CN114011447A - Preparation method of porous carbon nitride foam/hydrotalcite three-dimensional heterojunction material and application of porous carbon nitride foam/hydrotalcite three-dimensional heterojunction material in photocatalytic reduction of carbon dioxide - Google Patents
Preparation method of porous carbon nitride foam/hydrotalcite three-dimensional heterojunction material and application of porous carbon nitride foam/hydrotalcite three-dimensional heterojunction material in photocatalytic reduction of carbon dioxide Download PDFInfo
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- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 title claims abstract description 76
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 title claims abstract description 74
- 239000006260 foam Substances 0.000 title claims abstract description 73
- 229960001545 hydrotalcite Drugs 0.000 title claims abstract description 58
- 229910001701 hydrotalcite Inorganic materials 0.000 title claims abstract description 58
- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 title claims abstract description 56
- 239000000463 material Substances 0.000 title claims abstract description 52
- 229910002092 carbon dioxide Inorganic materials 0.000 title claims abstract description 38
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 230000009467 reduction Effects 0.000 title claims abstract description 11
- 239000001569 carbon dioxide Substances 0.000 title claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 9
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- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 7
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- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 7
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- 238000006243 chemical reaction Methods 0.000 claims description 54
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 239000008367 deionised water Substances 0.000 claims description 15
- 229910021641 deionized water Inorganic materials 0.000 claims description 15
- 229910052751 metal Inorganic materials 0.000 claims description 15
- 239000002184 metal Substances 0.000 claims description 15
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 14
- 150000003839 salts Chemical class 0.000 claims description 12
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- 238000001035 drying Methods 0.000 claims description 9
- 229910002651 NO3 Inorganic materials 0.000 claims description 7
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 7
- -1 iron ion Chemical class 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 6
- 229920000877 Melamine resin Polymers 0.000 claims description 5
- 239000012295 chemical reaction liquid Substances 0.000 claims description 5
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 4
- 229910052742 iron Inorganic materials 0.000 claims description 4
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 4
- 229910001453 nickel ion Inorganic materials 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 3
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 2
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 2
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 2
- 239000012300 argon atmosphere Substances 0.000 claims description 2
- 229910001429 cobalt ion Inorganic materials 0.000 claims description 2
- XLJKHNWPARRRJB-UHFFFAOYSA-N cobalt(2+) Chemical compound [Co+2] XLJKHNWPARRRJB-UHFFFAOYSA-N 0.000 claims description 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 2
- 229910001425 magnesium ion Inorganic materials 0.000 claims description 2
- 230000008569 process Effects 0.000 claims description 2
- 239000002131 composite material Substances 0.000 abstract description 26
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 7
- 238000002336 sorption--desorption measurement Methods 0.000 description 7
- 229910052724 xenon Inorganic materials 0.000 description 7
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 7
- 238000005520 cutting process Methods 0.000 description 6
- 229910000608 Fe(NO3)3.9H2O Inorganic materials 0.000 description 5
- LDDQLRUQCUTJBB-UHFFFAOYSA-N ammonium fluoride Chemical compound [NH4+].[F-] LDDQLRUQCUTJBB-UHFFFAOYSA-N 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 238000010335 hydrothermal treatment Methods 0.000 description 5
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 5
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- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
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- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
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- 125000000129 anionic group Chemical group 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052599 brucite Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
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- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 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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- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/007—Mixed salts
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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
- B01J35/20—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state
- B01J35/23—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state in a colloidal state
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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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- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
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Abstract
The invention discloses a preparation method of a porous carbon nitride foam/hydrotalcite three-dimensional heterojunction material and application of the porous carbon nitride foam/hydrotalcite three-dimensional heterojunction material in photocatalytic reduction of carbon dioxide. The method is rich in g-C3N4The porous carbon nitride foam is used as a carrier, urea is used as a precipitator, hydrotalcite nano-sheets are grown on the surface of the carrier in situ by adopting a hydrothermal method, and the porous carbon nitride foam is cut to obtain the nano-hydrotalcite nano-sheets with the thickness of 1-4mm and g-C3N4Porous carbon nitride foam with a hydrotalcite heterojunction structure/a hydrotalcite three-dimensional heterojunction material. According to the invention, the carbon nitride foam is selected as the carrier of the hydrotalcite, the problem of easy agglomeration of the hydrotalcite is solved by regulating and controlling the thickness of the material, and the CO of the composite material is effectively improved by utilizing the photocatalytic synergistic effect of the heterojunction2Adsorption PropertyAnd the photocatalytic performance is greatly improved, and the photocatalytic CO is greatly improved2Yield of reduction reaction. This is optimal when the thickness is 3mm, the composite material having the highest CO generation rate of 52.17 μmol g‑1h‑1。
Description
Technical Field
The invention belongs to the technical field of composite material preparation, and particularly relates to a preparation method of a porous carbon nitride foam/hydrotalcite three-dimensional heterojunction material and application of the porous carbon nitride foam/hydrotalcite three-dimensional heterojunction material in photocatalytic reduction of carbon dioxide.
Background
With the rapid development of modern industry, the energy crisis is caused by the excessive utilization of a large amount of fossil fuels, and the greenhouse effect is caused by excessive emission of carbon dioxide. Energy crisis and greenhouse effect seriously affect human survival and social development, and the control of CO2 emission becomes a key problem facing all human beings. The photocatalytic conversion technology using solar energy as a direct driving force is one of the ideal ways to effectively convert CO 2. The photocatalytic conversion technology can reduce CO2 into high-added-value fuels such as CO, methane and the like or other chemicals by utilizing a semiconductor catalyst at normal temperature and normal pressure, can even directly utilize solar energy and visible light to realize carbon cycle, and has the advantages of environmental protection, no secondary pollution and the like. Aiming at the problems of energy crisis, greenhouse effect caused by the increase of the concentration of CO2 and the like, the photocatalysis technology is considered as an ideal way for solving the two problems and has huge application prospect. Since the photocatalytic technology mainly uses semiconductors as catalysts, the development of novel and efficient CO2 adsorption and photocatalytic materials is the key point for breakthrough of the photocatalytic technology.
Hydrotalcite, also known as Layered Double Hydroxide (LDHs), has a general structural formula: [ M2+1-xM3+ x (OH)2] [ An- ] x/n.mH 2O, wherein M is a metal element, x is the molar ratio of the metal element, and An-is An interlayer anion, and the material is a typical anionic two-dimensional inorganic layered material and is composed of a brucite main layer plate with positive charges, the interlayer anion and solvation molecules. Because of the characteristics of laminate adjustability, chemical component variability, easy synthesis, thermal stability and memory effect, the composite material has been widely applied in the fields of photocatalysis and the like, and becomes one of the hot research contents in the field of energy and chemical industry at present. Nevertheless, the LDHs-based photocatalyst still has the defects of small specific surface area, complex recovery steps, low visible light utilization rate, easy agglomeration, low electron mobility, high photo-generated carrier recombination speed and the like in practical application, and the application of the LDHs-based photocatalyst in the field of photocatalytic reduction of CO2 is limited.
In addition, among many semiconductor-based photocatalysts, graphite-like phase carbon nitride (g-C3N4) has received attention for its excellent properties such as excellent chemical stability, inexpensive raw material source, strong C — N covalent bond, strong reducing property, easy preparation, no metal component, visible light response, and tunable electronic structure. But still has the problems of small specific surface area, low utilization efficiency of visible light, rapid recombination of photon-generated carriers, low quantum efficiency, lower specific surface area and the like.
In order to solve the above problems, various strategies have been adopted: the method comprises the steps of constructing a heterojunction by doping nitrogen vacancies or oxygen vacancies and noble metals or heteroatoms, introducing defects, and carrying out morphology control on the photocatalyst, for example, the photocatalyst is prepared into ultrathin nanosheets, nanowires, multilevel structures and the like to optimize the structure of the photocatalyst, increase the adsorption and enrichment capacity of the photocatalyst on CO2, and further improve the CO2 photocatalytic conversion efficiency and activity of the photocatalyst.
However, almost all studies to date have focused on powdered hydrotalcites (LDHs) and g-C3N4, and during the photocatalytic process, the powdered photocatalyst has problems of poor light transmittance and air permeability, complex recovery steps, and easy agglomeration, which seriously hinders the application of LDHs in the practical field. Therefore, the development of the photocatalyst which is high in efficiency and easy to recycle is of great significance to industrial and practical application.
Disclosure of Invention
Based on the technical problems in the prior art, the invention provides a preparation method of a porous carbon nitride foam/hydrotalcite three-dimensional heterojunction material and application of the porous carbon nitride foam/hydrotalcite three-dimensional heterojunction material in photocatalytic reduction of carbon dioxide.
The preparation method of the porous carbon nitride foam/hydrotalcite three-dimensional heterojunction material comprises the following steps: porous carbon nitride foam rich in g-C3N4 is used as a carrier, urea is used as a precipitator, hydrotalcite nanosheets are grown on the surface of the carrier in situ by a hydrothermal method, and the porous carbon nitride foam/hydrotalcite three-dimensional heterojunction material which is 1-4mm thick and has a g-C3N 4/hydrotalcite heterojunction structure is obtained by cutting.
The porous carbon nitride foam rich in g-C3N4 is prepared by pyrolyzing melamine sponge at high temperature.
The preparation method of the porous carbon nitride foam/hydrotalcite three-dimensional heterojunction material comprises the following specific steps: dissolving soluble divalent metal salt, soluble trivalent metal salt, urea and ammonium fluoride in water to prepare a reaction solution, wherein the molar ratio of divalent metal ions to trivalent metal ions is 2:1-3:1, immersing the porous carbon nitride foam rich in g-C3N4 in the reaction solution, carrying out closed hydrothermal reaction at the temperature of 100-120 ℃ for 8-24h, naturally cooling to room temperature after the reaction is finished, alternately washing with deionized water and ethanol, drying, and finally cutting into the porous carbon nitride foam/hydrotalcite three-dimensional heterojunction material with the thickness of 1-4 mm.
The soluble trivalent metal salt is one or more of ferric chloride, aluminum chloride, ferric nitrate and aluminum nitrate; the concentration of the trivalent metal salt in the reaction liquid is 0.007 to 0.03 mol/L.
The soluble divalent metal salt is one or more of chloride, nitrate and sulfate, and the divalent metal ions are selected from one or more of nickel ions, magnesium ions and cobalt ions; the concentration of the divalent metal salt in the reaction solution is 0.02-0.09 mol/L.
The concentration of urea in the reaction liquid is 0.1-0.3mol/L, and the concentration of ammonium fluoride is 0.05-0.25 mol/L.
The trivalent metal ions in the reaction liquid are iron ions with the concentration of 0.0214mol/L, the divalent metal ions are nickel ions with the concentration of 0.0643mol/L, the closed hydrothermal reaction is carried out for 8 hours at 120 ℃, and finally the porous carbon nitride foam/hydrotalcite three-dimensional heterojunction material with the thickness of 3mm is cut to have the best catalytic performance.
The preparation method of the porous carbon nitride foam rich in g-C3N4 comprises the following steps: heating the melamine sponge to 400-800 ℃ at the heating rate of 5-10 ℃/min in the nitrogen or argon atmosphere, roasting for 120min, naturally cooling to room temperature, alternately washing with deionized water and ethanol, and drying to obtain the g-C3N 4-rich porous carbon nitride foam.
The porous carbon nitride foam/hydrotalcite three-dimensional heterojunction material prepared by the method is applied to photocatalytic reduction of carbon dioxide.
The invention has the following beneficial effects:
1) according to the invention, the carbon nitride foam is selected as a carrier of the hydrotalcite, so that the hydrotalcite material is uniformly distributed, the dispersibility of the hydrotalcite is enhanced, and the problem that the hydrotalcite is easy to agglomerate is solved, so that more adsorption sites and active sites are exposed; the carbon nitride foam is rich in a semiconductor material g-C3N4, a heterojunction structure is constructed by the carbon nitride foam and hydrotalcite, and the obtained composite material has extremely high CO2 adsorption performance and photocatalytic performance by utilizing the photocatalytic synergistic effect of the heterojunction, wherein the CO2 adsorption capacity can reach 34.7cm3/g, the CO yield can reach 276 mu mol/g and is about 10 times of that of a pure LDHs powder material.
2) The porous carbon nitride foam/hydrotalcite three-dimensional heterojunction material with a specific thickness is prepared, and the thickness of the material is regulated and controlled, so that the CO2 adsorption performance and the photocatalytic performance of the composite material are effectively improved, and the yield of the photocatalytic CO2 reduction reaction is greatly improved. The optimum is reached when the thickness is 3mm, the composite material has the highest CO production rate of 52.17. mu. mol g-1 h-1.
3) The invention takes simple and easily obtained substances as raw materials, has simple and convenient experimental operation, short experimental period, high efficiency and low production cost, and is easy to realize scale production. The prepared composite material has good mechanical property and photocatalytic stability, good durability and easy recovery. According to the photocurrent characterization result, the composite material has extremely high photon-generated carrier separation efficiency and excellent photoelectric effect characteristics. The invention provides a new method and thought for constructing a novel and efficient CO2 material through photocatalytic conversion.
Drawings
FIG. 1(a-b) is an SEM photograph of NiFe-LDH and carbon nitride foams obtained in comparative example 1-2; (c-e) is SEM images of the porous carbon nitride foam/hydrotalcite three-dimensional heterojunction material prepared in example 3 at different magnifications; (f) is a cross-sectional SEM image of the porous carbon nitride foam/hydrotalcite three-dimensional heterojunction material prepared in example 3;
FIG. 2(a-b) are TEM images of the NiFe-LDH prepared in comparative example 1 and the porous carbon nitride foam/hydrotalcite three-dimensional heterojunction material prepared in example 3, respectively; (c) HRTEM of the porous carbon nitride foam/hydrotalcite three-dimensional heterojunction material prepared in example 3; (d-i) is a high-resolution high-angle annular dark field image and an EDSmapping graph of the porous carbon nitride foam/hydrotalcite three-dimensional heterojunction material prepared in the example 3;
FIG. 3(a-b) is an X-ray photoelectron spectrum (XPS) of Ni and Fe elements of the porous carbon nitride foam/hydrotalcite three-dimensional heterojunction material prepared in example 3 and NiFe-LDH prepared in comparative example 1;
FIG. 4(a) is a compressive stress-strain curve (strain values of 20%, 40% and 60%, respectively) of the porous carbon nitride foam/hydrotalcite three-dimensional heterojunction material prepared in example 3; (b) is a digital photo of the porous carbon nitride foam/hydrotalcite three-dimensional heterojunction material prepared in the example 3 after bending and compression treatment;
FIG. 5 is the CO2 adsorption-desorption isotherms of the porous carbon nitride foam/hydrotalcite three-dimensional heterojunction material prepared in example 3, NiFe-LDH and carbon nitride foam prepared in comparative examples 1-2;
FIG. 6 is a graph showing the photocurrent intensity test of the porous carbon nitride foam/hydrotalcite three-dimensional heterojunction materials prepared in examples 1-4 and NiFe-LDH prepared in comparative example 1;
FIG. 7 is a graph of the photocatalytic reduction CO2 performance of the porous carbon nitride foam/hydrotalcite three-dimensional heterojunction materials prepared in examples 1-4 and the NiFe-LDH and carbon nitride foams prepared in comparative examples 1-2;
fig. 8(a-b) is a graph of the performance of photocatalytic reduction CO2 of porous carbon nitride foam/hydrotalcite three-dimensional heterojunction materials with different thicknesses prepared in example 3 and (c) a digital photo.
Detailed Description
The following describes the embodiments of the present invention in further detail with reference to examples and comparative examples.
Example 1:
1) heating melamine sponge to 600 ℃ at the heating rate of 10 ℃/min in the nitrogen atmosphere, roasting for 100min, naturally cooling to room temperature, alternately washing with deionized water and ethanol, and drying to obtain the g-C3N 4-enriched porous carbon nitride foam. As shown in fig. 1b, the porous carbon nitride foam exhibits a smooth three-dimensional network structure with large pores of several tens to several hundreds of micrometers.
2) 0.202g (0.5mmol) of Fe (NO3) 3.9H 2O, 0.436g (1.5mmol) of Ni (NO3) 2.6H 2O, 1.201g (20mmol) of CO (NH2)2 and 0.370g (10mmol) of NH4F are weighed out and dissolved in 70mL of deionized water, and stirred to form a uniform reaction solution. Transferring the porous carbon nitride foam/hydrotalcite three-dimensional heterojunction material into a 100mL stainless steel reaction kettle with a polytetrafluoroethylene lining, immersing the porous carbon nitride foam (3 multiplied by 2cm3) treated in the step 1) into the reaction solution, carrying out ultrasonic treatment for 30min, sealing, putting the reaction solution into a 120 ℃ oven for hydrothermal treatment for 8h, naturally cooling to room temperature after the reaction is finished, taking out the reaction solution, respectively cleaning 3 times by using deionized water and absolute ethyl alcohol to remove impurities adsorbed on the surface of the composite material, drying the reaction solution in the oven at 60 ℃, and finally cutting the reaction solution into slices (the size is 3 multiplied by 2 multiplied by 0.5cm3) to obtain the porous carbon nitride foam/hydrotalcite three-dimensional heterojunction material with the thickness of 5mm, which is abbreviated as NCF-1.
NCF-1 was placed in the bottom of a 200mL quartz reactor and purged with high purity CO2 for 1.5h prior to reaction. And introducing CO2, and carrying out dark state adsorption-desorption equilibrium for 1 h. A300W xenon lamp is used as a light source for photocatalytic reaction, the light is irradiated for 5h, and the reaction product is quantitatively analyzed by using gas chromatography (Agilent 7890B). As shown in FIG. 7, the CO production rate of the NCF-1 composite was 11.6. mu. mol g-1 h-1.
Example 2:
1) the same as example 1;
2) 0.404g (1mmol) of Fe (NO3) 3.9H 2O, 0.872g (3mmol) of Ni (NO3) 2.6H 2O, 1.201g (20mmol) of CO (NH2)2 and 0.370g (10mmol) of NH4F are weighed out and dissolved in 70mL of deionized water, and stirred to form a uniform reaction solution. Transferring the porous carbon nitride foam/hydrotalcite three-dimensional heterojunction material into a 100mL stainless steel reaction kettle with a polytetrafluoroethylene lining, immersing the porous carbon nitride foam (3 multiplied by 2cm3) treated in the step 1) into the reaction solution, carrying out ultrasonic treatment for 30min, sealing, putting the reaction solution into a 120 ℃ oven for hydrothermal treatment for 8h, naturally cooling to room temperature after the reaction is finished, taking out the reaction solution, respectively cleaning for 3 times by using deionized water and absolute ethyl alcohol to remove impurities adsorbed on the surface of the composite material, drying the reaction solution in the oven at 60 ℃, and finally cutting the reaction solution into slices (with the size of 3 multiplied by 2 multiplied by 0.5cm3) to obtain the porous carbon nitride foam/hydrotalcite three-dimensional heterojunction material with the thickness of 5mm, which is abbreviated as NCF-2.
NCF-2 was placed in the bottom of a 200mL quartz reactor and purged with high purity CO2 for 1.5h prior to reaction. Sufficient CO2 is introduced, and the dark state adsorption-desorption is balanced for 1 h. A300W xenon lamp is used as a light source for photocatalytic reaction, the light is irradiated for 5h, and the reaction product is quantitatively analyzed by using gas chromatography (Agilent 7890B). As shown in FIG. 7, the CO production rate of the NCF-2 composite was 35.7. mu. mol g-1 h-1.
Example 3:
1) the same as example 1;
2) 0.606g (1.5mmol) of Fe (NO3) 3.9H 2O, 1.309g (4.5mmol) of Ni (NO3) 2.6H 2O, 1.201g (20mmol) of CO (NH2)2 and 0.370g (10mmol) of NH4F are weighed out and dissolved in 70mL of deionized water and stirred to form a uniform reaction solution. Transferring the porous carbon nitride foam into a 100mL stainless steel reaction kettle with a polytetrafluoroethylene lining, immersing the porous carbon nitride foam (3 multiplied by 2cm3) treated in the step 1) into the reaction solution, carrying out ultrasonic treatment for 30min, sealing, placing in a 120 ℃ oven for hydrothermal treatment for 8h, naturally cooling to room temperature after the reaction is finished, taking out, respectively cleaning 3 times by using deionized water and absolute ethyl alcohol to remove impurities adsorbed on the surface of the composite material, drying in the oven at 60 ℃, and finally cutting into sheets of 3 multiplied by 2 multiplied by 0.1cm3, 3 multiplied by 2 multiplied by 0.2cm3, 3 multiplied by 2 multiplied by 0.3cm3, 3 multiplied by 2 by 0.4cm3 and 3 multiplied by 2 multiplied by 0.5cm3 respectively to obtain the porous carbon nitride foam/hydrotalcite three-dimensional heterojunction material with the thickness of 1, 2, 3, 4 and 5mm respectively, which is abbreviated as NCF-3-1, NCF-3, NCF-2, NCF-3-3 and NCF-4, NCF-3-5.
And (3) performing characterization test on the prepared composite material: as shown in fig. 1c, the carbon nitride foam surface was uniformly covered with NiFe-LDH nanosheets. The magnified SEM image is shown in FIG. 1e, where the NiFe-LDH nanosheets are nearly perpendicular to the surface of the carbon nitride foam skeleton, and the thickness of the NiFe-LDH layer is about 0.84 μm. As shown in FIG. 2C, the HRTEM graph shows that there is a distinct interface between NiFe-LDH and g-C3N4 in the NiFe-LDH/CF sample, indicating the formation of a heterojunction in NiFe-LDH/g-C3N 4. In addition, HRTEM image also shows that the lattice spacings corresponding to the (002) crystal plane of g-C3N4 and the (015) crystal plane of NiFe-LDH are 0.325nm and 0.23nm respectively. In addition, EDS mapping images (FIG. 2d-i) show that the composite material is composed of Ni, Fe, C, N and O elements, and the component elements are uniformly distributed, further confirming that a heterojunction is successfully constructed between NiFe-LDH and g-C3N 4. The adsorption amount of CO2 of the composite material was 34.7cm3g-1 (FIG. 5), and the highest photocurrent efficiency was obtained (FIG. 6).
In FIG. 3a, Ni 2p of NiFe-LDH was split into two peaks, Ni 2p3/2 and Ni 2p1/2 of Ni2+, with peaks at 855.7eV and 873.4eV binding energies, respectively. And compared with pure NiFe-LDH, the position of the Ni 2p peak of the composite material is shifted to the position with low binding energy by 0.2 eV. This phenomenon also appears in the Fe 2p spectrum (fig. 3b), and the position of the Fe 2p peak of the sample after recombination shifts to a position where the binding energy is low compared to the single NiFe-LDH. The reduction of the binding energy of Ni 2p and Fe 2p indicates that stronger electron transfer exists between g-C3N4 and NiFe-LDH, and further illustrates the formation of a heterojunction between g-C3N4 and NiFe-LDH.
NCF-3-5 was placed in the bottom of a 200mL quartz reactor and purged with high purity CO2 for 1.5h prior to reaction. Sufficient CO2 is introduced, and the dark state adsorption-desorption is balanced for 1 h. A300W xenon lamp is used as a light source for photocatalytic reaction, the light is irradiated for 5h, and the reaction product is quantitatively analyzed by using gas chromatography (Agilent 7890B). As shown in FIG. 7, the NCF-3-5 composite had the highest CO production rate of 55.2. mu. mol g-1 h-1.
NCF-3-1, NCF-3-2, NCF-3-3, NCF-3-4 and NCF-3-5 were placed in the bottom of a 200mL quartz reactor, respectively, and purged with high purity CO2 for 1.5h before reaction. Sufficient CO2 is introduced, and the dark state adsorption-desorption is balanced for 1 h. A300W xenon lamp is used as a light source for photocatalytic reaction for illumination for 3h, and the reaction product is quantitatively analyzed by using gas chromatography (Agilent 7890B). As shown in fig. 8a, the yields of CO generated after the composite materials with different thicknesses are irradiated for 3h are different, and as can be seen from comparison of the yields of CO, when the thickness is smaller, the photocatalyst loading is lower, and the CO yield is lower, because the composite material has better light transmittance and air permeability, the photocatalyst loading is obviously increased and the CO yield is obviously increased with the increase of the thickness. However, when the thickness reaches 4mm, the light transmittance reaches the maximum, so that the yield of CO begins to stabilize and is not obviously increased, namely, the maximum light transmittance thickness of the composite material is 4 mm. Therefore, as shown in fig. 8b, as the thickness of the composite material increases, the CO generation rate increases first and then decreases. The NCF-3-3 composite had the highest CO production rate at a thickness of 3mm, 52.17. mu. mol g-1 h-1.
Example 4:
1) the same as example 1;
2) 0.808g (2mmol) of Fe (NO3) 3.9H 2O, 1.745g (6mmol) of Ni (NO3) 2.6H 2O, 1.201g (20mmol) of CO (NH2)2 and 0.370g (10mmol) of NH4F are weighed out and dissolved in 70mL of deionized water, and stirred to form a uniform reaction solution. Transferring the porous carbon nitride foam/hydrotalcite three-dimensional heterojunction material into a 100mL stainless steel reaction kettle with a polytetrafluoroethylene lining, immersing the porous carbon nitride foam (3 multiplied by 2cm3) treated in the step 1) into the reaction solution, carrying out ultrasonic treatment for 30min, sealing, putting the reaction solution into a 120 ℃ oven for hydrothermal treatment for 8h, naturally cooling to room temperature after the reaction is finished, taking out the reaction solution, respectively cleaning for 3 times by using deionized water and absolute ethyl alcohol to remove impurities adsorbed on the surface of the composite material, drying the reaction solution in the oven at 60 ℃, and finally cutting the reaction solution into slices (with the size of 3 multiplied by 2 multiplied by 0.5cm3) to obtain the porous carbon nitride foam/hydrotalcite three-dimensional heterojunction material with the thickness of 5mm, which is abbreviated as NCF-4.
NCF-4 was placed in the bottom of a 200mL quartz reactor and purged with high purity CO2 for 1.5h prior to reaction. Sufficient CO2 is introduced, and the dark state adsorption-desorption is balanced for 1 h. A300W xenon lamp is used as a light source for photocatalytic reaction, the light is irradiated for 5h, and the reaction product is quantitatively analyzed by using gas chromatography (Agilent 7890B). As shown in FIG. 7, the CO production rate of the NCF-4 composite was 14.2. mu. mol g-1 h-1.
Comparative example 1:
0.404g (1mmol) of Fe (NO3) 3.9H 2O, 0.872g (3mmol) of Ni (NO3) 2.6H 2O, 1.201g (20mmol) of CO (NH2)2 and 0.370g (10mmol) of NH4F are weighed out and dissolved in 70mL of deionized water and sonicated for 30min to form a homogeneous solution. Transferring the mixture into a stainless steel reaction kettle with a 100mL polytetrafluoroethylene lining, sealing, placing the reaction kettle in a 120 ℃ oven for hydrothermal treatment for 8h, and naturally cooling to room temperature after the reaction is finished. And (3) alternately washing the precipitate with deionized water and ethanol to be neutral, and drying in an oven at 60 ℃ to obtain the NiFe-LDH. As shown in FIG. 1a, NiFe-LDH is a three-dimensional flower-like structure composed of sheets with an average diameter of about 5 μm.
A20 mgNiFe-LDH powder sample is uniformly dispersed to the bottom of a 200mL quartz reactor, and the reactor is purged for 1.5h by high-purity CO2 before reaction. Sufficient CO2 is introduced, and the dark state adsorption-desorption is balanced for 1 h. A300W xenon lamp is used as a light source for photocatalytic reaction, the light is irradiated for 5h, and the reaction product is quantitatively analyzed by using gas chromatography (Agilent 7890B). As shown in FIG. 7, the production rate of CO for the NiFe-LDH material was 5.54. mu. mol g-1 h-1.
Comparative example 2:
the carbon nitride foam obtained in step 1) of example 1 was cut into thin pieces (dimensions 3X 2X 0.5cm3), i.e.5 mm thick, placed in the bottom of a 200mL quartz reactor and purged with high purity CO2 for 1.5h before reaction. Sufficient CO2 is introduced, and the dark state adsorption-desorption is balanced for 1 h. A300W xenon lamp is used as a light source for photocatalytic reaction, the light is irradiated for 5h, and the reaction product is quantitatively analyzed by using gas chromatography (Agilent 7890B). As shown in FIG. 7, the CO production rate of the carbon nitride foam was 9.02. mu. mol g-1 h-1.
The present invention has been disclosed in terms of the preferred embodiment, but it is not intended to be limited to the embodiment, and all technical solutions obtained by substituting or converting the equivalent embodiments fall within the scope of the present invention.
Claims (9)
1. A preparation method of a porous carbon nitride foam/hydrotalcite three-dimensional heterojunction material is characterized by comprising the following steps: to be rich in g-C3N4The porous carbon nitride foam is used as a carrier, urea is used as a precipitator, hydrotalcite nano-sheets are grown on the surface of the carrier in situ by adopting a hydrothermal method, and the porous carbon nitride foam is cut to obtain the nano-hydrotalcite nano-sheets with the thickness of 1-4mm and g-C3N4Porous carbon nitride foam with a hydrotalcite heterojunction structure/a hydrotalcite three-dimensional heterojunction material.
2. The method of claim 1, wherein the g-C-rich fraction is enriched in3N4The porous carbon nitride foam is obtained by pyrolyzing melamine sponge at high temperature.
3. The preparation method according to claim 1, comprising the following steps: dissolving soluble divalent metal salt, soluble trivalent metal salt, urea and ammonium fluoride in water to prepare reaction liquid,wherein the molar ratio of divalent metal ions to trivalent metal ions is 2:1-3:1, and the enriched fraction will be rich in g-C3N4The porous carbon nitride foam is immersed in the reaction solution, then the hydrothermal reaction is carried out for 8-24h in a closed environment at the temperature of 100-120 ℃, the reaction is naturally cooled to room temperature after the completion of the reaction, deionized water and ethanol are alternately washed, dried and finally cut into the porous carbon nitride foam/hydrotalcite three-dimensional heterojunction material with the thickness of 1-4 mm.
4. The preparation method according to claim 3, wherein the soluble trivalent metal salt is one or more of ferric chloride, aluminum chloride, ferric nitrate and aluminum nitrate; the concentration of the trivalent metal salt in the reaction liquid is 0.007 to 0.03 mol/L.
5. The preparation method according to claim 3, wherein the soluble divalent metal salt is one or more of chloride, nitrate and sulfate, and the divalent metal ion is one or more of nickel ion, magnesium ion and cobalt ion; the concentration of the divalent metal salt in the reaction solution is 0.02-0.09 mol/L.
6. The process according to claim 3, wherein the concentration of urea in the reaction solution is 0.1 to 0.3mol/L and the concentration of ammonium fluoride is 0.05 to 0.25 mol/L.
7. The preparation method according to claim 3, wherein the trivalent metal ion in the reaction solution is iron ion with a concentration of 0.0214mol/L, the divalent metal ion is nickel ion with a concentration of 0.0643mol/L, the reaction solution is subjected to closed hydrothermal reaction at 120 ℃ for 8h, and finally the reaction solution is cut into a 3mm porous carbon nitride foam/hydrotalcite three-dimensional heterojunction material.
8. The method of claim 3, wherein the g-C-rich fraction is enriched in3N4The preparation method of the porous carbon nitride foam comprises the following steps: heating the melamine sponge to 400-800 ℃ at the heating rate of 5-10 ℃/min in the nitrogen or argon atmosphere, roasting for 120min, and naturally coolingCooling to room temperature, alternately washing with deionized water and ethanol, and drying to obtain the product rich in g-C3N4Porous carbon nitride foam.
9. Use of the porous carbon nitride foam/hydrotalcite three-dimensional heterojunction material prepared by the method according to any one of claims 1 to 8 for photocatalytic reduction of carbon dioxide.
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