CN110787828B - AgNWs/g-C 3 N 4 Preparation method of photodegradation catalyst - Google Patents
AgNWs/g-C 3 N 4 Preparation method of photodegradation catalyst Download PDFInfo
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- 239000002042 Silver nanowire Substances 0.000 title claims abstract description 86
- 238000001782 photodegradation Methods 0.000 title claims abstract description 36
- 239000003054 catalyst Substances 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 239000002131 composite material Substances 0.000 claims abstract description 33
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 23
- 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 26
- 238000001035 drying Methods 0.000 claims description 19
- 238000005303 weighing Methods 0.000 claims description 19
- 238000003756 stirring Methods 0.000 claims description 17
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- 239000000843 powder Substances 0.000 claims description 14
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- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 12
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 12
- 101710134784 Agnoprotein Proteins 0.000 claims description 8
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- 238000009210 therapy by ultrasound Methods 0.000 claims description 7
- 238000004140 cleaning Methods 0.000 claims description 5
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 2
- 239000002070 nanowire Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 23
- 238000001338 self-assembly Methods 0.000 abstract description 6
- 238000012719 thermal polymerization Methods 0.000 abstract description 6
- 230000015556 catabolic process Effects 0.000 abstract description 5
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- 238000006731 degradation reaction 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
- 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
- 229910021591 Copper(I) chloride Inorganic materials 0.000 description 5
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical compound [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 description 5
- 235000019441 ethanol Nutrition 0.000 description 5
- 239000002245 particle Substances 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
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- 230000003197 catalytic effect Effects 0.000 description 2
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- 230000031700 light absorption Effects 0.000 description 2
- 230000005012 migration Effects 0.000 description 2
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- 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
- 238000004626 scanning electron microscopy Methods 0.000 description 2
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- XZMCDFZZKTWFGF-UHFFFAOYSA-N Cyanamide Chemical compound NC#N XZMCDFZZKTWFGF-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
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- 230000009286 beneficial effect Effects 0.000 description 1
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- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
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- 229910052697 platinum Inorganic materials 0.000 description 1
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- 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-C 3 N 4 The preparation method of the photodegradation catalyst is used for solving the problem of Ag/g-C prepared by the existing method 3 N 4 The 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 method 3 N 4 Then preparing AgNWs/g-C by a self-assembly method 3 N 4 Two-phase composite heterojunction of AgNWs and g-C 3 N 4 A good contact is formed. Compared with the background technology, the invention synthesizes the g-C by self-assembly AgNWs and thermal polymerization 3 N 4 Compounding AgNWs and g-C 3 N 4 Good 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 invention 3 N 4 The 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-C 3 N 4 A preparation method of a composite material, in particular to AgNWs/g-C 3 N 4 A 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 therefore, treatment of pollutants is critical for adultsHot spots of note. In 1972, japanese scientists Fujishima and Honda discovered that TiO was exposed to UV light 2 Hydrogen, 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, tiO 2 Is 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 material 3 N 4 And the material is proved to have photocatalytic performance, thereby opening the g-C 3 N 4 The major door to the photocatalytic study, however, due to pure g-C 3 N 4 The interior contains a large number of defects, which can be electron-hole recombination sites, and thus the catalytic performance is low.
The literature "Zhengjiale, guo ren Qing, chenjia, etc.. Ultrasonic regulation of Ag/g-C 3 N 4 Composite material and photocatalytic Performance study [ J]Ageing and application of synthetic materials, 2017,46 (6): 59-62 ″, discloses an Ag/g-C 3 N 4 Method for synthesizing composite material, which prepares g-C by solid phase heating method 3 N 4 Ultrasonic regulation to obtain lamellar g-C 3 N 4 In the form of sheets g-C 3 N 4 Reduction of AgNO by illumination in solution 3 Successfully prepares the Ultr-Ag/g-C 3 N 4 The composite photocatalytic material is compounded, the catalytic performance of the composite material is tested by taking rhodamine B as a simulated pollutant, and the result shows that the Ultr-Ag/g-C prepared by the method 3 N 4 Comparative pure g-C 3 N 4 The 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 low Ag particle content and poor photodegradability.
Published Ag/g-C 3 N 4 The 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, many studies are currently being made to improve excitons by using expensive platinum as a co-catalystSeparation efficiency and carrier mobility. AgNWs and g-C with slightly lower price 3 N 4 The 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 prepared 3 N 4 The 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 method 3 N 4 The invention provides an AgNWs/g-C composite material with poor photodegradability 3 N 4 A preparation method of a photodegradation catalyst. The method adopts a polyol method to prepare AgNWs, and adopts a thermal polymerization method to prepare g-C 3 N 4 Then preparing AgNWs/g-C by a self-assembly method 3 N 4 Two-phase composite heterojunction of AgNWs and g-C 3 N 4 A good contact is formed. The invention controls the g-C of AgNWs and AgNWs 3 N 4 In proportion, organic photodegradation catalysts with different photocatalytic capacities can be obtained. Compared with the background technology method, 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-assembly 3 N 4 Compounding AgNWs with g-C 3 N 4 Good 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 invention 3 N 4 The photodegradation catalyst can realize the complete degradation of the pollutant rhodamine B within 30min, and the photodegradation efficiency is obviously improved.
The technical scheme adopted by the invention for solving the technical problems is as follows: agNWs/g-C 3 N 4 The 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 the temperature of 540 ℃ to 560 ℃ for 3h to 6h, and grinding to obtain g-C 3 N 4 A powder;
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 AgNO 3 Adding 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 one 3 N 4 Dispersing 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 step 3 N 4 Is 0.5 to 10 percent, is stirred for 15 to 20 hours and then is dried for 8 to 15 hours at a temperature of between 60 and 80 ℃ to obtain AgNWs/g-C 3 N 4 A 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-C 3 N 4 Then preparing AgNWs/g-C by a self-assembly method 3 N 4 Two-phase composite heterojunction of AgNWs and g-C 3 N 4 A good contact is formed. The invention controls the g-C of AgNWs and AgNWs 3 N 4 In proportion, organic photodegradation catalysts with different photocatalytic capacities can be obtained. Compared with the background technology method, 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-assembly 3 N 4 Compounding AgNWs with g-C 3 N 4 Good 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 invention 3 N 4 The photodegradation catalyst can realize the treatment of the rhodamine B pollutant within 30minThe degradation is complete, 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 invention 3 N 4 X-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 3 3 N 4 Scanning Electron Microscopy (SEM) images of the photodegradation catalyst.
FIG. 3 shows AgNWs/g-C prepared by the method of example 3 of the present invention 3 N 4 SEM picture of two-phase composite heterojunction of photodegradation catalyst.
FIG. 4 shows AgNWs/g-C prepared by the method of example 3 3 N 4 Ultraviolet-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 3 3 N 4 The 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 grinding 3 N 4 Powder;
(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 AgNO 3 Adding into the solution obtained in step (2), adding 1ml CuCl with the concentration of 2mmol/L 2 Heating 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) Will be provided withDrying the silver nanowire solution obtained in the step (4) to obtain silver nanowires, and weighing 1g of g-C obtained in the step (1) 3 N 4 Dispersing 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-C 3 N 4 A 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 grinding 3 N 4 Powder;
(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 AgNO 3 Adding into the solution obtained in step (2), adding 1.5ml of CuCl with the concentration of 2.3mmol/L 2 Heating the solution to 120 ℃ under continuous stirring and preserving the heat for 0.8h to obtain a gray AgNWs solution;
(4) Centrifuging and washing 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) 3 N 4 Dispersing 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-C 3 N 4 A composite photodegradation catalyst.
Example 3:
(1) Sintering 7g of dicyanodiamine in a muffle furnace at 550 ℃ for 4h to obtain g-C through grinding 3 N 4 Powder;
(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) Weighing 0.5g AgNO 3 Adding into the solution obtained in step (2), adding 2ml of 2.64mmol/L CuCl 2 Continuously 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) 3 N 4 Dispersing the powder into 100ml of absolute ethyl alcohol, performing ultrasonic treatment for 30min, adding 0.02g of AgNWs obtained after drying in the step (4), stirring for 18h, and drying at 70 ℃ for 12h to obtain AgNWs/g-C 3 N 4 A composite photodegradation catalyst.
From FIG. 1AgNWs/g-C 3 N 4 The XRD pattern of the composite photodegradation catalyst shows that the composite material consists of g-C 3 N 4 And Ag two phases, illustrating g-C 3 N 4 The Ag is successfully compounded.
From FIG. 2AgNWs/g-C 3 N 4 The scanning electron microscope picture of the photodegradation catalyst shows that the main form of the obtained product is the nano wire and is mixed with a very small amount of nano particles. The 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-C 3 N 4 SEM pictures of two-phase composite heterojunction of photodegradation catalyst can show that AgNWs and g-C 3 N 4 The interface combination is very good, which indicates that AgNWs/g-C is successfully prepared 3 N 4 A composite material.
As can be seen from the ultraviolet-visible light absorption spectrum of the two-phase composite heterojunction in FIG. 4, agNWs/g-C prepared in the embodiment 3 N 4 The 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 example 3 N 4 The composite photodegradation catalyst can be used for 10minThe degradation rate is 60 percent, 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 grinding 3 N 4 A powder;
(2) Weighing 0.7g of PVP, adding the PVP into 60ml of glycol, heating to 110 ℃, magnetically stirring for 25min to obtain a PVP-glycol solution, and cooling to room temperature;
(3) Weighing 0.8g AgNO 3 Adding into the solution obtained in step (2), adding 3ml of CuCl with the concentration of 2.8mmol/L 2 Heating the solution to 140 ℃ under continuous stirring and preserving the heat for 1.2 hours to obtain a gray AgNWs solution;
(4) Centrifuging and washing 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) 3 N 4 Dispersing 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-C 3 N 4 A composite photodegradation catalyst.
Example 5:
(1) Sintering 12g of dicyanodiamine in a muffle furnace at 560 ℃ for 6h to obtain g-C through grinding 3 N 4 Powder;
(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 of AgNO 3 Adding into the solution obtained in step (2), adding 4ml of CuCl with the concentration of 3mmol/L 2 Heating 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) 3 N 4 Dispersing 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-C 3 N 4 A composite photodegradation catalyst.
Compared with the prior art, the AgNWs/g-C prepared by the invention 3 N 4 The composite photodegradation catalyst has small AgNWs diameter and large length-diameter ratio, and is uniformly loaded on g-C 3 N 4 To g-C 3 N 4 Good 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-C 3 N 4 The 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-C 3 N 4 Powder;
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 AgNO 3 Adding 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 keeping the temperature 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 dryingg-C obtained in step one 3 N 4 Dispersing 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 step 3 N 4 Is 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-C 3 N 4 A composite photodegradation catalyst;
the AgNWs/g-C 3 N 4 The composite photodegradation catalyst is mainly in the form of nanowires, the AgNWs has the diameter of 60-200 nm and the length of 15-25 μm.
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