CN114392763A - Preparation method of quadrangular tubular CN/NiS composite photocatalyst - Google Patents
Preparation method of quadrangular tubular CN/NiS composite photocatalyst Download PDFInfo
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- CN114392763A CN114392763A CN202210110710.4A CN202210110710A CN114392763A CN 114392763 A CN114392763 A CN 114392763A CN 202210110710 A CN202210110710 A CN 202210110710A CN 114392763 A CN114392763 A CN 114392763A
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 42
- 239000002131 composite material Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 18
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims abstract description 18
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229940078494 nickel acetate Drugs 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000001816 cooling Methods 0.000 claims abstract description 9
- 239000011780 sodium chloride Substances 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 7
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 5
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 5
- 238000000227 grinding Methods 0.000 claims abstract description 5
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000004570 mortar (masonry) Substances 0.000 claims abstract description 5
- 239000010453 quartz Substances 0.000 claims abstract description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims description 14
- -1 polytetrafluoroethylene Polymers 0.000 claims description 11
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 11
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 11
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000000919 ceramic Substances 0.000 claims description 8
- 238000005303 weighing Methods 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 238000009210 therapy by ultrasound Methods 0.000 claims 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 14
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 14
- 239000001257 hydrogen Substances 0.000 abstract description 14
- 238000004519 manufacturing process Methods 0.000 abstract description 13
- 239000003054 catalyst Substances 0.000 abstract description 5
- 240000004282 Grewia occidentalis Species 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 3
- 239000000376 reactant Substances 0.000 abstract description 3
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 abstract 2
- 238000005245 sintering Methods 0.000 abstract 1
- 238000002474 experimental method Methods 0.000 description 13
- 230000001699 photocatalysis Effects 0.000 description 8
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 5
- 239000004567 concrete Substances 0.000 description 3
- 229910000510 noble metal Inorganic materials 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000004627 transmission electron microscopy Methods 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
-
- B01J35/39—
-
- B01J35/613—
-
- 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
- B01J37/20—Sulfiding
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
- C01B3/042—Decomposition of water
Abstract
A preparation method of a quadrangular tubular CN/NiS composite photocatalyst relates to a preparation method of a photocatalyst, and belongs to the field of photocatalyst preparation. The invention aims to solve the problem of g-C3N4The method has the technical problem of low hydrogen production efficiency due to the problems, and comprises the following steps: firstly, placing NaCl, LiCl and KCl in a quartz mortar, adding melamine, grinding and sintering to obtain a quadrangular tubular C3N4(ii) a Two, taking the four-corner tube shape C3N4Ultrasonically treating, dripping nickel acetate solution, dripping thiourea solution, keeping at 150 deg.C for 4 hr, naturally cooling to room temperature, washing, and drying. The invention is realized by the pair g-C3N4Perform excellent appearance, structure and sizeThe specific surface area is increased; the contact degree of the catalyst and reactant molecules is improved by increasing the number of the surface active sites, so that the mass transfer efficiency is improved, and higher reaction activity is achieved. The specific surface area of the quadrangular tubular CN/NiS composite photocatalyst can reach 53.18m2The hydrogen production efficiency can reach 122 umol/g/h.
Description
Technical Field
The invention relates to a preparation method of a photocatalyst, belonging to the field of preparation of photocatalysts.
Background
g-C3N4As a non-metal semiconductor, it is one of the most potential semiconductor photocatalytic materials by virtue of an adjustable band gap structure and excellent light absorption performance. Albeit g-C3N4Has wide application in the field of photocatalysis, but g-C3N4The photocatalytic performance of the hydrogen is restricted by the problems of the hydrogen production system, so that the hydrogen production efficiency is low.
The auxiliary agent modification is an effective way for realizing effective separation of a photon-generated carrier so as to improve the photocatalytic activity. It is known that the noble metal Pt can be used as a reaction site for photocatalytic hydrogen production, but the high cost limits the practical application of the noble metal Pt. Therefore, it is necessary to develop a non-noble metal assistant with high efficiency.
Disclosure of Invention
The invention aims to solve the problem of g-C3N4The problem of the catalyst per se, which causes the technical problem of low hydrogen production efficiency, provides a preparation method of a four-corner tubular CN/NiS composite photocatalyst.
The preparation method of the quadrangular tubular CN/NiS composite photocatalyst comprises the following steps:
firstly, respectively weighing 5g of NaCl, 5g of LiCl and 5g of KCl, placing the NaCl, the LiCl and the KCl in a quartz mortar, adding 1.0g of melamine, grinding to a powder state, transferring the mixture to a ceramic crucible, then placing the ceramic crucible in a muffle furnace to heat to 450 ℃ at a heating rate of 1 ℃/min, keeping the temperature for 5 hours, naturally cooling to room temperature after the reaction is finished, and finally obtaining a yellow solid, namely a quadrangular tubular C3N4;
Secondly, taking 0.1g of quadrangular tubular C3N4Placing in 10mL deionized water, ultrasonic treating for 5min, and dripping 2-9mL nickel acetate (Ni (CH) with concentration of 0.05 mol/L)3COOH)2) Stirring the solution for 1h, dripping 10mL of thiourea solution with the concentration of 100g/L, transferring the mixture into polytetrafluoroethylene, placing the polytetrafluoroethylene in an oven, keeping the temperature at 150 ℃ for 4h, naturally cooling to room temperature, washing the polytetrafluoroethylene with deionized water and ethanol for three times respectively, and drying the cooled mixture at 50 ℃ for 12h to obtain the quadrangular tubular CN/NiS composite photocatalyst.
Weighing 50mg of quadrangular tubular CN/NiS composite photocatalyst, adding the quadrangular tubular CN/NiS composite photocatalyst into 40mL of deionized water, adding 10mL of methanol, then carrying out a photocatalytic hydrogen production experiment under visible light, and calculating the hydrogen production efficiency to reach 122 umol/g/h.
The invention is realized by the pair g-C3N4Optimizing the appearance, structure and size to increase the specific surface area; the contact degree of the catalyst and reactant molecules is improved by increasing the number of the surface active sites, so that the mass transfer efficiency is improved, and higher reaction activity is achieved. The method is simple and easy to implement, high in repeatability, safe and green, and the unique liquid phase reaction environment of the method is beneficial to reducing the restriction of the kinetic conditions of the reaction and promoting the diffusion of reactants and the mutual reaction. Has the advantages of low synthesis temperature, short reaction time, high purity of synthesized powder and small particle size.
NiS can be used as g-C3N4The hydrogen production active site is used for improving the photocatalytic hydrogen production performance. The specific surface area of the quadrangular tubular CN/NiS composite photocatalyst can reach 53.18m2The hydrogen production efficiency can reach 122 umol/g/h.
Drawings
FIG. 1 is an XPS plot of C in CN/NiS composite photocatalyst (CN/NiS-0.5 wt%) in experiment one;
FIG. 2 is an XPS plot of N in CN/NiS composite photocatalyst (CN/NiS-0.5 wt%) in experiment one;
FIG. 3 is an XPS plot of Ni in CN/NiS composite photocatalyst (CN/NiS-0.5 wt%) in experiment one;
FIG. 4 is an XPS plot of S in CN/NiS composite photocatalyst (CN/NiS-0.5 wt%) in experiment one;
FIG. 5 is a BET plot of the CN/NiS composite photocatalyst in experiment one;
FIG. 6 shows the square tube shape C obtained in the first step of the first experiment3N4Transmission electron microscopy images of;
FIG. 7 is a transmission electron microscope image of the CN/NiS composite photocatalyst in the first experiment;
FIG. 8 shows a CN/NiS composite photocatalyst and catalyst C in experiment I3N4(iii) a photocurrent profile of NiS;
FIG. 9 is a CN/NiS composite photocatalyst in experiment ICatalyst and catalyst C3N4Impedance profile of NiS.
Detailed Description
The technical solution of the present invention is not limited to the following specific embodiments, but includes any combination of the specific embodiments.
The first embodiment is as follows: the preparation method of the quadrangular tubular CN/NiS composite photocatalyst comprises the following steps:
firstly, respectively weighing 5g of NaCl, 5g of LiCl and 5g of KCl, placing the NaCl, the LiCl and the KCl in a quartz mortar, adding 1.0g of melamine, grinding to a powder state, transferring the mixture to a ceramic crucible, then placing the ceramic crucible in a muffle furnace to heat to 450 ℃ at a heating rate of 1 ℃/min, keeping the temperature for 5 hours, naturally cooling to room temperature after the reaction is finished, and finally obtaining a yellow solid, namely a quadrangular tubular C3N4;
Secondly, taking 0.1g of quadrangular tubular C3N4Placing in 10mL deionized water, ultrasonic treating for 5min, and dripping 2-9mL nickel acetate (Ni (CH) with concentration of 0.05 mol/L)3COOH)2) Stirring the solution for 1h, dripping 10mL of thiourea solution with the concentration of 100g/L, transferring the mixture into polytetrafluoroethylene, placing the polytetrafluoroethylene in an oven, keeping the temperature at 150 ℃ for 4h, naturally cooling to room temperature, washing the polytetrafluoroethylene with deionized water and ethanol for three times respectively, and drying the cooled mixture at 50 ℃ for 12h to obtain the quadrangular tubular CN/NiS composite photocatalyst.
The second embodiment is as follows: the difference between the present embodiment and the first embodiment is that 2mL of nickel acetate solution with a concentration of 0.05mol/L is added dropwise in the second step. The rest is the same as the first embodiment.
The third concrete implementation mode: the difference between this embodiment and the first or second embodiment is that 3mL of nickel acetate solution with a concentration of 0.05mol/L is added dropwise in the second step. The others are the same as in the first or second embodiment.
The fourth concrete implementation mode: the difference between this embodiment and one of the first to third embodiments is that 7mL of nickel acetate solution with a concentration of 0.05mol/L is added dropwise in the second step. The rest is the same as one of the first to third embodiments.
The fifth concrete implementation mode: the difference between this embodiment and one of the first to fourth embodiments is that 9mL of nickel acetate solution with a concentration of 0.05mol/L is added dropwise in the second step. The rest is the same as one of the first to fourth embodiments.
The following experiments are adopted to verify the effect of the invention:
experiment one:
the preparation method of the quadrangular tubular CN/NiS composite photocatalyst comprises the following steps:
firstly, respectively weighing 5g of NaCl, 5g of LiCl and 5g of KCl, placing the NaCl, the LiCl and the KCl in a quartz mortar, adding 1.0g of melamine, grinding to a powder state, transferring the mixture to a ceramic crucible, then placing the ceramic crucible in a muffle furnace to heat to 450 ℃ at a heating rate of 1 ℃/min, keeping the temperature for 5 hours, naturally cooling to room temperature after the reaction is finished, and finally obtaining a yellow solid, namely a quadrangular tubular C3N4;
Secondly, taking 0.1g of quadrangular tubular C3N4Placing in 10mL deionized water, ultrasonic treating for 5min, and adding 2mL nickel acetate (Ni (CH) with concentration of 0.05mol/L3COOH)2) Stirring the solution for 1h, dripping 10mL of thiourea solution with the concentration of 100g/L, transferring the mixture into polytetrafluoroethylene, placing the polytetrafluoroethylene in an oven, keeping the temperature at 150 ℃ for 4h, naturally cooling to room temperature, washing the polytetrafluoroethylene with deionized water and ethanol for three times respectively, and drying the mixture at 50 ℃ for 12h to obtain the quadrangular tubular CN/NiS composite photocatalyst (CN/NiS-0.5 wt%).
As can be seen from FIGS. 1-4, the composite photocatalyst contains four elements, namely C, N, Ni and S, which indicates that CN and NiS have been successfully compounded.
FIG. 5 shows that the specific surface area of the quadrangular tubular CN/NiS composite photocatalyst reaches 53.18m2/g。
FIG. 8 shows that the photocurrent of the tetragonal tubular CN/NiS composite photocatalyst is much greater than that of the single C3N4And a NiS photocatalyst.
FIG. 9 shows that the impedance of the four-corner tubular CN/NiS composite photocatalyst is much smaller than that of a single C3N4And a NiS photocatalyst, which shows that the photocurrent of the four-corner tubular CN/NiS composite photocatalyst is larger than that of the single C3N4And a NiS photocatalyst.
Weighing 50mg of quadrangular tubular CN/NiS composite photocatalyst (CN/NiS-0.5 wt%) and adding the quadrangular tubular CN/NiS composite photocatalyst into 40mL of deionized water, then adding 10mL of methanol, then carrying out a photocatalytic hydrogen production experiment under visible light, and calculating the hydrogen production efficiency to reach 122 umol/g/h.
Claims (5)
1. The preparation method of the quadrangular tubular CN/NiS composite photocatalyst is characterized by comprising the following steps of:
firstly, respectively weighing 5g of NaCl, 5g of LiCl and 5g of KCl, placing the NaCl, the LiCl and the KCl in a quartz mortar, adding 1.0g of melamine, grinding to a powder state, transferring the mixture to a ceramic crucible, then placing the ceramic crucible in a muffle furnace to heat to 450 ℃ at a heating rate of 1 ℃/min, keeping the temperature for 5 hours, naturally cooling to room temperature after the reaction is finished, and finally obtaining a yellow solid, namely a quadrangular tubular C3N4;
Secondly, taking 0.1g of quadrangular tubular C3N4Placing the mixture in 10mL of deionized water for 5min by ultrasonic treatment, then dripping 2-9mL of nickel acetate solution with the concentration of 0.05mol/L, stirring for 1h, dripping 10mL of thiourea solution with the concentration of 100g/L, transferring the mixture into polytetrafluoroethylene, placing the polytetrafluoroethylene in an oven, keeping the temperature at 150 ℃ for 4h, naturally cooling to room temperature, washing the mixture with the deionized water and ethanol for three times respectively, and drying the mixture at 50 ℃ for 12h to obtain the quadrangular tubular CN/NiS composite photocatalyst.
2. The method for preparing the quadrangular tube-shaped CN/NiS composite photocatalyst according to claim 1, wherein 2mL of nickel acetate solution with the concentration of 0.05mol/L is dropped in the step two.
3. The method for preparing the quadrangular tube-shaped CN/NiS composite photocatalyst according to claim 1, wherein 3mL of nickel acetate solution with the concentration of 0.05mol/L is dropped in the step two.
4. The method for preparing the quadrangular tube-shaped CN/NiS composite photocatalyst according to claim 1, wherein 7mL of nickel acetate solution with the concentration of 0.05mol/L is dropped in the step two.
5. The method for preparing the quadrangular tube-shaped CN/NiS composite photocatalyst according to claim 1, wherein 9mL of nickel acetate solution with the concentration of 0.05mol/L is dropped in the step two.
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CN102992282A (en) * | 2012-11-08 | 2013-03-27 | 南京大学 | Mesoporous C3N4 photocatalytic material prepared by using molten salt method and application thereof in photocatalysis field |
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CN109603875A (en) * | 2018-12-14 | 2019-04-12 | 深圳大学 | Carbon nitride material and its preparation method and application |
CN113578370A (en) * | 2021-09-07 | 2021-11-02 | 东北大学 | Preparation method of tubular carbon nitride photocatalyst loaded by carbon material |
CN113731394A (en) * | 2021-09-30 | 2021-12-03 | 贵州大学 | Preparation method of cerium dioxide-carbon nitride composite material with high photocatalytic performance |
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- 2022-01-29 CN CN202210110710.4A patent/CN114392763A/en active Pending
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