CN111715266A - LiCl-CN nanotube with visible light catalytic activity and preparation method and application thereof - Google Patents
LiCl-CN nanotube with visible light catalytic activity and preparation method and application thereof Download PDFInfo
- Publication number
- CN111715266A CN111715266A CN202010701668.4A CN202010701668A CN111715266A CN 111715266 A CN111715266 A CN 111715266A CN 202010701668 A CN202010701668 A CN 202010701668A CN 111715266 A CN111715266 A CN 111715266A
- Authority
- CN
- China
- Prior art keywords
- chloride
- licl
- visible light
- catalytic activity
- lithium salt
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000002071 nanotube Substances 0.000 title claims abstract description 39
- 230000003197 catalytic effect Effects 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 229910003002 lithium salt Inorganic materials 0.000 claims abstract description 27
- 159000000002 lithium salts Chemical class 0.000 claims abstract description 27
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims abstract description 25
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 18
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 239000000376 reactant Substances 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims abstract description 3
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 14
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims description 12
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 8
- 230000015556 catabolic process Effects 0.000 claims description 8
- 238000006731 degradation reaction Methods 0.000 claims description 8
- 230000001699 photocatalysis Effects 0.000 claims description 7
- MZRVEZGGRBJDDB-UHFFFAOYSA-N N-Butyllithium Chemical compound [Li]CCCC MZRVEZGGRBJDDB-UHFFFAOYSA-N 0.000 claims description 6
- 239000002351 wastewater Substances 0.000 claims description 5
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 4
- 239000001103 potassium chloride Substances 0.000 claims description 4
- 235000011164 potassium chloride Nutrition 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 3
- ZRXHLJNBNWVNIM-UHFFFAOYSA-N 3-methyl-1-benzofuran Chemical compound C1=CC=C2C(C)=COC2=C1 ZRXHLJNBNWVNIM-UHFFFAOYSA-N 0.000 claims description 2
- 235000019270 ammonium chloride Nutrition 0.000 claims description 2
- 239000011780 sodium chloride Substances 0.000 claims description 2
- 235000002639 sodium chloride Nutrition 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 6
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 abstract description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 5
- 229910002804 graphite Inorganic materials 0.000 abstract description 4
- 239000010439 graphite Substances 0.000 abstract description 4
- 239000003054 catalyst Substances 0.000 description 7
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 239000011941 photocatalyst Substances 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000013329 compounding Methods 0.000 description 2
- 238000003795 desorption Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000003517 fume Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- RCFXJKASZOGZLY-UHFFFAOYSA-N 3,4,5-trichloro-2h-oxazine Chemical compound ClC1=C(Cl)C(Cl)=CON1 RCFXJKASZOGZLY-UHFFFAOYSA-N 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910017852 NH2NH2 Inorganic materials 0.000 description 1
- OUUQCZGPVNCOIJ-UHFFFAOYSA-M Superoxide Chemical compound [O-][O] OUUQCZGPVNCOIJ-UHFFFAOYSA-M 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 150000001721 carbon Chemical class 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- MGNCLNQXLYJVJD-UHFFFAOYSA-N cyanuric chloride Chemical compound ClC1=NC(Cl)=NC(Cl)=N1 MGNCLNQXLYJVJD-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 229910001882 dioxygen Inorganic materials 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- VLKZOEOYAKHREP-UHFFFAOYSA-N hexane Substances CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- XIXADJRWDQXREU-UHFFFAOYSA-M lithium acetate Chemical compound [Li+].CC([O-])=O XIXADJRWDQXREU-UHFFFAOYSA-M 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000003032 molecular docking Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000005580 one pot reaction Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 230000015843 photosynthesis, light reaction Effects 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000004729 solvothermal method Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- BHZCMUVGYXEBMY-UHFFFAOYSA-N trilithium;azanide Chemical compound [Li+].[Li+].[Li+].[NH2-] BHZCMUVGYXEBMY-UHFFFAOYSA-N 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
Images
Classifications
-
- 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—
-
- 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
- C02F2101/34—Organic compounds containing oxygen
- C02F2101/345—Phenols
-
- 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
Abstract
The invention discloses a preparation method of LiCl-CN nano tubes with visible light catalytic activity, which comprises the following steps: (1) uniformly mixing chloride, lithium salt and melamine, placing the mixture in a crucible, and covering the crucible with a cover; (2) heating the crucible containing the reactants in the step (1), raising the temperature to 500-600 ℃ at the speed of 3-8 ℃/min, then preserving the heat for 3-5h, and cooling to 20-25 ℃; (3) adding chloride and lithium salt into the crucible in the step (2), raising the temperature to 500-; cooling to 20-25 deg.C, and drying. Compared with a graphite carbon nitride material, the LiCl-CN nano tube has the advantages of larger specific surface area and photocurrent density, smaller electrochemical resistance, better dispersibility and higher efficient visible light catalytic activity.
Description
Technical Field
The invention relates to the field of photocatalysts, in particular to a LiCl-CN nanotube with visible light catalytic activity and a preparation method and application thereof.
Background
The catalysts currently used in the field of photocatalysis mainly include metal oxide catalysts and non-oxide catalysts, among which the novel non-oxide photocatalyst graphite carbon nitride (g-C)3N4) With conventional metal oxide catalyst TiO2Compared with the prior art, the method has the following advantages: (1) the semiconductor strip edge position is very suitable, and the thermodynamic requirements of hydrogen production and oxygen production by photolysis of water are met; (2) the absorption spectrum range is wider, and the photocatalysis effect can be realized only under common visible light; (3) can effectively activate molecular oxygen to generate superoxide radical, and is more beneficial to the photocatalytic conversion of organic functional groups and the photocatalytic degradation of organic pollutants.
But g-C3N4The composite rate of photo-generated electrons and holes is high, although the composite probability can be effectively reduced by adopting methods such as ion doping or semiconductor compounding, the invention patent CN201310457642.X adopts active carbon and trichloro-oxazine (C)3N3C13) Lithium nitride (Li)3N) and the like as main raw materials, in a benzene solvent, by the processes of heating, pressurizing and the like, a Li-supported g-C is prepared3N4Activated carbon with photocatalytic function. The compounding probability is poor because pressurization and the use of benzene solvent are required, and special requirements are required on production equipment and organic reagents.
At present, the catalyst morphology is changed or K is doped+、NH4 +Al, Fe, Ni, V, W and other species are used for increasing O vacancy, and the degradation efficiency is improved by changing a carrier or changing a channel structure. In the prior literature for the synthesis of LiCl-CN nanotubes: synthetic effect of Li docking and Ag deployment for enhanced visual light catalytic performance of g-C3N4And a facility of photocatalytic efficacy of g-C3N4The by Li-interaction adopts a solvothermal method and a light deposition method to prepare the lithium-doped graphite carbon nitride photocatalyst, and mainly adopts melamine, cyanuric chloride, lithium acetate or n-butyllithium and the like as raw materials and NH2NH2、Et3N, N-hexane and the like are used as solvents and are crystallized and synthesized at a certain temperature. Has the disadvantages that a two-step method is needed, and the volatile organic solvent is used to cause harm to the environmentInert gas shielding is needed, which results in energy consumption.
Disclosure of Invention
Based on the above, the invention aims to overcome the defects of the prior art and provide a preparation method of LiCl-CN nanotubes with visible light catalytic activity.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: a preparation method of LiCl-CN nanotubes with visible light catalytic activity comprises the following steps:
(1) uniformly mixing chloride, lithium salt and melamine, placing the mixture in a crucible, and covering the crucible with a cover; wherein, the weight ratio of chloride, lithium salt and melamine is as follows: chloride: lithium salt: melamine ═ 9-11: (9-11): (1-2);
(2) heating the crucible containing the reactants in the step (1), raising the temperature to 500-600 ℃ at the speed of 3-8 ℃/min, then preserving the heat for 3-5h, and cooling to 20-25 ℃;
(3) adding chloride and lithium salt with the same weight as the crucible in the step (1) into the crucible in the step (2), heating to 500-; cooling to 20-25 ℃, and drying to obtain the LiCl-CN nano tube with visible light catalytic activity.
Preferably, in the step (1) and the step (3), the chloride is at least one of sodium chloride, potassium chloride, ammonium chloride and lithium chloride.
Preferably, in the step (1) and the step (3), the lithium salt is at least one of lithium chloride, lithium cyanide and n-butyl lithium.
Preferably, the chlorides and lithium salts in the step (1) and the step (3) have good catalytic dispersibility, large specific surface area and best degradation effect on bisphenol A with the same concentration.
Preferably, in the step (1), the chloride, the lithium salt and the melamine are firstly ground into 200-mesh powder, and then the chloride, the lithium salt and the melamine are uniformly mixed and placed in a crucible.
In addition, it should be noted that, when weighing the lithium salt, the final weighing is noted and the operation is rapid, so as to prevent the influence of weight deviation due to water absorption, and further, to prevent the generated ammonia gas from polluting the environment, it is necessary to purify the exhaust gas in a fume hood.
Preferably, in the step (2), the temperature is increased to 550 ℃ at the speed of 5 ℃/min, and the temperature is kept for 4 h; in the step (3), the temperature is increased to 550 ℃ at the speed of 5 ℃/min, and the temperature is kept for 2 h.
Preferably, in the step (1), the weight ratio of chloride, lithium salt and melamine is as follows: chloride: lithium salt: melamine 10: 10: 1.5.
preferably, the chloride is potassium chloride and the lithium salt is lithium chloride.
Preferably, the proportion of the reactants in the step (1) and the step (3) and the reaction conditions are adopted, so that the prepared catalyst has good dispersibility, large specific surface area and best degradation effect on bisphenol A with the same concentration.
Preferably, the preparation process of the LiCl-CN nanotube photocatalyst is carried out in a fume hood. And an air-isolated nitrogen or inert gas protection device is not needed, and the ammonia gas generated by the reaction can play a role in isolating air, so that the generated nano tube is prevented from being oxidized by air.
Meanwhile, the invention also provides the LiCl-CN nano tube with visible light catalytic activity prepared by the preparation method.
In addition, the invention also discloses an application of the LiCl-CN nano tube with visible light catalytic activity in catalytic degradation of bisphenol A-containing wastewater.
Preferably, the optimal catalytic degradation conditions are: the LiCl-CN nano tube is used in an amount of 0.3-0.5g, and is used for catalyzing the degradation of bisphenol A containing 10mg/L under normal temperature and visible light (the pH value of waste water is 5), and the bisphenol A can be completely photolyzed after the illumination time of 180 minutes.
Compared with the prior art, the invention has the beneficial effects that:
(1) the reactants of chloride, lithium salt and melamine used in the invention are common solid reagents in a laboratory, have no volatility and low toxicity at normal temperature, and release ammonia gas in the reaction in the process of preparing the LiCl-CN nano tube, so that special air isolation equipment is not needed, and the energy consumption is saved.
(2) The invention provides a simple method for synthesizing LiCl-CN nano tubes by a one-pot solid-phase reaction method, which is time-saving and does not need to add organic reagents.
(3) The invention effectively promotes g-C by Li doping modification3N4The high-activity visible light catalytic material for separating photoproduction electrons from holes on the surface of the material enhances the utilization rate of the material on visible light, and further improves the photocatalytic efficiency of the material.
Drawings
FIG. 1 shows LiCl-CN nanotubes (a, b) prepared according to the present invention and g-C in the prior art3N4(c, d) scanning electron micrographs;
FIG. 2 shows LiCl-CN nanotubes prepared according to the present invention and g-C in the prior art3N4N of the sample2Adsorption and desorption isotherm diagrams;
FIG. 3 shows LiCl-CN nanotubes prepared according to the present invention and g-C in the prior art3N4An electrochemical impedance map of (a);
FIG. 4 shows LiCl-CN nanotubes prepared according to the present invention and g-C in the prior art3N4Photocurrent density map of (a).
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to the accompanying drawings and specific embodiments.
The preparation process of the LiCl-CN nano tube in the embodiment of the invention comprises the following steps:
(1) respectively grinding reactants into 200-mesh powder, then fully and uniformly mixing the reactants of chloride, lithium salt and melamine according to the mass ratio of (9-11) to (1-2), placing the mixture in an alumina crucible, and covering the alumina crucible with a cover;
(2) heating the alumina crucible in the step (1) to 3-8 ℃ per minute, raising the temperature to 500-600 ℃, preserving the heat for 3.5-5h, taking out and cooling to 20-25 ℃;
(3) adding chloride and lithium salt with the same weight as the aluminum oxide crucible in the step (1) into the aluminum oxide crucible in the step (2), heating the mixture at the temperature of 3-8 ℃ per minute, raising the temperature to 500-600 ℃, and preserving the heat for 1-3 hours to prepare a yellow composite material solid LiCl-CN nanotube;
(4) and (3) catalytically degrading the LiCl-CN nano tube prepared in the step under normal temperature and visible light, wherein the pH of the wastewater is 3-11, the concentration of bisphenol A is 10mg/L, and the degradation time is 0-180 min.
The present application sets forth embodiments 1-18, and the selection of parameters in the process of preparing LiCl-CN nanotubes in specific embodiments 1-18 is shown in table 1:
TABLE 1
As is apparent from the test results in Table 1, 0.5g of the catalyst prepared in example 17 was able to completely photolyze 10mg/L of bisphenol A wastewater within 180 min.
LiCl-CN nanotubes (a, b) prepared by the invention and g-C in the prior art3N4(C, d) the scanning electron micrographs are shown in figure 1, the LiCl-CN nano tube prepared by the invention and the g-C in the prior art3N4N of the sample2The adsorption and desorption isotherms are plotted in FIG. 2, and the LiCl-CN nanotubes prepared by the invention and g-C in the prior art3N4The electrochemical impedance diagram of (a) is shown in figure 3; LiCl-CN nano tube prepared by the invention and g-C in the prior art3N4The photocurrent density graph of (a) is shown in fig. 4. As can be seen from the attached figures 1, 2, 3 and 4, the LiCl-CN nano-tube synthesized by the invention is compared with the graphite carbon nitride g-C on the market3N4More dispersivity (FIG. 1), larger specific surface area (FIG. 2), smaller electrochemical impedance (FIG. 3) and larger lightThe current density (fig. 4) is a visible light catalytic material with high activity.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (9)
1. A preparation method of LiCl-CN nanotubes with visible light catalytic activity is characterized by comprising the following steps:
(1) uniformly mixing chloride, lithium salt and melamine, placing the mixture in a crucible, and covering the crucible with a cover; wherein, the weight ratio of chloride, lithium salt and melamine is as follows: chloride: lithium salt: melamine ═ 9-11: (9-11): (1-2);
(2) heating the crucible containing the reactants in the step (1), raising the temperature to 500-600 ℃ at the speed of 3-8 ℃/min, then preserving the heat for 3-5h, and cooling to 20-25 ℃;
(3) adding chloride and lithium salt with the same weight as the crucible in the step (1) into the crucible in the step (2), heating to 500-; cooling to 20-25 ℃, and drying to obtain the LiCl-CN nano tube with visible light catalytic activity.
2. The method for preparing LiCl-CN nanotubes with visible light catalytic activity according to claim 1, wherein in the step (1) and the step (3), the chloride is at least one of sodium chloride, potassium chloride, ammonium chloride and lithium chloride.
3. The method for preparing LiCl-CN nanotubes with visible light catalytic activity according to claim 1, wherein in the step (1) and the step (3), the lithium salt is at least one of lithium chloride, lithium cyanide and n-butyl lithium.
4. The method for preparing LiCl-CN nanotubes with visible light catalytic activity according to claim 1, wherein in the step (1), the chloride, the lithium salt and the melamine are ground into 200-mesh powder, and then the chloride, the lithium salt and the melamine are uniformly mixed and placed in a crucible.
5. The method for preparing LiCl-CN nanotubes with visible light catalytic activity according to claim 1, wherein in the step (2), the temperature is increased to 550 ℃ at a speed of 5 ℃/min, and the temperature is kept for 4 h; in the step (3), the temperature is increased to 550 ℃ at the speed of 5 ℃/min, and the temperature is kept for 2 h.
6. The method for preparing LiCl-CN nanotubes with visible light catalytic activity according to claim 1, wherein in the step (1), the weight ratio of chloride, lithium salt and melamine is as follows: chloride: lithium salt: melamine 10: 10: 1.5.
7. the method for preparing LiCl-CN nanotubes with visible-light catalytic activity according to claim 1, wherein the chloride is potassium chloride and the lithium salt is lithium chloride.
8. LiCl-CN nanotubes with visible light catalytic activity prepared by the preparation method of any one of claims 1 to 7.
9. Use of LiCl-CN nanotubes having visible light photocatalytic activity according to claim 8 for the catalytic degradation of wastewater containing bisphenol A.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202010701668.4A CN111715266B (en) | 2020-07-20 | 2020-07-20 | LiCl-CN nanotube with visible light catalytic activity and preparation method and application thereof |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202010701668.4A CN111715266B (en) | 2020-07-20 | 2020-07-20 | LiCl-CN nanotube with visible light catalytic activity and preparation method and application thereof |
Publications (2)
Publication Number | Publication Date |
---|---|
CN111715266A true CN111715266A (en) | 2020-09-29 |
CN111715266B CN111715266B (en) | 2021-10-19 |
Family
ID=72572918
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202010701668.4A Active CN111715266B (en) | 2020-07-20 | 2020-07-20 | LiCl-CN nanotube with visible light catalytic activity and preparation method and application thereof |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN111715266B (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112844437A (en) * | 2021-02-03 | 2021-05-28 | 中山大学 | Preparation method of high-crystalline carbon nitride photo-Fenton catalyst and application of high-crystalline carbon nitride photo-Fenton catalyst in degradation of emerging pollutants |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
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 |
CN104801326A (en) * | 2015-03-25 | 2015-07-29 | 天津大学 | Surface-hydroxylated nano-pore carbon nitride photocatalytic material as well as preparation method and application thereof |
CN109364978A (en) * | 2018-12-06 | 2019-02-22 | 滨州学院 | Class fenton catalyst preparation method and its application in treatment of Organic Wastewater |
CN109603875A (en) * | 2018-12-14 | 2019-04-12 | 深圳大学 | Carbon nitride material and its preparation method and application |
-
2020
- 2020-07-20 CN CN202010701668.4A patent/CN111715266B/en active Active
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
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 |
CN104801326A (en) * | 2015-03-25 | 2015-07-29 | 天津大学 | Surface-hydroxylated nano-pore carbon nitride photocatalytic material as well as preparation method and application thereof |
CN109364978A (en) * | 2018-12-06 | 2019-02-22 | 滨州学院 | Class fenton catalyst preparation method and its application in treatment of Organic Wastewater |
CN109603875A (en) * | 2018-12-14 | 2019-04-12 | 深圳大学 | Carbon nitride material and its preparation method and application |
Non-Patent Citations (3)
Title |
---|
JIANNAN ZHAO, ET AL: "Novel band gap-tunable K–Na co-doped graphitic carbon nitrideprepared by molten salt method", 《APPLIED SURFACE SCIENCE》 * |
YING ZHOU, ET AL: "Highly crystalline lithium chloride-intercalated graphitic carbon nitride hollow nanotubes for effective lead removal", 《ENVIRONMENTAL SCIENCE NANO》 * |
高洪林: "无机离子修饰提高g-C3N4光催化性能的研究", 《中国博士学位论文全文数据库工程科技I辑》 * |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112844437A (en) * | 2021-02-03 | 2021-05-28 | 中山大学 | Preparation method of high-crystalline carbon nitride photo-Fenton catalyst and application of high-crystalline carbon nitride photo-Fenton catalyst in degradation of emerging pollutants |
Also Published As
Publication number | Publication date |
---|---|
CN111715266B (en) | 2021-10-19 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN109908959B (en) | Core-shell ZnO/precious metal @ ZIF-8 photocatalytic material and preparation method and application thereof | |
CN112808313B (en) | Nitrogen-doped carbon quantum dot/metal organic framework material MOF-5 photocatalyst and preparation method and application thereof | |
CN107837816B (en) | Fe2O3/g-C3N4Composite system, preparation method and application | |
CN108620113B (en) | Preparation method of nitrogen-doped carbon-cerium composite nanosheet | |
CN111468147A (en) | Porous carbon composite titanium dioxide-oxyhalide photocatalyst and preparation method thereof | |
CN112076777B (en) | For CO2Reduced photocatalyst and preparation method thereof | |
CN112473717B (en) | Nickel monoatomic/functionalized graphite-phase carbon nitride composite catalyst | |
CN112076738A (en) | Boron-doped defective zinc oxide and preparation method and application thereof | |
CN111659453B (en) | Catalyst for visible light-ozone synergistic catalysis and preparation method thereof | |
CN113862700A (en) | Fe-N-C/MoO2Nano composite electrocatalyst and its preparing method and use | |
CN112473712A (en) | CeO treated with different atmospheres2/g-C3N4Heterojunction material, preparation method and application thereof | |
CN111974444A (en) | Preparation method and application of small-pore molecular sieve supported noble metal material prepared by one-pot method | |
CN111644192A (en) | g-C3N4@CdxZn1-xSe composite photocatalyst and preparation method and application thereof | |
CN111715266B (en) | LiCl-CN nanotube with visible light catalytic activity and preparation method and application thereof | |
CN110339852B (en) | CoO @ nitrogen and sulfur co-doped carbon material/CdS composite photocatalytic material, and preparation method and application thereof | |
CN114797942A (en) | Porous metal (iron, nickel and cobalt) doped graphite phase carbon nitride photocatalyst and preparation method and application thereof | |
CN109395759B (en) | Fe with core-shell structure3C nano particle and preparation method and application thereof | |
CN108906110B (en) | Preparation method and application of photocatalyst | |
CN1958158A (en) | Catalysis materials of cobalt oxide, nickel oxide, preparation method and application | |
CN107497427B (en) | Preparation method of silver/graphene/zinc oxide composite material capable of degrading formaldehyde | |
CN111167434B (en) | Photocatalytic composite material Cr for degrading gaseous pollutants2O3-SnO2And preparation method and application thereof | |
CN115555042B (en) | Preparation method of carbon nanotube catalyst, carbon nanotube catalyst and application thereof | |
CN113976107B (en) | Method for preparing Mn-based composite catalyst by using organic waste liquid and application of Mn-based composite catalyst in decomposition of indoor formaldehyde | |
CN114471624B (en) | NiSe 2 /Mn 0.3 Cd 0.7 S heterojunction photocatalyst, and in-situ synthesis method and application thereof | |
CN110523425B (en) | Molybdenum dioxide/nitrogen doped reduced graphene full-spectrum response photocatalyst and preparation method thereof |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
GR01 | Patent grant | ||
GR01 | Patent grant |