CN110787828A - AgNWs/g-C3N4Preparation method of photodegradation catalyst - Google Patents
AgNWs/g-C3N4Preparation method of photodegradation catalyst Download PDFInfo
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- 239000002042 Silver nanowire Substances 0.000 title claims abstract description 90
- 238000001782 photodegradation Methods 0.000 title claims abstract description 36
- 239000003054 catalyst Substances 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title abstract description 23
- 239000002131 composite material Substances 0.000 claims abstract description 31
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000002360 preparation method Methods 0.000 claims abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 31
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 28
- 238000001035 drying Methods 0.000 claims description 21
- 238000005303 weighing Methods 0.000 claims description 18
- 238000003756 stirring Methods 0.000 claims description 17
- 238000010438 heat treatment Methods 0.000 claims description 15
- 239000000843 powder Substances 0.000 claims description 14
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 12
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 12
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 12
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(I) nitrate Inorganic materials [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 12
- 238000005119 centrifugation Methods 0.000 claims description 7
- 238000004140 cleaning Methods 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 7
- 238000005245 sintering Methods 0.000 claims description 7
- 238000009210 therapy by ultrasound Methods 0.000 claims description 7
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 2
- 238000001338 self-assembly Methods 0.000 abstract description 6
- 238000012719 thermal polymerization Methods 0.000 abstract description 6
- 238000013329 compounding Methods 0.000 abstract description 5
- 239000003344 environmental pollutant Substances 0.000 abstract description 5
- 231100000719 pollutant Toxicity 0.000 abstract description 5
- 238000004917 polyol method Methods 0.000 abstract description 5
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 abstract description 5
- 229940043267 rhodamine b Drugs 0.000 abstract description 5
- 230000015556 catabolic process Effects 0.000 abstract description 4
- 238000006731 degradation reaction Methods 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 3
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 abstract description 3
- 239000012071 phase Substances 0.000 description 11
- 230000001699 photocatalysis Effects 0.000 description 10
- 235000019441 ethanol Nutrition 0.000 description 5
- 229910021591 Copper(I) chloride Inorganic materials 0.000 description 4
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical compound [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 229910052709 silver Inorganic materials 0.000 description 3
- 239000004332 silver Substances 0.000 description 3
- 101710134784 Agnoprotein Proteins 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000000862 absorption spectrum Methods 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000031700 light absorption Effects 0.000 description 2
- 238000013508 migration Methods 0.000 description 2
- 230000005012 migration Effects 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 239000011941 photocatalyst Substances 0.000 description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 230000006798 recombination Effects 0.000 description 2
- 238000005215 recombination Methods 0.000 description 2
- 238000002310 reflectometry Methods 0.000 description 2
- XZMCDFZZKTWFGF-UHFFFAOYSA-N Cyanamide Chemical compound NC#N XZMCDFZZKTWFGF-UHFFFAOYSA-N 0.000 description 1
- -1 Hydrogen Chemical class 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003426 co-catalyst Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- 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
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/48—Silver or gold
- B01J23/50—Silver
-
- B01J35/23—
-
- B01J35/39—
-
- B01J35/399—
-
- 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
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- 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 AgNWs/g-C3N4A preparation method of a photodegradation catalyst, which is used for solving the problem of Ag/g-C prepared by the existing method3N4The photodegradability of the composite material is poor. The technical proposal is that AgNWs is prepared by adopting a polyol method, and g-C is prepared by a thermal polymerization method3N4Then preparing AgNWs/g-C by a self-assembly method3N4Two-phase composite heterojunction of AgNWs and g-C3N4A good contact is formed. Compared with the background technology, the invention synthesizes the g-C by self-assembly AgNWs and thermal polymerization3N4Compounding AgNWs with g-C3N4Good contact is formed, and the interface combination of the silver powder and the graphite-like phase carbon nitride is improved. The invention is madePrepared AgNWs/g-C3N4The photodegradation catalyst can realize the complete degradation of the rhodamine B pollutant within 30min, and the photodegradation efficiency is obviously improved.
Description
Technical Field
The invention relates to Ag/g-C3N4Process for the preparation of composite materials, in particularAnd an AgNWs/g-C3N4A preparation method of a photodegradation catalyst.
Background
In recent years, with the rapid progress of industrialization, human consumption of energy is increasing, fossil fuel causes serious environmental pollution, and thus, the treatment of pollutants is a hot spot for adults to pay attention. In 1972, Japanese scientists Fujishima and Honda discovered that TiO was exposed to UV light2Hydrogen, a clean energy source, can be produced by decomposing water through photocatalysis, and has caused a hot trend of research on semiconductor photocatalysts all over the world.
Hitherto, TiO2Is recognized as one of the most potential photocatalysts, but has a wide energy band gap and certain photocatalytic activity only in an ultraviolet region, so that the utilization rate of sunlight is low. In 2009, g-C was successfully synthesized by professor Wangxinchen university of Fuzhou at 550 ℃ by using cyanamide as a raw material3N4And the material is proved to have photocatalytic performance, thereby opening the g-C3N4The main door of the photocatalytic study, but due to pure g-C3N4The interior contains a large number of defects which can be electron-hole recombination sites and therefore have poor catalytic performance.
The literature "Zhengjiale, Guo ren Qing, Chenjia, etc.. ultrasonic regulation of Ag/g-C3N4Composite material and photocatalytic Performance study [ J]Ageing and application of synthetic materials, 2017,46(6): 59-62 ″, discloses an Ag/g-C3N4Method for synthesizing composite material, which prepares g-C by solid phase heating method3N4Ultrasonic regulation to obtain lamellar g-C3N4In the form of sheets g-C3N4Reduction of AgNO by illumination in solution3Successfully prepare the Ultr-Ag/g-C3N4The composite photocatalytic material is tested for catalytic performance by taking rhodamine B as a simulated pollutant, and the result shows that the Ultr-Ag/g-C prepared by the method3N4Comparative pure g-C3N4The photodegradability is greatly improved, and more than 70 percent of degradation can be realized within 80 min. However, the composite material synthesized by the method has extremely low content of Ag particles and is photodegradableThe performance is poor.
Published Ag/g-C3N4The composite material mostly adopts silver particles as a load, the silver particles are less in load, the combination with the silver particles is poor, and the photodegradation effect is poor. In addition, in order to improve photocatalytic efficiency, much research is currently being conducted on the use of expensive platinum as a co-catalyst to improve exciton separation efficiency and carrier mobility. AgNWs and g-C with slightly lower price3N4The two nano materials can generate a new heterostructure through compounding, an optimal interface is obtained through regulating the morphology of the two nano materials, so that exciton separation and carrier rapid migration are promoted, hole-exciton compounding is further avoided, and better photocatalytic degradation performance is expected to be obtained. Thus, AgNWs/g-C was designed and prepared3N4The composite photocatalytic material has great significance in both academic research and practical application.
Disclosure of Invention
In order to overcome the problem that the Ag/g-C prepared by the prior method3N4The invention provides an AgNWs/g-C composite material with poor photodegradability3N4A preparation method of a photodegradation catalyst. The method adopts a polyol method to prepare AgNWs, and adopts a thermal polymerization method to prepare g-C3N4Then preparing AgNWs/g-C by a self-assembly method3N4Two-phase composite heterojunction of AgNWs and g-C3N4A good contact is formed. The invention controls the g-C of AgNWs and AgNWs3N4In proportion, organic photodegradation catalysts with different photocatalytic capacities can be obtained. Compared with the background technology, the invention prepares AgNWs with the diameter of 60 nm-200 nm and the length of 15 mu m-25 mu m by a polyol method, and then synthesizes the AgNWs with g-C synthesized by a thermal polymerization method through self-assembly3N4Compounding AgNWs with g-C3N4Good contact is formed, and the interface combination of the silver powder and the graphite-like phase carbon nitride is improved. AgNWs/g-C prepared by the invention3N4The photodegradation catalyst can realize the complete degradation of the rhodamine B pollutant within 30min, and the photodegradation efficiency is obviously improved.
The invention solves the technical problemThe technical scheme is as follows: AgNWs/g-C3N4The preparation method of the photodegradation catalyst is characterized by comprising the following steps:
step one, placing 5g to 12g of dicyanodiamine into a muffle furnace for sintering at 540 ℃ to 560 ℃ for 3h to 6h, and grinding to obtain g-C3N4Powder;
step two, weighing 0.1 to 1g of polyvinylpyrrolidone, adding the polyvinylpyrrolidone into 35 to 70ml of ethylene glycol, heating to 70 to 120 ℃, stirring for 5 to 30min, obtaining PVP-ethylene glycol solution, and cooling;
step three, weighing 0.2 g-1 g AgNO3Adding the solution obtained in the second step, adding 1-4 ml of copper chloride solution with the concentration of 2-3 mmol/L, heating to 110-150 ℃, and preserving heat for 0.5-1.5 h to obtain a gray AgNWs solution;
step four, centrifugally cleaning the solution obtained in the step three for 2 to 6 times by using absolute ethyl alcohol at the rotating speed of 4000 to 6000rpm, and dispersing the solution into 10 to 30ml of absolute ethyl alcohol after centrifugation to form an AgNWs solution;
step five, drying the silver nanowire solution obtained in the step four to obtain AgNWs, and drying the g-C obtained in the step one3N4Dispersing the powder into 80-120 ml of absolute ethyl alcohol, performing ultrasonic treatment for 10-50 min, and adding AgNWs, AgNWs and g-C obtained by drying in the fourth step3N4Is 0.5 to 10 percent, is stirred for 15 to 20 hours and then is dried for 8 to 15 hours at the temperature of between 60 and 80 ℃ to obtain AgNWs/g-C3N4A composite photodegradation catalyst.
The invention has the beneficial effects that: the method adopts a polyol method to prepare AgNWs, and adopts a thermal polymerization method to prepare g-C3N4Then preparing AgNWs/g-C by a self-assembly method3N4Two-phase composite heterojunction of AgNWs and g-C3N4A good contact is formed. The invention controls the g-C of AgNWs and AgNWs3N4In proportion, organic photodegradation catalysts with different photocatalytic capacities can be obtained. Compared with the background technology, the invention prepares AgNWs with the diameter of 60 nm-200 nm and the length of 15 mu m-25 mu m by a polyol method, and theng-C synthesized by AgNWs and thermal polymerization through self-assembly3N4Compounding AgNWs with g-C3N4Good contact is formed, and the interface combination of the silver powder and the graphite-like phase carbon nitride is improved. AgNWs/g-C prepared by the invention3N4The photodegradation catalyst can realize the complete degradation of the rhodamine B pollutant within 30min, and the photodegradation efficiency is obviously improved.
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
Drawings
FIG. 1 shows AgNWs/g-C prepared by the method of example 3 of the present invention3N4X-ray diffraction pattern (XRD) of the two-phase composite heterojunction of the photodegradation catalyst.
FIG. 2 shows AgNWs/g-C prepared by the method of example 33N4Scanning Electron Microscopy (SEM) images of the photodegradation catalyst.
FIG. 3 shows AgNWs/g-C prepared by the method of example 3 of the present invention3N4SEM picture of two-phase composite heterojunction of photodegradation catalyst.
FIG. 4 shows AgNWs/g-C prepared by the method of example 33N4Ultraviolet-visible light absorption spectrum of the two-phase composite heterojunction of the photodegradation catalyst.
FIG. 5 shows AgNWs/g-C prepared by the method of example 33N4The effect graph of photodegradation of the two-phase composite heterojunction of the photodegradation catalyst under the action of visible light.
Detailed Description
The following examples refer to fig. 1-5.
Example 1:
(1) placing 5g of dicyanodiamine into a muffle furnace for sintering at 540 ℃ for 3h to obtain g-C through grinding3N4Powder;
(2) weighing 0.1g of PVP, adding into 35ml of ethylene glycol, heating to 70 ℃, magnetically stirring for 5min to obtain a PVP-ethylene glycol solution, and cooling to room temperature;
(3) weighing 0.2g AgNO3Adding into the solution obtained in step (2), adding 1ml of 2mmol/LCuCl2Heating the solution to 110 ℃ under continuous stirring and preserving heat for 0.5h to prepare a gray AgNWs solution;
(4) centrifuging and cleaning the solution obtained in the step (3) for 2 times by using ethanol at the rotating speed of 4000rpm, and dispersing the solution into 10ml of absolute ethanol after centrifugation to form a silver nanowire solution;
(5) drying the silver nanowire solution obtained in the step (4) to obtain silver nanowires, and weighing 1g of g-C obtained in the step (1)3N4Dispersing the powder into 80ml of absolute ethyl alcohol, performing ultrasonic treatment for 10min, adding 0.005g of AgNWs obtained after drying in the step (4), stirring for 15h, and then drying at 60 ℃ for 8h to obtain AgNWs/g-C3N4A composite photodegradation catalyst.
Example 2:
(1) placing 6g of dicyanodiamine into a muffle furnace for sintering at 545 ℃ for 3.5h to obtain g-C through grinding3N4Powder;
(2) weighing 0.2g of PVP, adding into 45ml of ethylene glycol, heating to 80 ℃, magnetically stirring for 10min to obtain a PVP-ethylene glycol solution, and cooling to room temperature;
(3) weighing 0.4g AgNO3Adding into the solution obtained in step (2), adding 1.5ml of CuCl with the concentration of 2.3mmol/L2Heating the solution to 120 ℃ under continuous stirring and preserving heat for 0.8h to obtain a gray AgNWs solution;
(4) centrifuging and cleaning the solution obtained in the step (3) for 3 times by using ethanol at the rotating speed of 4500rpm, and dispersing the solution into 15ml of absolute ethanol after centrifugation to form a silver nanowire solution;
(5) drying the silver nanowire solution obtained in the step (4) to obtain silver nanowires, and weighing 1g of g-C obtained in the step (1)3N4Dispersing the powder into 90ml of absolute ethyl alcohol, performing ultrasonic treatment for 20min, adding 0.01g of AgNWs obtained after drying in the step (4), stirring for 16h, and drying at 65 ℃ for 10h to obtain AgNWs/g-C3N4A composite photodegradation catalyst.
Example 3:
(1) placing 7g of dicyanodiamine into a muffle furnace for sintering at 550 ℃ for 4h, and grinding to obtain g-C3N4Powder;
(2) weighing 0.4g of PVP, adding into 50ml of ethylene glycol, heating to 100 ℃, magnetically stirring for 20min to obtain a solution with PVP-ethylene glycol, and cooling to room temperature;
(3) 0.5g of AgNO is weighed3Adding into the solution obtained in step (2), adding 2ml of CuCl with the concentration of 2.64mmol/L2Continuously stirring the solution, heating to 130 ℃, and preserving heat for 1h to obtain a gray AgNWs solution;
(4) centrifuging and cleaning the solution obtained in the step (3) for 4 times by using ethanol at the rotating speed of 5000rpm, and dispersing the solution into 20ml of absolute ethanol after centrifugation to form a silver nanowire solution;
(5) drying the silver nanowire solution obtained in the step (4) to obtain silver nanowires, and weighing 1g of g-C obtained in the step (1)3N4Dispersing the powder into 100ml absolute ethyl alcohol, performing ultrasonic treatment for 30min, adding 0.02g AgNWs obtained after drying in the step (4), stirring for 18h, and drying at 70 ℃ for 12h to obtain AgNWs/g-C3N4A composite photodegradation catalyst.
From FIG. 1AgNWs/g-C3N4The XRD pattern of the composite photodegradation catalyst shows that the composite material consists of g-C3N4And Ag two phases, illustrating g-C3N4The Ag is successfully compounded.
From FIG. 2AgNWs/g-C3N4The scanning electron microscope picture of the photodegradation catalyst shows that the main form of the obtained product is a nanowire mixed with a very small amount of nanoparticles. AgNWs are relatively uniform in size, with diameters between 60nm and 200nm, lengths between 15 μm and 25 μm, and a few AgNWs that are too long to be counted beyond the field of view.
From FIG. 3AgNWs/g-C3N4SEM pictures of two-phase composite heterojunction of photodegradation catalyst can show that AgNWs and g-C3N4The interface combination is good, which indicates that AgNWs/g-C is successfully prepared3N4A composite material.
As can be seen from the ultraviolet-visible light absorption spectrum of the two-phase composite heterojunction shown in FIG. 4, AgNWs/g-C prepared in the embodiment3N4The reflectivity of the photodegradation catalyst to visible light and far ultraviolet light is 10%, and the reflectivity to near ultraviolet light is 70%, which shows that the composite material has good absorption capacity to visible light.
As can be seen from FIG. 5, AgNWs/g-C prepared in this example3N4The photodegradation rate of the composite photodegradation catalyst is 60% within 10min, and the rhodamine B can be completely degraded within 30 min.
Example 4:
(1) sintering 10g of dicyanodiamine in a muffle furnace at 555 ℃ for 5h to obtain g-C by grinding3N4Powder;
(2) weighing 0.7g of PVP, adding the PVP into 60ml of ethylene glycol, heating to 110 ℃, magnetically stirring for 25min to obtain a PVP-ethylene glycol solution, and cooling to room temperature;
(3) weighing 0.8g AgNO3Adding into the solution obtained in step (2), adding 3ml of CuCl with the concentration of 2.8mmol/L2Continuously stirring the solution, heating to 140 ℃, and preserving heat for 1.2 hours to obtain a gray AgNWs solution;
(4) centrifuging and cleaning the solution obtained in the step (3) for 5 times by using ethanol at the rotating speed of 5500rpm, and dispersing the solution into 25ml of absolute ethanol after centrifugation to form a silver nanowire solution;
(5) drying the silver nanowire solution obtained in the step (4) to obtain silver nanowires, and weighing 1g of g-C obtained in the step (1)3N4Dispersing the powder into 110ml of absolute ethyl alcohol, performing ultrasonic treatment for 40min, adding 0.05g of AgNWs obtained after drying in the step (4), stirring for 19h, and drying at 75 ℃ for 14h to obtain AgNWs/g-C3N4A composite photodegradation catalyst.
Example 5:
(1) placing 12g of dicyanodiamine into a muffle furnace for sintering at 560 ℃ for 6h, and grinding to obtain g-C3N4Powder;
(2) weighing 1g of polyvinylpyrrolidone (PVP) and adding the PVP into 70ml of ethylene glycol, heating to 120 ℃, magnetically stirring for 30min to obtain a PVP-ethylene glycol solution, and cooling to room temperature;
(3) weighing 1g AgNO3Adding into the solution obtained in step (2), adding 4ml of CuCl with the concentration of 3mmol/L2Heating the solution to 150 ℃ under continuous stirring, and keeping the temperature for 1.5h to obtain a gray AgNWs solution;
(4) centrifuging and cleaning the solution obtained in the step (3) for 6 times by using ethanol at the rotating speed of 6000rpm, and dispersing the solution into 30ml of absolute ethanol after centrifugation to form a silver nanowire solution;
(5) drying the silver nanowire solution obtained in the step (4) to obtain silver nanowires, and weighing 1g of g-C obtained in the step (1)3N4Dispersing the powder into 120ml of absolute ethyl alcohol, performing ultrasonic treatment for 50min, adding 0.1g of AgNWs obtained after drying in the step (4), stirring for 20h, and drying at 80 ℃ for 15h to obtain AgNWs/g-C3N4A composite photodegradation catalyst.
Compared with the prior art, the AgNWs/g-C prepared by the invention3N4The composite photodegradation catalyst has small AgNWs diameter and large length-diameter ratio, and is uniformly loaded on g-C3N4To g-C3N4Good contact is formed, interface combination of the two is improved, exciton separation and rapid carrier migration are promoted, hole-exciton recombination is further avoided, and photocatalytic degradation capability is greatly improved.
Claims (1)
1. AgNWs/g-C3N4The preparation method of the photodegradation catalyst is characterized by comprising the following steps of:
step one, placing 5g to 12g of dicyanodiamine into a muffle furnace for sintering at 540 ℃ to 560 ℃ for 3h to 6h, and grinding to obtain g-C3N4Powder;
step two, weighing 0.1 to 1g of polyvinylpyrrolidone, adding the polyvinylpyrrolidone into 35 to 70ml of ethylene glycol, heating to 70 to 120 ℃, stirring for 5 to 30min, obtaining PVP-ethylene glycol solution, and cooling;
step three, weighing 0.2 g-1 g AgNO3Adding the solution obtained in the second step, adding 1-4 ml of copper chloride solution with the concentration of 2-3 mmol/L, heating to 110-150 ℃, and preserving heat for 0.5-1.5 h to obtain a gray AgNWs solution;
step four, centrifugally cleaning the solution obtained in the step three for 2 to 6 times by using absolute ethyl alcohol at the rotating speed of 4000 to 6000rpm, and dispersing the solution into 10 to 30ml of absolute ethyl alcohol after centrifugation to form an AgNWs solution;
step five, drying the silver nanowire solution obtained in the step four to obtain AgNWs, and drying the g-C obtained in the step one3N4Dispersing the powder into 80-120 ml of absolute ethyl alcohol, performing ultrasonic treatment for 10-50 min, and adding AgNWs, AgNWs and g-C obtained by drying in the fourth step3N4Is 0.5 to 10 percent, is stirred for 15 to 20 hours and then is dried for 8 to 15 hours at the temperature of between 60 and 80 ℃ to obtain AgNWs/g-C3N4A composite photodegradation catalyst.
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