CN108328692B - Photocatalytic fuel cell system and method for recovering noble metal silver and degrading organic matters through photoelectrocatalysis - Google Patents
Photocatalytic fuel cell system and method for recovering noble metal silver and degrading organic matters through photoelectrocatalysis Download PDFInfo
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Abstract
The invention belongs to the technical field of catalysis, and provides a photocatalytic fuel cell system which comprises a bismuth vanadate photo-anode membrane electrode, a copper oxide/cuprous oxide heterojunction photo-cathode membrane electrode and an electrolyte solution. The invention has the advantages that the photocatalytic fuel cell system does not need an external power supply when performing photoelectrocatalysis recovery of noble metal silver in wastewater and degrading organic matters, can efficiently recover low-concentration noble metal silver ions in the wastewater, and can effectively remove the organic matters.
Description
Technical Field
The invention belongs to the technical field of catalysis, and relates to a photocatalytic fuel cell system and a method for recovering noble metal silver and degrading organic matters by utilizing the photocatalytic fuel cell system through photoelectrocatalysis.
Background
Silver is a naturally occurring precious metal, has limited storage capacity and relatively limited yield, and is widely used in the industries of electronics, chemical engineering, photosensitive materials and the like. Silver-containing wastewater is often produced, however, in processes involving the production and use of silver. Because silver ions have strong toxicity to human and livestock, silver removal and recovery need to be considered, and the recovery treatment of the precious metal silver not only has environmental protection value, but also has important social and economic significance.
At present, the main methods for recovering silver include an electrolytic method, a metal substitution method, an ion exchange method, and the like. The electrolysis and metal replacement method has the greatest advantages that the method can recover the metallic silver with higher purity, but is only suitable for recovering the silver in the silver-containing wastewater with high concentration, and the concentration of the silver in the treated wastewater still can not reach the discharge standard.
Photocatalytic wastewater fuel cells (PFCs) use light as an energy source to drive fuel cells to degrade pollutants. The traditional photocatalytic wastewater fuel cell system consists of a semiconductor photo-anode membrane electrode and an auxiliary cathode, wherein the cathode and the anode are connected through a lead, under illumination, the semiconductor photo-anode membrane electrode generates photo-generated holes and photo-generated electrons, the photo-generated electrons are transmitted to the cathode through an external circuit to generate a reduction reaction, and meanwhile, the residual photo-generated holes of the photo-anode membrane electrode can generate a catalytic oxidation reaction, so that the integration of organic matter degradation and electric energy recovery is realized.
In recent years, photocatalytic fuel cells have not only achieved visible light drive, but have also gradually moved toward bipolar photocatalytic fuel cells composed of photoanode membrane electrodes and photocathode membrane electrodes, and have been gradually applied to wastewater treatment.
Disclosure of Invention
The invention aims to strengthen the low-concentration silver ions in the water catalytically recovered by a photocatalytic fuel cell system and degrade organic matters. Therefore, an efficient photocatalytic fuel cell system is constructed and applied to wastewater containing low-concentration silver ions and organic matters, and the silver ions in the wastewater can be rapidly degraded, removed and recovered through the photoelectrocatalysis effect.
The technical scheme of the invention is as follows:
a photocatalytic fuel cell system comprises a bismuth vanadate photo-anode membrane electrode, a copper oxide/cuprous oxide heterojunction photo-cathode membrane electrode and an electrolyte solution; visible light with the wavelength of more than 420nm is used as a photocatalytic light source, and the cathode and the anode are connected by a lead.
Further, the bismuth vanadate photoanode membrane electrode is obtained by firstly obtaining a bismuth oxyiodide electrode through electrodeposition, then soaking the obtained bismuth oxyiodide electrode in a dimethyl sulfoxide solution of vanadyl acetylacetonate, and calcining the soaked bismuth oxyiodide electrode in a muffle furnace.
Further, the concentration of the dimethyl sulfoxide solution of the vanadyl acetylacetone ester is 0.2-0.5M, and the soaking time is 10-30 seconds.
Further, the calcining temperature in the muffle furnace is 400-500 ℃, and the calcining time is 0.8-1.2 h.
Further, the copper oxide/cuprous oxide heterojunction photocathode membrane electrode is obtained by firstly obtaining a cuprous oxide electrode through electrodeposition, and then placing the obtained cuprous oxide electrode into a muffle furnace for calcination.
Further, the calcining temperature of the cuprous oxide electrode in the muffle furnace is 350-450 ℃, and the calcining time is 1.5-3 h.
Further, the electrolyte is sodium sulfate, and the concentration of the electrolyte solution is 50.0-100.0 mM.
The invention also provides a method for recovering the noble metal silver by photoelectrocatalysis and degrading organic matters, which comprises the following operation steps: the photocatalytic fuel cell system is added into a reactor of wastewater containing silver ions and organic matters, and a photoelectrocatalysis reaction is carried out under the action of visible light, so that the organic matters in the wastewater are degraded and removed, and simultaneously, the silver ions in the wastewater are recovered.
Further, the time of the photoelectrocatalysis reaction is 120-240 min.
Furthermore, the concentration of silver ions in the wastewater is less than 50 mg/L, and the concentration of organic matters is less than 10 mg/L.
Has the advantages that:
the invention provides a photocatalytic fuel cell system and a method for recovering noble metal silver through photoelectrocatalysis and degrading organic matters by the photocatalytic fuel cell system under visible light, wherein the photocatalytic fuel cell system comprises a bismuth vanadate photo-anode membrane electrode, a copper oxide/cuprous oxide heterojunction photo-cathode membrane electrode and an electrolyte, the system is applied to waste water containing low-concentration silver ions and organic matters, and under the action of visible light, the photocatalytic fuel cell can be driven to react through self-bias without consuming extra electric energy, so that the aim of saving energy and resources simultaneously is fulfilled. The method can efficiently recover low-concentration noble metal silver ions in the wastewater, can effectively remove organic matters, and has the recovery rate of the silver ions up to 100 percent and the removal rate of organic phenol over 60 percent.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a scanning electron microscope image of a bismuth vanadate photoanode membrane electrode prepared according to an embodiment of the present invention;
FIG. 2 is a scanning electron microscope image of a prepared copper oxide/cuprous oxide heterojunction photocathode membrane electrode of the embodiment of the invention;
FIG. 3 is a scanning electron microscope image of the copper oxide/cuprous oxide heterojunction photocathode membrane electrode of example 1 after silver recovery;
FIG. 4 is a scanning electron micrograph of a copper oxide/cuprous oxide heterojunction photocathode membrane electrode of example 2 after silver recovery.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The embodiment of the invention provides a photocatalytic fuel cell system, which comprises a bismuth vanadate photo-anode membrane electrode, a copper oxide/cuprous oxide heterojunction photo-cathode membrane electrode and an electrolyte solution; visible light with the wavelength of more than 420nm is used as a photocatalytic light source, and the cathode and the anode are connected by a lead.
The photocatalytic fuel cell system can realize self-bias driving reaction under the action of visible light, does not need additional electric energy consumption, and achieves the purpose of saving energy and resources simultaneously.
Under the action of visible light, the photocatalysed fuel cell system semiconductor bismuth vanadate photocathode membrane electrode and copper oxide/cuprous oxide membrane electrode photocathode generate photoproduction holes and photoproduction electrons, wherein the photoproduction electrons generated by the anode are transmitted to the copper oxide/cuprous oxide photocathode through an external circuit and are compounded with the holes of the copper oxide/cuprous oxide photocathode, the rest photoproduction electrons of the photocathode generate reduction reaction with silver ions, and meanwhile, the rest photoproduction holes of the photocathode can generate catalytic oxidation reaction with organic matters, so that the integration of organic matter degradation and electric energy recovery is realized. The silver recovered on the electrode also plays a certain role in strengthening the degradation of organic matters. The system can be used in wastewater containing silver ions and organic matters, generates photoproduction electrons and photoproduction holes with strong oxidizing property, and can react with metal silver ions and organic matters in electrolyte to realize the recovery of degraded organic matters and metal silver.
In the embodiment of the invention, the bismuth vanadate photoanode membrane electrode is a bismuth vanadate membrane electrode serving as a photoanode, and the copper oxide/cuprous oxide heterojunction photocathode membrane electrode is a copper oxide/cuprous oxide heterojunction membrane electrode serving as a photocathode.
In one embodiment of the invention, the bismuth vanadate photoanode membrane electrode is obtained by firstly obtaining a bismuth oxyiodide electrode through electrodeposition, then soaking the obtained bismuth oxyiodide electrode in a dimethyl sulfoxide solution of vanadyl acetylacetonate, and calcining the soaked bismuth oxyiodide electrode in a muffle furnace; the copper oxide/cuprous oxide heterojunction photocathode membrane electrode is obtained by firstly obtaining a cuprous oxide electrode through electrodeposition, and then putting the obtained cuprous oxide electrode into a muffle furnace for calcination.
In the embodiment of the invention, under the illumination with the wavelength of 420nm, a semiconductor bismuth vanadate photo-anode and a copper oxide/cuprous oxide photo-cathode generate photo-generated holes and photo-generated electrons, wherein the photo-generated electrons generated by the anode are transmitted to the copper oxide/cuprous oxide photo-cathode through an external circuit and are compounded with the holes of the copper oxide/cuprous oxide photo-cathode, the rest photo-generated electrons of the photo-cathode are subjected to reduction reaction with silver ions, and meanwhile, the rest photo-generated holes of the photo-anode can be subjected to catalytic oxidation reaction with organic matters, so that the integration of organic matter degradation and electric energy recovery is realized.
In an embodiment of the invention, the bismuth vanadate photoanode membrane electrode is obtained by firstly obtaining a bismuth oxyiodide electrode through electrodeposition, then soaking the obtained bismuth oxyiodide electrode in a dimethyl sulfoxide solution of vanadyl acetylacetonate, and calcining the soaked bismuth oxyiodide electrode in a muffle furnace.
In one embodiment of the present invention, the concentration of the dimethylsulfoxide solution of vanadyl acetylacetonate is 0.2-0.5M and the soaking time is 10-30 seconds, the concentration of the dimethylsulfoxide solution of vanadyl acetylacetonate may be 0.2M, 0.3M, 0.4M, 0.5M, etc., preferably 0.4M, and the soaking time may be 10, 20, 30 seconds, preferably 20 seconds.
In an embodiment of the invention, the calcination temperature in the muffle furnace is 400-500 ℃, and the calcination time is 0.8-1.2 h. The calcining temperature is 400 ℃ and the calcining time is respectively 1.2h and 0.8h at 500 ℃, the calcining temperature in the muffle furnace is preferably 450 ℃, and the calcining time is 1 h.
In one embodiment of the present invention, the deposition solution of the precursor bismuth oxyiodide in the preparation method of bismuth oxyiodide electrodeposition is prepared by mixing 100M L aqueous nitric acid solution containing 0.0075M bismuth nitrate and 0.4M sodium iodide and having pH of 1.2 with 45M L0.3.3M ethanol solution of p-benzoquinone.
In one embodiment of the invention, the preparation method of the bismuth oxyiodide electrodeposition has the applied voltage of-0.1V and the SnO doped with fluorine2Transparent conductive glass (FTO) is used as a working electrode, a counter electrode is a platinum wire, and the reference electrode is a silver/silver chloride electrode.
In a preferred embodiment of the invention, the preparation method of the bismuth vanadate anode comprises the steps of mixing 100M L of aqueous nitric acid solution containing 0.0075M bismuth nitrate and 0.4M sodium iodide and having a pH value of 1.2 with 45M L0.3.3M ethanol solution of p-benzoquinone to prepare a bismuth oxyiodide electrode, wherein the applied voltage in the electrodeposition method is-0.1V, FTO is a working electrode, a platinum wire is a counter electrode, and the reference electrode is a silver/silver chloride electrode, immersing the bismuth oxyiodide electrode in 0.4M dimethyl sulfoxide solution of vanadyl acetylacetonate for 20 seconds, and then putting the obtained electrode into a muffle furnace to calcine at 450 ℃ for 1 hour to obtain the bismuth vanadate photo-anode membrane electrode.
In another embodiment of the invention, the copper oxide/cuprous oxide heterojunction photocathode membrane electrode is obtained by firstly obtaining a cuprous oxide electrode through electrodeposition, and then placing the obtained cuprous oxide electrode into a muffle furnace for calcination.
The copper oxide/cuprous oxide heterojunction photocathode membrane electrode in the embodiment of the invention is a heterojunction photocathode membrane electrode formed at the joint of the copper oxide and the cuprous oxide.
In one embodiment of the invention, the calcination temperature of the cuprous oxide electrode in the muffle furnace is 350-450 ℃, and the calcination time is 1.5-3 h.
In one embodiment of the present invention, the cuprous oxide electrode electrodeposition preparation method is a method in which the deposition solution of the precursor cuprous oxide is a mixed aqueous solution containing 0.48M copper sulfate and 3M sodium lactate.
In one embodiment of the invention, in the preparation method of cuprous oxide electrode electrodeposition, the applied voltage is-0.3V, FTO glass is used as a working electrode, a counter electrode is a platinum wire, and a reference electrode is a calomel electrode.
In a preferred embodiment of the present invention, the preparation method of the copper oxide/cuprous oxide heterojunction cathode comprises: the deposition solution of the precursor cuprous oxide was a mixed aqueous solution containing 0.48M copper sulfate and 3M sodium lactate. And (3) obtaining the cuprous oxide electrode by an electrodeposition method, wherein the applied voltage is-0.3V, the FTO glass is used as a working electrode, the counter electrode is a platinum wire, and the reference electrode is a calomel electrode. And then, putting the obtained electrode into a muffle furnace to calcine for 2 hours at the temperature of 400 ℃ to obtain the copper oxide/cuprous oxide heterojunction cathode.
In another aspect, an embodiment of the present invention further provides a method for recovering noble metal silver and degrading organic matters through photoelectrocatalysis by using the above photocatalytic fuel cell system under visible light, including the following steps: adding the photocatalytic fuel cell system into a reactor of wastewater containing silver ions and organic matters, forming self-bias by photoproduction holes and photoproduction electrons generated under the action of visible light, degrading and removing the organic matters in the wastewater through a photoelectrocatalysis reaction, and simultaneously recovering the silver ions in the wastewater.
The method applies the PFC system to the wastewater containing low-concentration silver ions and organic matters, realizes the degradation of pollutants and the synchronous recovery of the silver ions by utilizing the photoelectrocatalysis action of the PFC system, and improves the efficiency of degrading the organic matters and recovering the low-concentration silver ions by the PFC photoelectrocatalysis system.
In the embodiment of the invention, under the action of visible light, the photocatalytic fuel cell system generates photogenerated electrons and photogenerated holes with strong oxidizing property in wastewater containing low-concentration silver ions and organic matters, and the photogenerated holes can be mixed with OH or H2The O bonding generates hydroxyl radical with strong oxidizing property. The specific reaction mechanism is as follows:
under the action of visible light, the semiconductor bismuth vanadate photo-anode membrane electrode and the copper oxide/cuprous oxide heterojunction photo-cathode membrane electrode generate photo-generated holes and photo-generated electrons, wherein the photo-generated electrons generated by the anode are transmitted to the copper oxide/cuprous oxide heterojunction photo-cathode through an external circuit and are compounded with the holes, and the rest photo-generated electrons of the photo-cathode and silver ions undergo a reduction reaction, so that the recovery of the silver ions in the wastewater is realized. Meanwhile, the residual photo-generated holes or hydroxyl radicals of the photo-anode can perform catalytic oxidation reaction with organic matters, so that the degradation of the organic matters is realized. The silver recovered on the electrode also plays a certain role in strengthening the degradation of organic matters.
In another embodiment of the invention, the concentration of silver ions in the wastewater is less than 50 mg/L, and the concentration of organic matters is less than 10 mg/L.
Further, the organic matters in the wastewater comprise phenolic compounds, such as common disinfectant phenol and fine chemical intermediate p-nitrophenol. Furthermore, the organic matters in the wastewater also comprise diclofenac sodium and the like of anti-inflammatory analgesic.
Further, the silver ions in the wastewater come from silver nitrate and the like.
In an embodiment of the present invention, the time of the photoelectrocatalysis reaction is 120-240min, which may be 120min, 150min, 180min, 240 min.
In yet another embodiment of the present invention, the visible light is visible light with a wavelength greater than 420 nm.
The invention is further illustrated by the following specific examples.
Example 1 photocatalytic fuel cell system and method for recovering noble metal silver and degrading organic matters through photoelectrocatalysis thereof
A photocatalytic fuel cell photoelectrocatalysis system comprises a bismuth vanadate photo-anode membrane electrode, a copper oxide/cuprous oxide heterojunction photo-cathode membrane electrode and an electrolyte solution.
The preparation method of the bismuth vanadate anode comprises the steps of mixing a precursor bismuth oxyiodide deposition solution with 100M L of nitric acid aqueous solution containing 0.0075M bismuth nitrate and 0.4M sodium iodide and having the pH value of 1.2 with 45M L0.3.3M p-benzoquinone ethanol solution to prepare the bismuth oxyiodide electrode through an electrodeposition method, wherein the added voltage in the electrodeposition method is-0.1V, FTO is a working electrode, a counter electrode is a platinum wire, the reference electrode is a silver/silver chloride electrode, the bismuth oxyiodide electrode is immersed in 0.4M dimethyl sulfoxide solution of vanadyl acetylacetonate for 20 seconds, and then the obtained electrode is placed in a muffle furnace to be calcined at 450 ℃ for 1 hour to obtain the bismuth vanadate photo-anode membrane electrode.
The preparation method of the copper oxide/cuprous oxide heterojunction cathode comprises the following steps: the deposition solution of the precursor cuprous oxide was a mixed aqueous solution containing 0.48M copper sulfate and 3M sodium lactate. And (3) obtaining the cuprous oxide electrode by an electrodeposition method, wherein the applied voltage is-0.3V, the FTO glass is used as a working electrode, the counter electrode is a platinum wire, and the reference electrode is a calomel electrode. And then, putting the obtained electrode into a muffle furnace to calcine for 2 hours at the temperature of 400 ℃ to obtain the copper oxide/cuprous oxide heterojunction cathode.
The electrolyte is sodium sulfate, and the total concentration of the electrolyte in the wastewater is 100.0 mM.
The method for recovering the noble metal silver and degrading the organic matters by utilizing the photoelectrocatalysis of the photocatalysis fuel cell system comprises the following steps:
(1) a simulated wastewater of L m in volume containing 20 mg/L of silver nitrate and 5 mg/L of phenol was prepared as water to be treated, NaOH was added, and the initial pH was adjusted to 7.
(2) In the photoelectric reactor, a bismuth vanadate electrode is arranged as a membrane electrode photo-anode, and a copper oxide/cuprous oxide heterojunction electrode is arranged as a membrane electrode photo-cathode; visible light with the wavelength of more than 420nm is used as a photocatalytic light source, and the cathode and the anode are connected by a lead. Adding the prepared water to be treated into a photoelectric reactor, and adding 100mM sodium sulfate electrolyte; the electrochemical reaction time was 240 min.
(3) In the reaction, samples were taken every 60min, each time 1m L, then the water samples were pretreated, and the phenol degradation efficiency was determined by high performance liquid chromatography, 69.3%.
(4) In the reaction, samples were also taken every 60min, 2m L was taken each time, the water sample was filtered and subjected to ICP test, and the recovery rate of silver ions was determined to be 100%.
(5) Photoelectric property characterization of the electrode: and (5) carrying out scanning electron microscope test on the cathode and the anode after the silver is recovered.
Embodiment 2 a photocatalytic fuel cell system and a method for recovering noble metal silver and degrading organic matters through photoelectrocatalysis thereof
The preparation method of the photocatalytic system of the photocatalytic fuel cell is the same as that of example 1.
The method for recovering noble metal silver by photoelectrocatalysis and simultaneously degrading organic matters by utilizing the photocatalysis fuel cell system comprises the following steps of example 1, wherein the concentration of silver nitrate in the step (1) is 40 mg/L, and the degradation rate of final phenol and the recovery rate of silver ions are 83.7 percent and 100 percent respectively.
Claims (10)
1. A photocatalytic fuel cell system is characterized in that the photocatalytic fuel cell system comprises a bismuth vanadate photo-anode membrane electrode, a copper oxide/cuprous oxide heterojunction photo-cathode membrane electrode and an electrolyte solution; visible light with the wavelength of more than 420nm is used as a photocatalytic light source, and the cathode and the anode are connected by a lead.
2. The photocatalytic fuel cell system as set forth in claim 1, wherein the bismuth vanadate photoanode membrane electrode is obtained by first obtaining a bismuth oxyiodide electrode by electrodeposition, then soaking the obtained bismuth oxyiodide electrode in a dimethyl sulfoxide solution of vanadyl acetylacetonate, and calcining the soaked electrode in a muffle furnace.
3. A photocatalytic fuel cell system as in claim 2, characterized by that, the concentration of the dimethyl sulfoxide solution of vanadyl acetylacetonate is 0.2-0.5M and the soaking time is 10-30 seconds.
4. The photocatalytic fuel cell system as set forth in claim 2, wherein the calcination temperature in the muffle furnace is 400-500 ℃ and the calcination time is 0.8-1.2 h.
5. The photocatalytic fuel cell system as set forth in claim 1, wherein the copper oxide/cuprous oxide heterojunction photocathode membrane electrode is obtained by first obtaining a cuprous oxide electrode by electrodeposition, and then calcining the obtained cuprous oxide electrode in a muffle furnace.
6. The photocatalytic fuel cell system as set forth in claim 5, wherein the cuprous oxide electrode is calcined in a muffle furnace at a temperature of 350-450 ℃ for a time of 1.5-3 h.
7. A photocatalytic fuel cell system according to claim 1, characterized in that the electrolyte is sodium sulfate and the concentration of the electrolyte solution is 50.0-100.0 mM.
8. A method for recovering noble metal silver and degrading organic matters simultaneously through photoelectrocatalysis is characterized by comprising the following operation steps: the photocatalytic fuel cell system according to any one of claims 1 to 7 is added to a reactor for wastewater containing silver ions and organic substances, and a photoelectrocatalytic reaction is carried out under the action of visible light.
9. The method as claimed in claim 8, wherein the time of the photoelectrocatalytic reaction is 120-240 min.
10. The method for recovering the noble metal silver through the photoelectrocatalysis and degrading the organic matters as claimed in claim 8, wherein the concentration of the silver ions in the wastewater is less than 50 mg/L, and the concentration of the organic matters is less than 10 mg/L.
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