CN114016082A - Method for directly depositing and recovering metal bismuth on conductive substrate by utilizing solar energy - Google Patents
Method for directly depositing and recovering metal bismuth on conductive substrate by utilizing solar energy Download PDFInfo
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- CN114016082A CN114016082A CN202111324490.7A CN202111324490A CN114016082A CN 114016082 A CN114016082 A CN 114016082A CN 202111324490 A CN202111324490 A CN 202111324490A CN 114016082 A CN114016082 A CN 114016082A
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- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 32
- 239000000758 substrate Substances 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 title claims abstract description 21
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 16
- 239000002184 metal Substances 0.000 title claims abstract description 16
- 238000000151 deposition Methods 0.000 title claims abstract description 14
- 229910002915 BiVO4 Inorganic materials 0.000 claims abstract description 22
- 229910000416 bismuth oxide Inorganic materials 0.000 claims abstract description 3
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 25
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- AZQWKYJCGOJGHM-UHFFFAOYSA-N 1,4-benzoquinone Chemical compound O=C1C=CC(=O)C=C1 AZQWKYJCGOJGHM-UHFFFAOYSA-N 0.000 claims description 6
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 239000011521 glass Substances 0.000 claims description 6
- 239000012528 membrane Substances 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 4
- FSJSYDFBTIVUFD-SUKNRPLKSA-N (z)-4-hydroxypent-3-en-2-one;oxovanadium Chemical compound [V]=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O FSJSYDFBTIVUFD-SUKNRPLKSA-N 0.000 claims description 3
- 229910021607 Silver chloride Inorganic materials 0.000 claims description 3
- 230000002378 acidificating effect Effects 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 238000001354 calcination Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 239000003792 electrolyte Substances 0.000 claims description 3
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 3
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 claims description 3
- 239000010409 thin film Substances 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- FGHSTPNOXKDLKU-UHFFFAOYSA-N nitric acid;hydrate Chemical compound O.O[N+]([O-])=O FGHSTPNOXKDLKU-UHFFFAOYSA-N 0.000 claims 1
- 239000000126 substance Substances 0.000 abstract description 7
- 238000011084 recovery Methods 0.000 abstract description 5
- 238000002474 experimental method Methods 0.000 abstract description 2
- 238000005286 illumination Methods 0.000 abstract 1
- 239000010408 film Substances 0.000 description 14
- 238000004070 electrodeposition Methods 0.000 description 4
- 230000007613 environmental effect Effects 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229910017604 nitric acid Inorganic materials 0.000 description 3
- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- 238000006722 reduction reaction Methods 0.000 description 2
- 241000282414 Homo sapiens Species 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 239000003295 industrial effluent Substances 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000001055 reflectance spectroscopy Methods 0.000 description 1
- 238000000985 reflectance spectrum Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000005067 remediation Methods 0.000 description 1
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- C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
- C25C1/22—Electrolytic production, recovery or refining of metals by electrolysis of solutions of metals not provided for in groups C25C1/02 - C25C1/20
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- B01J23/20—Vanadium, niobium or tantalum
- B01J23/22—Vanadium
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Abstract
Hair brushThe invention relates to a method for directly depositing and recovering metal bismuth on a conductive substrate by utilizing solar energy. The technical scheme is as follows: KOH solution is added into the anode chamber at the upper layer of the I-shaped electrolytic cell device, and acidified Bi (NO) is added into the cathode chamber at the lower layer3)3A solution; BiVO (bismuth oxide) is added4A photoelectrode is used as an anode and is arranged in the anode chamber, a conductive substrate is used as a cathode and is arranged in the cathode chamber, and a lead is used for leading the BiVO4The photoelectrode is connected with the conductive substrate; direct irradiation of BiVO with sunlight4Photoelectrode for 30 minutes. Through experiments, elemental bismuth is found to be deposited on the conductive substrate of the cathode chamber after illumination. The method for directly utilizing solar energy and directly depositing the bismuth simple substance without the help of external voltage can realize the storage of solar energy and the recovery of bismuth metal.
Description
Technical Field
The invention relates to a method for depositing metal bismuth on a cathode conductive substrate by irradiating a light anode by using solar energy, and further recycling the metal bismuth. The method uses semiconductor material BiVO4As an anode, BiVO was irradiated with sunlight4The film can reduce metal bismuth on the cathode conductive substrate without external voltage. The method for depositing the metal bismuth only by utilizing the solar energy can convert the solar energy into the chemical energy, and realize the long-term storage of the solar energy and the recovery of the metal bismuth.
Background
In recent years, the economic society and science of human beings are continuously developed, nonferrous metals and mineral resources rich in bismuth are continuously reduced, and therefore, the recovery of bismuth from secondary resources of bismuth is gradually an important source of bismuth. The recovery of metals from industrial effluents by means of electrodeposition is now in use on the market, but is accompanied by the problem of high energy consumption associated with electrodeposition. The solar energy has the advantages of universality, harmlessness, inexhaustibility and the like, can ensure the sustainable economic growth and meet the requirement of environmental protection, and is a potential solution for relieving energy shortage and realizing environmental remediation. The semiconductor catalyst with the photocatalytic function can convert solar energy, has the advantages of no toxicity, environmental friendliness, stability, high efficiency and the like, has a good prospect in the aspect of energy conversion, and has three basic processes: 1) the energy of the exciting light is larger than the band gap of the semiconductor material; 2) separating photon-generated carriers; 3) the separated photoproduction holes are subjected to oxidation reaction, and photoproduction electrons can enter a cathode through an external circuit to be subjected to reduction reaction. The method for directly depositing the bismuth metal on the cathode by utilizing the solar energy through the mechanism has practical significance.
Disclosure of Invention
The invention aims to use a semiconductor material BiVO with good photocatalytic performance under the conditions of no external voltage, only using solar energy and not consuming other energy4As an anode, under the irradiation of sunlight, metal bismuth is deposited on a cathode, and the method can realize the conversion from solar energy to chemical energy and is applied to the recovery of heavy metals in industrial wastewater.
The technical scheme adopted by the invention is as follows: a method for directly depositing and recovering metal bismuth on a conductive substrate by utilizing solar energy comprises the following steps:
1) KOH solution is added into the anode chamber at the upper layer of the I-shaped electrolytic cell device, and acidified Bi (NO) is added into the cathode chamber at the lower layer3)3A solution;
2) BiVO (bismuth oxide) is added4A photoelectrode is used as an anode and is arranged in the anode chamber, a conductive substrate is used as a cathode and is arranged in the cathode chamber, and a lead is used for leading the BiVO4The photoelectrode is connected with the conductive substrate;
3) direct irradiation of BiVO with sunlight4Photoelectrode for 30 minutes.
Preferably, the concentration of the KOH solution is 1 mol/L.
Preferably, the acidified Bi (NO)3)3The preparation method of the solution comprises the following steps: adding Bi (NO)3)3·5H2Dissolving O in acidic aqueous solution with the volume ratio of concentrated nitric acid to water being 1.1:24, and stirring until the solution is clear and transparent to obtain acidified Bi (NO) with the concentration of 0.25mol/L3)3And (3) solution.
Preferably, the BiVO4The preparation method of the photoelectrode comprises the following steps: mixing KI and Bi (NO)3)3·5H2Adding O into deionized water, stirring, and regulating the obtained mixtureAfter the pH value of the solution is 1.5-2.0, dropwise adding an ethanol solution of p-benzoquinone, uniformly mixing to obtain an electrolyte, taking conductive glass FTO as a working electrode, Ag/AgCl as a reference electrode and a platinum wire as a counter electrode, and depositing for 3-5 minutes under the bias voltage of-0.1-0.15V to form a BiOI layer on the conductive glass FTO of the working electrode; dropwise adding a dimethyl sulfoxide solution of vanadyl acetylacetonate onto the formed BiOI layer, calcining the BiOI layer for 2 hours at 350-550 ℃ in a muffle furnace, and converting the BiOI into BiVO4After cooling to room temperature, the mixture was immersed in NaOH solution to remove excess V2O5Finally, washing with deionized water and drying to obtain BiVO with the surface covered with BiVO4BiVO of thin film4And a photoelectrode.
Preferably, the bottom of the connecting pipeline between the anode chamber at the upper layer and the cathode chamber at the lower layer is provided with a proton membrane.
Preferably, the intensity of sunlight is 100mW cm-2。
Compared with the prior art, the invention has the beneficial effects that:
1. the solar energy-saving solar photovoltaic power generation system only utilizes solar energy, does not need external voltage, and accords with the concepts of energy conservation, emission reduction and environmental protection.
2. The invention can deposit bismuth metal on the cathode by only utilizing solar energy, and is a method capable of storing solar energy for a long time and recovering metal bismuth.
Drawings
FIG. 1 is BiVO4BiVO on photoelectrode4Scanning electron microscope images of the film (a) and the bismuth simple substance (b).
FIG. 2 is BiVO4BiVO on photoelectrode4XRD patterns of the film (a) and the bismuth simple substance (b).
FIG. 3 is BiVO4BiVO on photoelectrode4Ultraviolet-visible diffuse reflectance spectrum of the film.
Figure 4a is a photochemical cell performance test.
Fig. 4b is a comparison of the cathode conductive substrate before and after the experiment.
FIG. 5 is a schematic structural view of an I-shaped electrolytic cell device.
Detailed Description
Example 1 a method for recovering metallic bismuth by direct deposition on a conductive substrate using solar energy
The method comprises the following steps
1)BiVO4Preparing a photoelectrode:
20mmol KI and 2mmol Bi (NO)3)3·5H2Adding O into 50mL of deionized water, stirring uniformly, adjusting the pH of the obtained mixed solution to about 1.7 by using a small amount of dilute nitric acid, and then dropwise adding 20mL of 0.23mol/L ethanol solution of p-benzoquinone to obtain the electrolyte. And (2) taking the conductive glass FTO as a working electrode, Ag/AgCl as a reference electrode and a platinum wire as a counter electrode, and carrying out electro-deposition for 5 minutes by adopting an electrochemical deposition method under the bias voltage of-0.12V to obtain a BiOI layer on the conductive glass FTO of the working electrode. 0.15mL of dimethyl sulfoxide containing 0.2M vanadyl acetylacetonate was added dropwise to the electrodeposited BiOI layer, followed by calcination at 450 ℃ for 2h in a muffle furnace to convert the BiOI to BiVO4. BiVO to be formed4After cooling the electrode to room temperature, it was immersed in 1M NaOH for about 30min to remove excess V2O5Finally, washing the membrane by deionized water and drying the membrane to obtain the membrane coated with BiVO4BiVO of film (3-1)4A photoelectrode (3).
2) Preparation of photochemical cell-I-shaped electrolytic cell device
The structure of the I-shaped electrolytic cell device is shown in figure 5.
50mL of KOH solution with the concentration of 1mol/L is added into the anode chamber (1-1) at the upper layer of the I-shaped electrolytic cell device (1).
Adding acidified Bi (NO) with concentration of 0.25mol/L into cathode chamber (1-2) at lower layer of I-shaped electrolytic cell device (1)3)3Solution (6.06 g of Bi (NO)3)3·5H2O was dissolved in an acidic aqueous solution at a volume ratio of concentrated nitric acid to water of 1.1:24 to prepare a 50ml solution, and the solution was stirred until it was clear and transparent).
The bottom of a connecting pipeline between the anode chamber (1-1) and the cathode chamber (1-2) is provided with a proton membrane (2).
The surface is covered with BiVO4BiVO of film (3-1)4The photoelectrode (3) is used as an anode and is arranged in the anode chamber (1-1).
A pure FTO conductive substrate (4) was placed in the cathode chamber (1-2) as a cathode.
BiVO is connected with a lead (5)4The photoelectrode and the FTO conductive substrate are connected.
3) Depositing bismuth metal
The light intensity is 100mW cm-2Simulated solar light irradiation BiVO4And depositing a bismuth simple substance on the conductive substrate of the cathode for 30 minutes.
(II) Performance testing
1) Scanning electron microscope
BiVO prepared4Respectively scanning elementary bismuth deposited on the photoelectrode and cathode conductive substrate by using an electron microscope, and carrying out BiVO4BiVO on photoelectrode4And (5) characterizing the shapes of the film and the simple substance bismuth. The results are shown in FIG. 1.
As can be seen from a of FIG. 1, BiVO was prepared4Photoelectrode, BiVO can be seen4The film is a three-dimensional network structure composed of irregular particles. As can be seen from b in FIG. 1, the deposited elemental bismuth has a curled sheet-like structure.
2) XRD test
For BiVO4The films and deposits were characterized and the results are shown in FIG. 2.
For BiVO as shown in a in FIG. 24The film is characterized, BiVO4The film had diffraction peaks mainly at 28.8 °, 30.6 °, 34.5 °, 39.8 °, 42.5 °, 46.0 °, 53.2 °, and 58.5 °, and the diffraction peaks of the sample corresponded to the (-121), (040), (200), (211), (051), (132), (-161), and (321) diffraction planes of the bismuth orthovanadates (JCPDS 14-0688), respectively.
The deposited metal was characterized and the results are shown in figure 2 b. The deposits have diffraction peaks mainly at 22.5 °, 23.8 °, 27.2 °, 37.9 °, 39.6 °, 48.7 °, 62.2 °, 64.5 °, and 70.8 °, which correspond to the (003), (101), (012), (104), (110), (202), (116), (122), and (214) diffraction planes of bismuth (JCPDS-No.05-0519), respectively.
3) Ultraviolet-visible diffuse reflectance spectroscopy detection
The ultraviolet-visible diffuse reflection test was performed on the bismuth vanadate film, and the results are shown in fig. 3.
As can be seen from fig. 3, the bismuth vanadate film starts to absorb light at a wavelength of about 500nm, i.e., absorbs both ultraviolet light and visible light.
4) Photochemical cell performance testing
The bismuth vanadate films were tested and the results are shown in FIGS. 4a and 4 b. FIG. 4a is BiVO4And the photoelectrode is an I-t characteristic curve measured when the metal bismuth is deposited under the simulated sunlight irradiation. As can be seen from FIG. 4a, BiVO is irradiated under simulated sunlight4In the case of thin films, BiVO in the first 900s4The current density of the photoelectrode is from 0.8mA/cm2Reduced to 0.05mA/cm2And subsequently tends to stabilize. Fig. 4b is a front and back comparison graph on a cathode conductive substrate under the condition that simulated sunlight irradiates a BiVO4 photoelectrode for 30 minutes. As can be seen from fig. 4b, after 30 minutes, elemental bismuth is precipitated on the conductive substrate of the cathode.
Claims (6)
1. A method for directly depositing and recovering metal bismuth on a conductive substrate by utilizing solar energy is characterized by comprising the following steps:
1) KOH solution is added into the anode chamber at the upper layer of the I-shaped electrolytic cell device, and acidified Bi (NO) is added into the cathode chamber at the lower layer3)3A solution;
2) BiVO (bismuth oxide) is added4A photoelectrode is used as an anode and is arranged in the anode chamber, a conductive substrate is used as a cathode and is arranged in the cathode chamber, and a lead is used for leading the BiVO4The photoelectrode is connected with the conductive substrate;
3) direct irradiation of BiVO with sunlight4Photoelectrode for 30 minutes.
2. The method of claim 1, wherein the concentration of the KOH solution is 1 mol/L.
3. The method of claim 1, wherein the acidified Bi (NO) is3)3The preparation method of the solution comprises the following steps: adding Bi (NO)3)3·5H2Dissolving O in concentrated nitric acid (water) in volume ratio1.1:24 in an acidic aqueous solution, and stirring until the solution is clear to obtain acidified Bi (NO) with the concentration of 0.25mol/L3)3And (3) solution.
4. The method of claim 1, wherein the BiVO is4The preparation method of the photoelectrode comprises the following steps: mixing KI and Bi (NO)3)3·5H2And adding O into deionized water, uniformly stirring, adjusting the pH of the obtained mixed solution to 1.5-2.0, dropwise adding an ethanol solution of p-benzoquinone, and uniformly mixing to obtain the electrolyte. Depositing for 3-5 minutes under the bias voltage of-0.1-0.15V by taking conductive glass FTO as a working electrode, Ag/AgCl as a reference electrode and a platinum wire as a counter electrode, and forming a BiOI layer on the conductive glass FTO of the working electrode; dropwise adding a dimethyl sulfoxide solution of vanadyl acetylacetonate onto the formed BiOI layer, calcining the BiOI layer for 2 hours at 350-550 ℃ in a muffle furnace, and converting the BiOI into BiVO4After cooling to room temperature, the mixture was immersed in NaOH solution to remove excess V2O5Finally, washing with deionized water and drying to obtain BiVO with the surface covered with BiVO4BiVO of thin film4And a photoelectrode.
5. The method according to claim 1, wherein a proton membrane is provided at the bottom of the connecting pipe between the anode chamber of the upper layer and the cathode chamber of the lower layer.
6. The method of claim 1, wherein the solar light intensity is 100 mW-cm-2。
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| JP2001172731A (en) * | 1999-12-14 | 2001-06-26 | Nippon Mining & Metals Co Ltd | Method for recovering bismuth |
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| JP2019203199A (en) * | 2019-07-23 | 2019-11-28 | Ｊｘ金属株式会社 | Electrolytic method of bismuth |
| CN112410819A (en) * | 2020-11-10 | 2021-02-26 | 北京化工大学 | Composite bismuth-based photoanode for photoelectrocatalytic decomposition of water and preparation method thereof |
| CN113502513A (en) * | 2021-08-12 | 2021-10-15 | 辽宁大学 | Method for directly depositing copper metal by utilizing solar energy |
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| JP2001172731A (en) * | 1999-12-14 | 2001-06-26 | Nippon Mining & Metals Co Ltd | Method for recovering bismuth |
| CN108149020A (en) * | 2018-01-12 | 2018-06-12 | 四川大学 | The technique for preparing bismuth using zinc anode sludge waste residue |
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