239000007833 carbon precursor Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 239000007857 degradation product Substances 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000005087 graphitization Methods 0.000 description 1
- 238000009396 hybridization Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000010525 oxidative degradation reaction Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000007539 photo-oxidation reaction Methods 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- 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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- B—PERFORMING OPERATIONS; TRANSPORTING
- 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
-
- 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
-
- 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 a CNC/g-C 3N4 nano composite material, a preparation method and an application thereof, wherein the nano composite material is prepared from raw materials containing urea and cellulose nanocrystals through thermal polymerization to obtain a CNC/g-C 3N4 nano composite material with three-dimensional nano structure size and novel structure. The invention has simple operation and good repeatability, effectively improves the photocatalysis performance of the graphite phase carbon nitride, and further expands the high-efficiency means of modifying 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 a CNC/g-C 3N4 nano composite material and preparation and application thereof.
Background
The graphite-phase carbon nitride (g-C 3N4) is a nontoxic semiconductor material with cheap and easily available raw materials, and compared with other commonly used semiconductor materials such as TiO 2, znO and the like, the graphite-phase carbon nitride has the advantages of no metal element, narrower band gap (2.7 ev) and good chemical stability, so the g-C 3N4 has great potential in the aspects of solar energy conversion, pollutant degradation and the like. At present, g-C 3N4 is widely applied to various fields such as fuel cells, photocatalytic degradation, gas storage, carbon dioxide reduction, hydrogen production by photocatalytic water splitting and the like. However, the g-C 3N4 prepared by the traditional method has the defects of insufficient light absorption, small specific surface area, rapid carrier recombination and the like, thereby greatly reducing the degradation efficiency of organic pollutants. Therefore, scholars at home and abroad can improve the photocatalytic capability of g-C 3N4 through various ways, such as metal doping, nonmetal doping, morphology regulation, compounding with other materials and the like.
The preparation method of the CN110327955A carbon fiber interpenetrating micro heterojunction carbon nitride photocatalyst has the advantages of complex synthesis steps and long preparation period. The cellulose nano microcrystal regulates and controls the morphological structure, and the g-C 3N4 nano material is formed on the surface of the microcrystal with nano size to form the three-dimensional nano structure size, so that the cellulose nano microcrystal has novel structure, simple synthesis method and good circulation stability. The conduction band valence band regulation and control directions of graphite to carbon nitride are different, CN110327955A regulates and controls the reduction performance of g-C 3N4, and the reduction performance is applied to O 2 reduction to generate H 2O2.
Disclosure of Invention
The invention aims to solve the technical problem of providing a CNC/g-C 3N4 nano composite material, and preparation and application thereof, wherein the CNC/g-C 3N4 nano composite material with a novel structure is of a three-dimensional nano structure size, so that the defects of insufficient light absorption, small specific surface area, rapid carrier recombination and the like of g-C 3N4 prepared by a traditional method are overcome, and the degradation efficiency of the composite material on organic pollutants is improved.
The CNC/g-C 3N4 nano composite material is obtained by thermal polymerization of a raw material containing urea and cellulose nanocrystals.
The invention discloses a preparation method of a CNC/g-C 3N4 nano composite material, which comprises the following steps:
Adding cellulose nanocrystalline CNC solution into the melted urea, stirring, mixing uniformly, calcining, and cooling to obtain the CNC/g-C 3N4 nanocomposite.
The preferred mode of the preparation method is as follows:
The melted urea is specifically: and (3) placing urea in a container and sealing, and placing the container in an oil bath pot at 140-150 ℃ for heating to melt the urea.
The concentration of the cellulose nanocrystalline CNC solution is 0.5-2.5 g/L.
The mass ratio of CNC to urea is as follows: 1:2.8X10 5～1:1.25×105.
The stirring time is 5-10 min.
The calcination is to heat from room temperature to 350-400 ℃ at a heating rate of 3-10 ℃/min, and calcine for 1-2 h at the temperature; then the temperature is set to 550-600 ℃ at a heating rate of 3-10 ℃/min, and the calcination is carried out for 2-3 h at the temperature.
Pouring the mixture into a crucible after stirring and mixing uniformly, tightly wrapping the crucible by using tinfoil, tightly covering a crucible cover, calcining in a muffle furnace, and uncovering and cooling after the muffle furnace is cooled to 200 ℃.
The CNC/g-C 3N4 nano composite material is applied as a photocatalyst.
The cellulose nanometer microcrystal regulates and controls the morphological structure, and the g-C 3N4 nanometer material is formed on the surface of the nanometer microcrystal to form the three-dimensional nanometer structure, so that the structure is novel, the synthesis method is simple, and the cycle stability is good.
The invention improves the oxidation capability of g-C 3N4 through the structure nano regulation and control, and applies the g-C 3N4 to the photooxidation degradation of organic pollutants.
The cellulose nanocrystalline (cellulose nanocrystal, CNC) is a rigid short rod-like crystal with a diameter of 2-20 nm and a length of 100-500 nm. The crystallinity is high, and the nano biomass charcoal with higher graphitization degree and larger specific surface area can be prepared by using the nano biomass charcoal as a carbon precursor. On one hand, the g-C 3N4 and CNC hybridization can utilize the high-quality conductivity of the carbon material to inhibit the recombination of photogenerated carriers; on the other hand, CNC has larger specific surface area, and meanwhile, a C-O-C bond is formed between the CNC and g-C 3N4 in the polymerization process, so that the hydrophilicity is improved. The synergistic effect of the factors ensures that the prepared CNC/g-C 3N4 photocatalytic material has excellent and stable photocatalytic performance and has important application potential in the aspect of environmental purification.
Advantageous effects
1. The preparation method adopts a one-step polymerization method, is simple and easy to implement, has strong repeatability and does not need subsequent treatment.
2. The results of the visible light photocatalytic performance test of the product show that the degradation rate of the CNC/g-C 3N4 composite photocatalytic material prepared by the invention on rhodamine B simulated wastewater reaches more than 95%, and the degradation rate of g-C 3N4 prepared under the same condition is only about 45%.
3. The CNC/g-C 3N4 composite photocatalytic material prepared by the method can inhibit the recombination of photogenerated carriers. In addition, the C-O-C bond formed between CNC and g-C 3N4 improves the hydrophilicity of the material, and the CNC/g-C 3N4 nanocomposite material shows stronger adsorption and photocatalytic activity compared with the original g-C 3N4.
Drawings
FIG. 1 is a graph comparing the degradation efficiency of the CNC/g-C 3N4 prepared in example 1 and the g-C 3N4 photocatalyst prepared in comparative example 1 to RhB.
Figure 2 is the cycling stability of example 1.
Detailed Description
The application will be further illustrated with reference to specific examples. It is to be understood that these examples are illustrative of the present application and are not intended to limit the scope of the present application. Furthermore, it should be understood that various changes and modifications can be made by one skilled in the art after reading the teachings of the present application, and such equivalents are intended to fall within the scope of the application as defined in the appended claims.
Raw material sources and specification parameters:
Urea (analytically pure, national drug group chemicals);
rhodamine B (RhB) analytically pure, shanghai taitant technology;
Cellulose Nanocrystalline (CNC) (length 50-200 nm, diameter 5-20 nm, molecular weight: 35000 or so, shanghai flash Nano technology Co., ltd.)
Example 1
(1) 10.5G urea was weighed into a 150mL beaker and sealed, and the beaker was placed in an oil bath at 150℃and heated.
(2) After the urea was completely melted, 40. Mu.l CNC solution (1 g/L) was added and stirred for 5min, and mixed well.
(3) After the reactants are uniformly mixed, pouring the mixture into a 30mL corundum crucible, tightly wrapping the crucible by high-temperature-resistant tinfoil, tightly covering a crucible cover, placing the crucible cover in a muffle furnace, performing high-temperature treatment under an air atmosphere, and calcining at the temperature rising rate of 5 ℃/min for 1h at 400 ℃ at room temperature. Then heating to 550 ℃ and calcining for 3 hours (the heating rate is 5 ℃/min).
(4) And opening the cover to cool after the muffle furnace is cooled to 200 ℃, taking out the corundum crucible, opening the sealed tinfoil, and obtaining 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 was completely melted, 80. Mu.l CNC solution (1 g/L) was added and stirred for 5min, and mixed well.
(3) After the reactants are uniformly mixed, pouring the mixture into a 30mL corundum crucible, tightly wrapping the crucible by high-temperature-resistant tinfoil, tightly covering a crucible cover, placing the crucible cover in a muffle furnace, performing high-temperature treatment under an air atmosphere, and calcining at the temperature rising rate of 5 ℃/min for 1h at 400 ℃ at room temperature. Then heating to 600 ℃ and calcining for 3 hours (the heating rate is 5 ℃/min).
(4) And opening the cover to cool after the muffle furnace is cooled to 200 ℃, taking out the corundum crucible, opening the sealed tinfoil, and obtaining 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 tin foil after being closed, and the crucible is transferred into a muffle furnace for heat treatment, and the temperature is raised to 400 ℃ at a heating rate of 5 ℃/min, and the crucible is calcined for 1h. Then the mixture is heated to 550 ℃ at 5 ℃/min and calcined for 3 hours. A yellow powder, i.e. graphite-phase carbon nitride, abbreviated gCN, was obtained.
Taking example 1 as an example, the performance was tested:
The teaching of applying the product of example 1 to the degradation of rhodamine B comprises in particular the following steps:
20mg of catalyst is weighed and dispersed in 50mL of rhodamine B solution with initial concentration of 5mg/L respectively, a magnetic stirrer is started, and the catalyst and target degradation products reach adsorption and desorption balance after dark adsorption for 30 min. Subsequently, a 500W xenon lamp was turned on, 4mL was sampled every 30 minutes, and the solution was filtered through a 0.22 μm microporous filter membrane, and the absorbance of the solution was measured at the maximum absorption wavelength of each substance by a UV-3100 type ultraviolet-visible spectrophotometer. The result shows that the degradation rate of the CNC/g-C 3N4 composite photocatalytic material prepared by the invention on rhodamine B simulated wastewater reaches more than 95%, and after 3 times of circulation, the degradation rate still reaches more than 85%, and the circulation performance is good. And the degradation rate of g-C 3N4 prepared under the same condition as that of comparative example 1 is only about 45%.
The invention is different from the CN 110327955A in structure, the CN 110327955A is mainly used for producing hydrogen peroxide by reducing, and the invention aims at obtaining the photocatalysis material with novel structure and high catalytic efficiency by regulating and controlling the three-dimensional nano structure size, improving the adsorption and oxidation performance of graphite phase carbon nitride and promoting the more effective oxidative degradation of organic pollutants. There is no comparability between the two in the application direction.
Claims (5)
1. A method for preparing a CNC/g-C 3N4 nanocomposite, comprising:
Adding a cellulose nanocrystalline CNC solution into the melted urea, stirring, mixing uniformly, calcining, and cooling to obtain a CNC/g-C 3N4 nanocomposite; pouring the mixture into a crucible after stirring and mixing uniformly, tightly wrapping the crucible by using tinfoil, tightly covering a crucible cover, calcining in a muffle furnace, and uncovering and cooling after the muffle furnace is cooled to 200 ℃;
wherein the calcination is to heat up from room temperature to 350-400 ℃ at a heating rate of 3-10 ℃/min, and calcine for 1-2 h at the temperature; then the temperature is set to 550-600 ℃ at a heating rate of 3-10 ℃/min, and the calcination is carried out for 2-3 h at the temperature; wherein the concentration of the cellulose nanocrystalline CNC solution is 0.5-2g/L; the mass ratio of CNC to urea is as follows: 1:2.8X10 5～1:1.25×105.
2. The method according to claim 1, characterized in that said melted urea is in particular: and (3) placing the urea in a container and sealing, and heating the container in an oil bath at 140-150 ℃ to enable the urea to be completely melted.
3. The method according to claim 1, wherein the stirring time is 5 to 10 minutes.
4. A CNC/g-C 3N4 nanocomposite prepared according to the process of claim 1, characterized in that it is obtained by thermal polymerization from a feedstock containing urea, cellulose nanocrystals.
5. Use of the CNC/g-C 3N4 nanocomposite of claim 1 as a photocatalyst.
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| CN108295904A (en) * | 2018-02-02 | 2018-07-20 | 陕西科技大学 | A kind of cu ferrite/Cellulose nanocrystal catalyst and preparation method thereof |
| CN110327955B (en) * | 2019-06-13 | 2022-01-04 | 福建农林大学 | Preparation method of carbon fiber interpenetrating micro-heterojunction carbon nitride photocatalyst |
| CN110560127A (en) * | 2019-09-09 | 2019-12-13 | 辽宁石油化工大学 | Preparation method of graphite phase carbon nitride with large specific surface area |
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