CN112759035A - Resource recovery mobile photoelectrochemical system in high-salinity wastewater - Google Patents

Resource recovery mobile photoelectrochemical system in high-salinity wastewater Download PDF

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CN112759035A
CN112759035A CN202110033939.8A CN202110033939A CN112759035A CN 112759035 A CN112759035 A CN 112759035A CN 202110033939 A CN202110033939 A CN 202110033939A CN 112759035 A CN112759035 A CN 112759035A
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wastewater
photoelectrochemical
cbz
photoelectrochemical system
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CN112759035B (en
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何小松
崔骏
席北斗
邓雪娇
涂响
裴元生
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Chinese Research Academy of Environmental Sciences
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    • 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
    • C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
    • 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
    • C02F2101/10—Inorganic compounds
    • C02F2101/20—Heavy metals or heavy metal compounds
    • 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
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2201/00—Apparatus for treatment of water, waste water or sewage
    • C02F2201/46—Apparatus for electrochemical processes

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Abstract

A mobile photoelectrochemical system for resource recovery in high-salinity wastewater. The invention provides a flow type photoelectrochemical system for synchronously degrading organic matters and recovering heavy metals by utilizing high-salinity wastewater and an application method thereof.

Description

Resource recovery mobile photoelectrochemical system in high-salinity wastewater
Technical Field
The invention belongs to the technical field of wastewater reclamation, and relates to a visible light driven flow type photoelectrochemical (FPEC) system, a method for degrading organic matters in high-salt wastewater and recovering heavy metals and electric energy and application thereof.
Background
The imbalance development between economy and resources leads to the attention of resource technology. The wastewater contains abundant organic matters and metal ions and is a potential resource. The process of recycling waste water is accompanied with energy consumption. Solar energy is used as a green energy source and can be continuously converted into driving force for recycling wastewater. However, the light-driven wastewater recycling technology is limited due to the limitations of low photoelectric conversion efficiency, unclear mechanism and the like.
The treatment of high-salinity wastewater has been a difficult point in the field of water treatment. The electrochemical treatment technology is widely used for treating high-salinity and high-organic wastewater. However, inorganic ions mainly containing chloride ions are liable to damage the structure of the surface film layer of the metal electrode, resulting in reduced stability of the electrode, poor quality of effluent water, and increased cost for treating ton waste water. The destruction of the film structure is mainly due to electron transfer at the interface between the metal electrode and the corrosive medium. In a photoelectrochemical system, under the illumination condition, the surface of a photoanode can generate photoproduction electrons and holes, and the photoelectrochemical system structure can promote the migration of the photoproduction electrons between the photoanode and a cathode, improve the directional transfer capability and the comprehensive utilization efficiency of the photoproduction electrons and ensure the stability of the cathode. The electrons can effectively collect electric energy in the directional transmission process of the external circuit, and can be secondarily utilized. In addition, the photo-generated electrons generated on the surface of the photoanode can be used for reduction and recovery of heavy metal ions in the solution. Meanwhile, the cavity generated on the surface of the photo-anode can promote the generation of high-activity free radicals and promote the degradation of coexisting organic matters. Therefore, the construction of the wastewater resource recycling technology based on the photoelectrochemical system has important research value.
The invention constructs the FPEC system on the basis of the photoelectrochemistry system, improves the continuous operation capability of the photoelectrochemistry system, realizes the aims of continuously degrading organic matters and recovering electric energy and heavy metals in a high-salinity wastewater environment, and provides theoretical reference and technical support for the light-driven wastewater recycling technology.
Disclosure of Invention
Based on the technical background, the inventor of the invention has made a sharp approach, and provides a flow-type photoelectrochemical system with a resource recovery function for high-salt wastewater treatment, which comprises a photoelectrochemical reactor and a water circulation system, wherein the photoelectrochemical reactor comprises a photoanode, a metal cathode, an external circuit and a water cooling circulation system.
The invention provides a flowing type photoelectrochemical system with a resource recovery function in high-salinity wastewater, which comprises the following components in part by weight: the device comprises a photoelectrochemical reactor and a water circulation system, wherein the photoelectrochemical reactor comprises a photoanode, a metal cathode, an external circuit and the water circulation system.
The second aspect of the invention provides a use of the flow-type photoelectrochemical system with the resource recovery function according to the first aspect of the invention for wastewater treatment.
The third aspect of the present invention provides a method for wastewater treatment and electric energy recovery using the flow-type photoelectrochemical system having the resource recovery function according to the first aspect of the present invention, the method comprising the steps of:
step 1, placing wastewater to be treated in a photoelectrochemical system;
and 2, setting treatment conditions for treatment.
The resource recovery flow type photoelectrochemical system in the high-salinity wastewater provided by the invention has the following advantages:
(1) the mobile photoelectrochemical system with the resource recovery function in the high-salinity wastewater does not need external energy input, and only needs to be driven by visible light to realize the conversion from solar energy to electric energy;
(2) the flowing type photoelectrochemical system with the resource recovery function in the high-salinity wastewater has the advantages of strong stability, lower cost and better effluent quality;
(3) the mobile photoelectrochemical system with the resource recovery function in the high-salinity wastewater has an excellent wastewater treatment effect, realizes metal recovery while improving the organic matter degradation efficiency, and has strong power generation capacity and long-term stable operation capacity.
Drawings
FIG. 1 shows a mechanism diagram of a resource recovery flow type photoelectrochemical system in high salinity wastewater according to the present invention;
FIG. 2 is a diagram of an experimental apparatus of a mobile photoelectrochemical system for resource recovery from high salinity wastewater according to the present invention;
FIG. 3 shows CBZ and Cu under long term operating conditions for example 6 of the present invention2+A graph of concentration change of (c);
FIG. 4 is a graph showing the change of current and voltage with time under a long-term operation condition in example 6 of the present invention;
FIG. 5-a shows a scanning electron micrograph of the surface of an original 304 stainless steel electrode used in example 6 of the present invention;
FIG. 5-b shows a scanning electron micrograph of an unprotected 304 stainless steel electrode surface under long-term operating conditions of example 6 of the present invention;
FIG. 5-c shows SEM pictures of the surface of a 304 stainless steel electrode protected under long-term operating conditions in example 6 of the present invention;
FIG. 5-d shows a SEM of the surface of a 304 stainless steel electrode after the surface precipitates are removed under long-term operating conditions in example 6 of the present invention;
fig. 6 shows a photograph of the surface of cathode 304 stainless steel under long-term treatment conditions of comparative example 13 of the present invention.
Description of the reference numerals
2-a light source;
3-a water circulation system;
4-a quartz window;
6-a photoanode;
7-a metal cathode;
8-an external circuit;
9-a photoelectrochemical reactor;
10-water cooling circulation system.
Detailed Description
The present invention will be described in detail below, and features and advantages of the present invention will become more apparent and apparent with reference to the following description.
The first aspect of the present invention provides a mobile photoelectrochemical system having a resource recovery function, the photoelectrochemical system comprising: a photoelectrochemical reactor 9 and a water circulation system 3, wherein the photoelectrochemical reactor 9 comprises a light source 2, a photoanode 6, a metal cathode 7, an external circuit 8 and a water circulation system 10.
The photo-anode 6, the metal cathode 7 and the water-cooling circulation system 10 are located inside the photoelectrochemical reactor 9, one end of the external circuit 8 is connected with the photo-anode 6, the other end of the external circuit is connected with the metal cathode 7, and the water-cooling circulation system 10 is installed along the inner wall of the side edge of the photoelectrochemical reactor 9 to form a loop, as shown in fig. 2. The water circulation system 3 is located outside the photoelectrochemical reactor 9 and is communicated with two ends of the photoelectrochemical reactor 9, as shown in fig. 2.
In the invention, the water circulation system is a photoelectrochemical reactor for conveying wastewater, the wastewater is treated in the photoelectrochemical reactor and flows out of the photoelectrochemical reactor through the water circulation system, the water circulation system comprises a pipeline and a water storage tank, the pipeline is used for conveying the wastewater, and the water storage tank is used for storing.
In order to ensure that the flowing type photoelectrochemical system with the resource recovery function can normally operate, the photoelectrochemical reactor also comprises a light-transmitting quartz window 4. The light-transmitting quartz window 4 is positioned on one side of the photo-anode 6, the light source 2 is positioned outside the photoelectrochemical reactor 9, and the quartz window 4 is positioned between the photo-anode 6 and the light source 2.
According to the invention, visible light passes through the light-transmitting quartz window to excite the light-generated anode to generate photo-generated electrons and holes so as to excite the operation of the whole system.
In the practical application process of the photoelectrochemical system, external energy input is not needed, and degradation of organic matters and metal recovery can be realized only by means of visible light.
The photo-anode is a photo-anode with strong photoresponse sensitivity, and according to a preferred embodiment of the invention, the photo-anode is selected from one or more of titanium dioxide, carbon quantum dots, ferric oxide, tungsten oxide, molybdenum disulfide, vanadium bismuth tetroxide and Mxene, but is not limited to the above materials, preferably selected from one or more of titanium dioxide, carbon quantum dots, tungsten oxide, molybdenum disulfide and Mxene, and more preferably selected from one or more of titanium dioxide, carbon quantum dots, tungsten oxide and molybdenum disulfide.
The carbon quantum dots are a novel carbon-based zero-dimensional material, have excellent optical properties, good water solubility, low toxicity and environmental friendliness, and simultaneously have the advantages of wide raw material source, low cost, good biocompatibility and the like.
In the invention, the carbon quantum dots are used as the photo-anode material, so that the photoelectrochemical system has the advantages of low cost, environmental friendliness and the like, and tests show that the photoelectrochemical system can effectively remove organic pollutants and improve the recovery and the electricity generation quantity of metals. Meanwhile, the photo-anode has high photo-current density under the illumination condition, and the photo-current density is 50-120 mu A/cm2。
According to the invention, the metal cathode is selected from stainless steel, aluminum alloy, carbon steel, brass, nickel-based material or platinum sheet, but is not limited to the above materials, preferably from stainless steel, carbon steel, brass or platinum sheet, and more preferably from stainless steel or platinum sheet.
The metal cathode of different materials can influence the effect of photoelectrochemistry system to the treatment of waste water, metal recovery efficiency and power generation volume, and the inventor finds that the metal cathode of chooseing for use above-mentioned material especially chooses stainless steel and platinum sheet for use as the metal cathode can effectively improve the degradation efficiency to organic matter in the waste water, improves the recovery efficiency and the power generation volume of metal simultaneously.
The external circuit comprises a lead for connecting the photo-anode and the metal cathode, and as shown in fig. 2, the length of the lead is 1-30 cm, preferably 2-20 cm, and more preferably 4-10 cm.
The length of the lead has an influence on the electricity generation quantity of the photoelectrochemical system, particularly has a remarkable influence on the degradation efficiency of organic matters and the metal recovery rate, the degradation efficiency of the organic matters in the wastewater can be reduced due to the fact that the lead is too short, the metal recovery efficiency in the wastewater to be treated can be reduced if the lead is too long, and the electricity generation quantity of the photoelectrochemical system can be reduced due to the fact that the lead is too long or too short.
The wire is made of four-iron four-aluminum, copper-clad aluminum, high-conductivity aluminum, copper-clad silver, bronze, oxygen-free copper, brass, red copper or tinned copper, preferably four-iron four-aluminum, high-conductivity aluminum, copper-clad silver, brass, red copper or tinned copper, and more preferably high-conductivity aluminum, brass or tinned copper.
The technical principle of the flowing type photoelectrochemical system with the resource recovery function provided by the invention is as follows: under the excitation of visible light, a photoelectrochemical system introduced into the wastewater to be treated generates photo-generated electrons and holes, the holes react with water to generate high-activity free radicals for removing organic pollutants in the high-salinity wastewater, the photo-generated electrons are transferred to the surface of a metal cathode from the photo-anode through an external circuit, one part of electrons are used as electron donors and are used for recovering metals, the other part of electrons are used as electron donors and are reacted with chloride ions in the wastewater to show the protection effect of the photo-generated cathode, the photo-generated cathode is used for the stability of the system, and meanwhile, electric energy can be recovered through the external circuit. The technical schematic diagram is shown in fig. 1.
The mobile photoelectrochemical system with the resource recovery function has high organic matter degradation efficiency and heavy metal ion recovery efficiency in wastewater, the organic matter degradation efficiency is 60-90%, the heavy metal ion recovery efficiency is 30-70%, and meanwhile, the mobile photoelectrochemical system with the resource recovery function has the advantages thatHigher electricity generation amount can be realized in the wastewater treatment, and the electricity generation amount is 40-70W/(m)3Solution x m2Electrode area).
Due to the introduction of the photo-generated cathodic protection concept, the photoelectrochemical system can keep stable operation for a long time, namely, the high-salinity wastewater can be efficiently treated for a long time, and the treatment time can exceed 48 hours. After the wastewater is treated for 48 hours, the degradation efficiency of CBZ in the wastewater is 49-80%, the recovery efficiency of heavy metal ions is 6-20%, and the electricity generation amount can still reach 25-50W/(m)3Solution x m2Electrode area).
The second aspect of the invention provides a use of the flow-type photoelectrochemical system with resource recovery function according to the first aspect of the invention for wastewater treatment, particularly for high-salinity wastewater treatment, for example, it can be used for the treatment and resource recovery of copper-containing wastewater, landfill leachate and the like in the pharmaceutical industry.
The third aspect of the present invention provides a method for wastewater treatment and electric energy recovery using the flow-type photoelectrochemical system having the resource recovery function according to the first aspect of the present invention, the method comprising the steps of:
step 1, placing wastewater to be treated in a photoelectrochemical system;
and 2, setting treatment conditions for treatment.
This step is specifically described and illustrated below.
Step 1, placing wastewater to be treated in a photoelectrochemical system.
In step 1 of the present invention, wastewater to be treated is first placed in a photoelectrochemical system, which is preferably a flow-type photoelectrochemical system having a resource recovery function according to the first aspect of the present invention, and the photoelectrochemical system includes: the device comprises a photoelectrochemical reactor and a water circulation system, wherein the photoelectrochemical reactor comprises a light source, a photoanode, a metal cathode, an external circuit and the water circulation system.
The photo-anode, the metal cathode and the water-cooling circulating system are located inside the photoelectrochemical reactor, one end of an external circuit is connected with the photo-anode, the other end of the external circuit is connected with the metal cathode, and the water-cooling circulating system is installed along the inner wall of the side edge of the photoelectrochemical reactor to form a loop. The water circulation system is positioned outside the photoelectrochemical reactor and communicated with two ends of the photoelectrochemical reactor.
The photoelectrochemical reactor also included a light transmissive quartz window. The light-transmitting quartz window is positioned on one side of the photo-anode, the light source is positioned on the outer side of the photoelectrochemical reactor, and the quartz window is positioned between the photo-anode and the light source.
In the wastewater treatment process, the water circulation system conveys wastewater to the photoelectrochemical reactor, so that the photoanode and the metal cathode are immersed in the wastewater, the visible light penetrates through the quartz window to excite the photoanode, so that the wastewater is treated in the photoelectrochemical reactor, and then the wastewater flows out of the photoelectrochemical reactor through the water circulation system.
The driving force of the photoelectrochemical system is visible light, and the photoanode generates photo-generated electrons and holes under the excitation of the visible light so as to trigger the operation of the whole system.
According to a preferred embodiment of the present invention, the photo-anode is selected from one or more of titanium dioxide, carbon quantum dots, ferric oxide, tungsten oxide, molybdenum disulfide, vanadium bismuth tetroxide and Mxene, but not limited to the above materials, preferably selected from one or more of titanium dioxide, carbon quantum dots, tungsten oxide, molybdenum disulfide and Mxene, and more preferably selected from one or more of titanium dioxide, carbon quantum dots, tungsten oxide and molybdenum disulfide.
The metal cathode is selected from stainless steel, aluminum alloy, carbon steel, brass, nickel-based material or platinum sheet, but is not limited to the above materials, preferably selected from stainless steel, carbon steel, brass or platinum sheet, and more preferably selected from stainless steel or platinum sheet.
The external circuit comprises a lead for connecting the photo-anode and the metal cathode, wherein the length of the lead is 1-30 cm, the preferred length of the lead is 2-20 cm, and the more preferred length of the lead is 4-10 cm.
The wire is made of four-iron four-aluminum, copper-clad aluminum, high-conductivity aluminum, copper-clad silver, bronze, oxygen-free copper, brass, red copper or tinned copper, preferably four-iron four-aluminum, high-conductivity aluminum, copper-clad silver, brass, red copper or tinned copper, and more preferably high-conductivity aluminum, brass or tinned copper.
Experiments show that the concentration of organic matters, the concentration of heavy metal ions and the concentration of salt in the wastewater to be treated all influence the treatment effect of the photoelectrochemical system, and in order to ensure good treatment effect, the wastewater to be treated can be diluted first, so that the concentration of the organic matters and the concentration of the heavy metal ions in the wastewater to be treated are reduced.
The concentration of organic matters in the wastewater to be treated is 0.1-20 mol/L, preferably 0.3-15 mol/L, and more preferably 0.5-10 mol/L.
The inventor finds that the concentration of organic matters in the wastewater is related to the treatment effect of the photoelectrochemical system on the wastewater in the test process, the high concentration of the organic matters can reduce the degradation efficiency of the photoelectrochemical system on the organic matters, the recovery efficiency and the electricity generation quantity of metal ions are improved along with the increase of the concentration of the organic matters, but the recovery efficiency and the electricity generation quantity of the metal ions can be inhibited if the concentration of the organic matters is too high.
Therefore, in order to ensure the treatment effect of the wastewater to be treated, the wastewater can be diluted to the above concentration range, and the photoelectrochemical system provided by the invention has a better treatment effect on the wastewater with the above concentration range.
The concentration of the heavy metal ions is 0.01-5 mol/L, preferably 0.05-2 mol/L, and more preferably 0.1-1 mol/L.
The influence of the concentration of the heavy metal ions on the degradation efficiency of the organic matters in the wastewater is small, the improvement of the concentration of the heavy metal ions can improve the degradation efficiency of the organic matters in the wastewater to a small extent, but the influence on the degradation efficiency and the power generation quantity of the heavy metal ions in the wastewater is large, the concentration of the heavy metal ions is higher, the power generation quantity is greatly improved, and meanwhile, the recovery efficiency of the heavy metal ions can be obviously reduced. When the wastewater is diluted to the range of the concentration of the heavy metal ions, the photoelectrochemical system has higher degradation efficiency of organic matters in the wastewater and recovery efficiency of the heavy metal ions, and has higher electricity production.
The salinity concentration of the wastewater to be treated is 0.05-5%, the preferable salinity concentration is 0.1-4%, and the more preferable salinity concentration is 0.3-2%.
Too high salt concentration in the wastewater can reduce the organic matter degradation efficiency, metal ion recovery efficiency and electricity generation quantity of the photoelectrochemical system in the wastewater.
And 2, setting treatment conditions for treatment.
After the wastewater to be treated is placed in a photoelectrochemical system, corresponding treatment conditions are set for wastewater treatment.
The treatment conditions of the invention are that the treatment is carried out under the illumination: the illumination conditions are as follows: 1 to 3 sunlight, preferably 1 to 2 sunlight, and more preferably 1 sunlight.
The visible light is used as an excitation light source in the invention, so that the system can operate without inputting external energy, thereby realizing the degradation and metal recovery of organic matters in the wastewater and simultaneously converting the light energy into electric energy.
Under the illumination condition, the photocurrent density generated by the photoanode is 20-150 muA/cm2Preferably, the photocurrent density is 50-120 muA/cm2More preferably, the photocurrent density is 70 to 110 μ A/cm2。
The flow rate of the wastewater conveyed by the water circulation system, namely the flow rate of the wastewater in the photoelectrochemical system is 1-10 mL/min, preferably 3-7 mL/min, and more preferably 5 mL/min.
The photoelectrochemical system can realize long-term stable operation in wastewater, after the photoelectrochemical system is operated and treated for 48 hours, the degradation efficiency of the photoelectrochemical system on CBZ in the wastewater is 49-80%, the recovery efficiency of heavy metal ions is 6-20%, and the electricity generation amount can still reach 25-50W/(m3Solution x m2Electrode area).
The invention has the following beneficial effects:
(1) the flowing type photoelectrochemical system with the resource recovery function in the high-salinity wastewater does not need external energy input, the driving force for degrading organic matters and recovering heavy metals of the system is visible light, and meanwhile, the electric energy can be recovered through an external circuit while the directional movement of electrons is strengthened, so that the conversion from solar energy to electric energy is realized;
(2) the mobile photoelectrochemical system with the resource recovery function in the high-salinity wastewater has strong stability, and chloride ions in the high-salinity wastewater have the capacity of destroying the surface film structure of the metal electrode, so that the stability of the electrode is reduced, the quality of effluent water is poor, and the treatment cost per ton of wastewater is increased. By constructing the FPEC system and introducing a photoproduction cathodic protection concept, the directional movement of photoproduction electrons is strengthened, the photoproduction cathodic protection capability of a photoanode is improved, and the stable operation of the FPEC system in a high-salt environment is ensured;
(3) the mobile photoelectrochemical system with the resource recovery function in the high-salinity wastewater has high degradation efficiency on organic matters in the wastewater, the degradation efficiency on the organic matters can reach 60-90%, and the recovery efficiency on heavy metal ions is 30-70%;
(4) the mobile photoelectrochemical system with the resource recovery function in the high-salinity wastewater can realize higher electricity generation amount in the wastewater treatment process, and the electricity generation amount is 40-70W/(m)3Solution x m2Electrode area).
Examples
The invention is further illustrated by the following specific examples, which are intended to be illustrative only and not limiting to the scope of the invention.
Example 1
The photoanode shown in FIG. 2 is titanium dioxide, carbon quantum dots and tungsten oxide, the metal cathode is Pt (platinum), the length of the wire (made of brass) is 5cm, the resource recovery flow type photoelectrochemical system with a light-transmitting quartz window is used for treating organic matters (carbamazepine, CBZ) with the concentration of 5mol/L and heavy metals (Cu)2+) High salinity wastewater (solution volume 1L) with concentration of 0.5mol/L and salt concentration of 0.5% and flow rate set to 5 mL/min. The light intensity was set to 1 sun.
After the reaction was carried out for 180min, the CBZ degradation efficiency in the wastewater was found to be 75.62%, Cu2+The recovery efficiency of (A) was 52.55%, and the power generation amount was 56.57W/(m)3Solution x m2Electrode area).
Reaction ofAfter 48 hours, the CBZ degradation efficiency in the wastewater is measured to be 73.85 percent, and the Cu content is measured2+The recovery efficiency of (A) was 9.34%, and the power generation amount was 45.34W/(m)3Solution x m2Electrode area).
Example 2
The procedure of example 1 was repeated except that: the photo-anode is made of titanium dioxide, carbon quantum dots and molybdenum disulfide.
After the reaction was carried out for 180min, the CBZ degradation efficiency in the wastewater was found to be 68.83%, Cu2+The recovery efficiency of (A) was 48.61%, and the power generation amount was 52.84W/(m)3Solution x m2Electrode area).
After 48 hours of reaction, the CBZ degradation efficiency in the wastewater is measured to be 56.34 percent, and Cu is measured2+The recovery efficiency of (2) was 8.56%, and the power generation amount was 37.09W/(m)3Solution x m2Electrode area).
Example 3
The procedure of example 1 was repeated except that: the photo-anode is Mxene and molybdenum disulfide.
After the reaction was carried out for 180min, the CBZ degradation efficiency in the wastewater was found to be 66.29%, Cu2+The recovery efficiency of (A) was 39.75%, and the power generation amount was 49.98W/(m)3Solution x m2Electrode area).
After the reaction is carried out for 48 hours, the CBZ degradation efficiency in the wastewater is 59.96 percent, and the Cu content is measured2+The recovery efficiency of (A) was 9.09%, and the power generation amount was 35.34W/(m)3Solution x m2Electrode area).
Example 4
The procedure of example 1 was repeated except that: the salt concentration was 1%.
After the reaction was carried out for 180min, the CBZ degradation efficiency in the wastewater was found to be 71.08%, Cu2+The recovery efficiency of (A) was 49.96%, and the power generation amount was 54.39W/(m)3Solution x m2Electrode area).
After 48 hours of reaction, the CBZ degradation efficiency in the wastewater is measured to be 49.99 percent, and Cu is measured2+The recovery efficiency of (A) was 8.08%, and the electricity generation amount was 40.02W/(m)3Solution x m2Electrode area).
Example 5
The procedure of example 2 was repeated except that: the salt concentration was 1%.
After the reaction was carried out for 180min, the CBZ degradation efficiency in the wastewater was found to be 64.02%, Cu2+The recovery efficiency of (A) was 41.54%, and the power generation amount was 51.88W/(m)3Solution x m2Electrode area).
The reaction is carried out for 48 hours, and the measured CBZ degradation efficiency in the wastewater is 61.02 percent, and the Cu content is2+The recovery efficiency of (A) was 9.14%, and the power generation amount was 38.02W/(m)3Solution x m2Electrode area).
Example 6
The procedure of example 3 was repeated except that: the salt concentration was 1%.
After the reaction was carried out for 180min, the CBZ degradation efficiency in the wastewater was found to be 59.96%, Cu2+The recovery efficiency of (A) was 33.83%, and the power generation amount was 47.72W/(m)3Solution x m2Electrode area).
After 48 hours of reaction, the CBZ degradation efficiency in the wastewater is measured to be 56.84 percent, and Cu is measured2+The recovery efficiency of (A) was 10.09%, and the power generation amount was 44.74W/(m)3Solution x m2Electrode area).
Example 7
The procedure of example 1 was repeated except that: the salt concentration was 1.5%.
After the reaction was carried out for 180min, the CBZ degradation efficiency in the wastewater was found to be 67.21%, Cu2+The recovery efficiency of (A) was 45.83%, and the power generation amount was 52.99W/(m)3Solution x m2Electrode area).
After the reaction is carried out for 48 hours, the CBZ degradation efficiency in the wastewater is 68.83 percent, and the Cu content is measured2+The recovery efficiency of (A) was 6.22%, and the power generation amount was 39.63W/(m)3Solution x m2Electrode area).
Example 8
The procedure of example 2 was repeated except that: the salt concentration was 1.5%.
After the reaction was carried out for 180min, the CBZ degradation efficiency in the wastewater was found to be 61.11%, Cu2+The recovery efficiency of (A) was 36.21%, and the power generation amount was 50.88W/(m)3Solution x m2Electrode area).
After the reaction is carried out for 48 hours, the CBZ degradation efficiency in the wastewater is 59.04 percent, and the Cu content is measured2+The recovery efficiency of (2) was 8.34%, and the electricity generation amount was 25.54W/(m)3Solution x m2Electrode area).
Example 9
The procedure of example 3 was repeated except that: the salt concentration was 1.5%.
After the reaction was carried out for 180min, the CBZ degradation efficiency in the wastewater was found to be 57.29%, Cu2+The recovery efficiency of (A) was 28.14%, and the power generation amount was 46.69W/(m)3Solution x m2Electrode area).
After 48 hours of reaction, the CBZ degradation efficiency in the wastewater is 57.21 percent and the Cu content is measured2+The recovery efficiency of (A) was 7.09%, and the power generation amount was 33.09W/(m)3Solution x m2Electrode area).
Example 10
The procedure of example 1 was repeated except that: the salt concentration was 2%.
After the reaction was carried out for 180min, the CBZ degradation efficiency in the wastewater was found to be 63.30%, Cu2+The recovery efficiency of (A) was 42.56%, and the power generation amount was 50.12W/(m)3Solution x m2Electrode area).
After the reaction is carried out for 48 hours, the CBZ degradation efficiency in the wastewater is 62.57 percent, and the Cu content is measured2+The recovery efficiency of (A) was 9.10%, and the power generation amount was 28.48W/(m)3Solution x m2Electrode area).
Example 11
The procedure of example 2 was repeated except that: the salt concentration was 2%.
After the reaction was carried out for 180min, the CBZ degradation efficiency in the wastewater was found to be 56.33%, Cu2+The recovery efficiency of (A) was 32.03%, and the power generation amount was 51.01W/(m)3Solution x m2Electrode area).
After 48 hours of reaction, the CBZ degradation efficiency in the wastewater is measured to be 50.84 percent, and Cu is measured2+The recovery efficiency of (D) was 8.37%, and the power generation amount was 33.66W/(m)3Solution x m2Electrode area).
Example 12
The procedure of example 3 was repeated except that: the salt concentration was 2%.
After the reaction was carried out for 180min, the CBZ degradation efficiency in the wastewater was found to be 51.08%, Cu2+The recovery efficiency of (A) was 24.43%, and the power generation amount was 45.22W/(m)3Solution x m2Electrode area).
After the reaction is carried out for 48 hours, the CBZ degradation efficiency in the wastewater is 58.67 percent, and the Cu content is measured2+The recovery efficiency of (D) was 8.15%, and the electricity generation amount was 31.04W/(m)3Solution x m2Electrode area).
Table 1 shows the results of 180min treatment in examples 1-12.
TABLE 1 test results of examples 1-12 after 180min treatment
Figure BDA0002892731460000161
As can be seen from table 1, the photocurrent density generated by the anode made of titanium dioxide, carbon quantum dots, and tungsten oxide under the action of light is the highest, and the degradation efficiency of organic substances in wastewater, the recovery efficiency of metal ions, and the power generation amount are the highest. Meanwhile, along with the increase of the concentration of salt in the wastewater, the degradation efficiency of the photoelectrochemical system on organic matters, the recovery efficiency of metal ions and the electricity generation amount are gradually reduced.
Example 13
The procedure of example 1 was repeated except that: the metal cathode was 304 stainless steel.
After the reaction was carried out for 180min, the CBZ degradation efficiency in the wastewater was found to be 70.84%, Cu2+The recovery efficiency of (2) was 49.91%, and the power generation amount was 52.13W/(m)3Solution x m2Electrode area).
Example 14
The procedure of example 1 was repeated except that: the metal cathode was Q235-b carbon steel.
After the reaction was carried out for 180min, the CBZ degradation efficiency in the wastewater was found to be 69.96%, Cu2+The recovery efficiency of (A) was 26.52%, and the power generation amount was 51.87W/(m)3Solution x m2Electrode area).
Example 15
The procedure of example 1 was repeated except that: the metal cathode was 304 stainless steel with a salt concentration of 1%.
After the reaction was carried out for 180min, the CBZ degradation efficiency in the wastewater was found to be 67.79%, Cu2+The recovery efficiency of (A) was 45.51%, and the power generation amount was 50.96W/(m)3Solution x m2Electrode area).
Example 16
The procedure of example 1 was repeated except that: the metal cathode is Q235-b carbon steel, and the salt concentration is 1%.
After the reaction was carried out for 180min, the CBZ degradation efficiency in the wastewater was found to be 62.13%, Cu2+The recovery efficiency of (A) was 23.36%, and the power generation amount was 49.38W/(m)3Solution x m2Electrode area).
Example 17
The procedure of example 1 was repeated except that: the metal cathode was 304 stainless steel with a salt concentration of 1.5%.
After the reaction was carried out for 180min, the CBZ degradation efficiency in the wastewater was found to be 62.56%, Cu2+The recovery efficiency of (A) was 40.88%, and the power generation amount was 46.32W/(m)3Solution x m2Electrode area).
Example 18
The procedure of example 1 was repeated except that: the metal cathode was Q235-b carbon steel with a salt concentration of 1.5%.
After the reaction was carried out for 180min, the CBZ degradation efficiency in the wastewater was found to be 56.36%, Cu2+The recovery efficiency of (A) was 20.09%, and the power generation amount was 44.58W/(m)3Solution x m2Electrode area).
Example 19
The procedure of example 1 was repeated except that: the metal cathode was 304 stainless steel with a salt concentration of 2%.
After the reaction was carried out for 180min, the CBZ degradation efficiency in the wastewater was found to be 59.13%, Cu2+The recovery efficiency of (2) was 37.98%, and the power generation amount was 45.59W/(m)3Solution x m2Electrode surfaceProduct).
Example 20
The procedure of example 1 was repeated except that: the metal cathode was Q235-b carbon steel with a salt concentration of 2%.
After the reaction was carried out for 180min, the CBZ degradation efficiency in the wastewater was found to be 50.55%, Cu2+The recovery efficiency of (A) was 16.94%, and the power generation amount was 40.46W/(m)3Solution x m2Electrode area).
Example 21
The procedure of example 1 was repeated except that: the length of the wire is 6 cm.
After the reaction was carried out for 180min, the CBZ degradation efficiency in the wastewater was found to be 69.32%, Cu2+The recovery efficiency of (A) was 47.13%, and the electricity generation amount was 51.02W/(m)3Solution x m2Electrode area).
Example 22
The procedure of example 1 was repeated except that: the length of the wire is 7 cm.
After the reaction was carried out for 180min, the CBZ degradation efficiency in the wastewater was found to be 67.55%, Cu2+The recovery efficiency of (A) was 44.83%, and the power generation amount was 49.38W/(m)3Solution x m2Electrode area).
Example 23
The procedure of example 1 was repeated except that: the length of the wire is 8 cm.
After the reaction was carried out for 180min, the CBZ degradation efficiency in the wastewater was found to be 62.09%, Cu2+The recovery efficiency of (A) was 40.96%, and the power generation amount was 45.13W/(m)3Solution x m2Electrode area).
Example 24
The procedure of example 1 was repeated except that: the length of the wire is 9 cm.
After the reaction was carried out for 180min, the CBZ degradation efficiency in the wastewater was found to be 60.11%, Cu2+The recovery efficiency of (A) was 37.21%, and the power generation amount was 42.09W/(m)3Solution x m2Electrode area).
Example 25
The procedure of example 1 was repeated except that: the concentration of CBZ was 1 mol/L.
After the reaction was carried out for 180min, the CBZ degradation efficiency in the wastewater was found to be 82.34%, Cu2+The recovery efficiency of (A) was 53.04%, and the power generation amount was 51.04W/(m)3Solution x m2Electrode area).
Example 26
The procedure of example 1 was repeated except that: the concentration of CBZ was 3 mol/L.
After the reaction was carried out for 180min, the CBZ degradation efficiency in the wastewater was found to be 78.04%, Cu2+The recovery efficiency of (A) was 52.03%, and the power generation amount was 53.96W/(m)3Solution x m2Electrode area).
Example 27
The procedure of example 1 was repeated except that: the concentration of CBZ was 7 mol/L.
After the reaction was carried out for 180min, the CBZ degradation efficiency in the wastewater was found to be 71.02%, Cu2+The recovery efficiency of (A) was 54.55%, and the power generation amount was 58.84W/(m)3Solution x m2Electrode area).
Example 28
The procedure of example 1 was repeated except that: the concentration of CBZ was 9 mol/L.
After the reaction was carried out for 180min, the CBZ degradation efficiency in the wastewater was measured to be 60.32%, Cu2+The recovery efficiency of (A) was 52.09%, and the power generation amount was 57.04W/(m)3Solution x m2Electrode area).
Example 29
The procedure of example 1 was repeated except that: cu2+The concentration of (2) is 0.1 mol/L.
After the reaction was carried out for 180min, the CBZ degradation efficiency in the wastewater was found to be 74.38%, Cu2+The recovery efficiency of (A) was 66.34%, and the power generation amount was 49.33W/(m)3Solution x m2Electrode area).
Example 30
The procedure of example 1 was repeated except that: cu2+The concentration of (2) is 0.3 mol/L.
After the reaction was carried out for 180min, the CBZ degradation efficiency in the wastewater was found to be 73.96%, Cu2+The recovery efficiency of (A) was 60.82%, and the power generation amount was 52.76W/(m)3Solution x m2Electrode area).
Example 31
The procedure of example 1 was repeated except that: cu2+The concentration of (2) is 0.7 mol/L.
After the reaction was carried out for 180min, the CBZ degradation efficiency in the wastewater was found to be 75.02%, Cu2+The recovery efficiency of (2) was 47.73%, and the power generation amount was 59.84W/(m)3Solution x m2Electrode area).
Example 32
The procedure of example 1 was repeated except that: cu2+The concentration of (2) is 0.9 mol/L.
After the reaction was carried out for 180min, the CBZ degradation efficiency in the wastewater was found to be 76.33%, Cu2+The recovery efficiency of (A) was 42.96%, and the electricity generation amount was 63.96W/(m)3Solution x m2Electrode area).
Example 33
The photoanode shown in FIG. 2 is made of titanium dioxide, carbon quantum dots and tungsten oxide, the metal cathode is made of 304 stainless steel, the length of the lead (made of brass) is 5cm, the resource recovery flow type photoelectrochemical system with a light-transmitting quartz window is used for treating organic matters (carbamazepine, CBZ) with the concentration of 0.5mol/L and heavy metals (Cu)2+) In the high-salinity wastewater (solution volume 15.3L) having a concentration of 0.2mol/L and a concentration of 1000mg/L of sodium chloride, the flow rate was set to 5 mL/min. The light intensity was set at 100mW/m2(i.e., 1 sunlight).
CBZ and Cu2+The cumulative concentrations of (A) and (B) are respectively 7.65mol (15.3L multiplied by 0.5mol/L) and 3.06mol (15.3L multiplied by 0.2mol/L), CBZ and Cu in the wastewater are treated in the wastewater treatment process2+The removal efficiency of (2) was tested, and the test results are shown in FIG. 3. As can be seen from FIG. 3, after the reaction proceeded for 48 hours, CBZ and Cu in the wastewater were obtained2+The removal efficiency of (a) was 75.63% and 44.76%, respectively.
And meanwhile, the electricity generation quantity is tested, the test result is shown in figure 4, as can be seen from figure 4, the reaction is carried out for 48 hours, and the average output voltage of the photoelectrochemical system is 56.79W/(m)3Solution x m2Electrode area), the photoelectric conversion efficiency reaches 13.39%.
Comparative example
Comparative example 1
The procedure of example 1 was repeated except that: no external circuit is provided (i.e., no wires are provided between the photoanode and the metal cathode).
After 48 hours of reaction, the CBZ degradation efficiency in the wastewater is 65.12 percent, and the electricity generation is 27.96W/(m)3Solution x m2Electrode area).
Compared with the example 1, the degradation efficiency and the electricity generation quantity of the CBZ are reduced, which shows that the introduction of the photo-generated cathodic protection can improve the degradation efficiency and the electricity generation quantity of the system on the CBZ under the long-term operation.
Comparative example 2
The procedure of example 2 was repeated except that: no external circuit is provided (i.e., no wires are provided between the photoanode and the metal cathode).
After 48 hours of reaction, the CBZ degradation efficiency in the wastewater is 50.49 percent, and the electricity generation is 30.03W/(m)3Solution x m2Electrode area).
Compared with the example 2, the CBZ degradation efficiency and the electricity generation quantity are reduced, which shows that the introduction of the photo-generated cathodic protection can improve the CBZ degradation efficiency and the electricity generation quantity under the long-term operation of the system.
Comparative example 3
The procedure of example 3 was repeated except that: no external circuit is provided (i.e., no wires are provided between the photoanode and the metal cathode).
After 48 hours of reaction, the CBZ degradation efficiency in the wastewater is 49.16 percent, and the electricity generation is 28.84W/(m)3Solution x m2Electrode area).
Comparative example 4
The procedure of example 4 was repeated except that: no external circuit is provided (i.e., no wires are provided between the photoanode and the metal cathode).
After 48 hours of reaction, the CBZ degradation efficiency in the wastewater is 42.33 percent, and the electricity generation is 33.90W/(m)3Solution x m2Electrode area).
Comparative example 5
The procedure of example 5 was repeated except that: no external circuit is provided (i.e., no wires are provided between the photoanode and the metal cathode).
After 48 hours of reaction, the CBZ degradation efficiency in the wastewater is 54.84 percent, and the electricity generation is 29.88W/(m)3Solution x m2Electrode area).
Comparative example 6
The procedure of example 6 was repeated except that: no external circuit is provided (i.e., no wires are provided between the photoanode and the metal cathode).
After 48 hours of reaction, the CBZ degradation efficiency in the wastewater is 45.67 percent, and the electricity generation is 31.12W/(m)3Solution x m2Electrode area).
Comparative example 7
The procedure of example 7 was repeated except that: no external circuit is provided (i.e., no wires are provided between the photoanode and the metal cathode).
After 48 hours of reaction, the CBZ degradation efficiency in the wastewater is 55.85 percent, and the electricity generation is 25.77W/(m)3Solution x m2Electrode area).
Comparative example 8
The procedure of example 8 was repeated except that: no external circuit is provided (i.e., no wires are provided between the photoanode and the metal cathode).
After 48 hours of reaction, the CBZ degradation efficiency in the wastewater is 47.22 percent, and the electricity generation is 22.23W/(m)3Solution x m2Electrode area).
Comparative example 9
The procedure of example 9 was repeated except that: no external circuit is provided (i.e., no wires are provided between the photoanode and the metal cathode).
After 48 hours of reaction, the CBZ degradation efficiency in the wastewater is 44.91 percent, and the electricity generation amount is 29.41W/(m)3Solution x m2Electrode area).
Comparative example 10
The procedure of example 10 was repeated except that: no external circuit is provided (i.e., no wires are provided between the photoanode and the metal cathode).
After 48 hours of reaction, the CBZ degradation efficiency in the wastewater is 53.84 percent, and the electricity generation amount is 23.39W/(m)3Solution x m2Electrode area).
Comparative example 11
The procedure of example 11 was repeated except that: no external circuit is provided (i.e., no wires are provided between the photoanode and the metal cathode).
After 48 hours of reaction, the CBZ degradation efficiency in the wastewater is 39.99 percent, and the electricity generation is 30.04W/(m)3Solution x m2Electrode area).
Comparative example 12
The procedure of example 12 was repeated except that: no external circuit is provided (i.e., no wires are provided between the photoanode and the metal cathode).
After 48 hours of reaction, the CBZ degradation efficiency in the wastewater is 45.21 percent, and the electricity generation amount is 26.78W/(m)3Solution x m2Electrode area).
Comparative example 13
The procedure of example 33 was repeated except that: no external circuit is provided (i.e., no wires are provided between the photoanode and the metal cathode).
After the reaction was carried out for 48 hours, a photograph of the surface of the cathode 304 stainless steel is shown in FIG. 6, and it can be seen from FIG. 6 that the surface of the cathode 304 stainless steel was corroded seriously after the treatment for 48 hours without the cathodic protection.
Examples of the experiments
Experimental example 1 scanning Electron microscope test
The surface of the 304 stainless steel used for the cathode in example 33, which was not in the original state, was subjected to a scanning electron microscope test, and the test result is shown in fig. 5-a; the surface of the 304 stainless steel which is not protected after the long-term experiment of the comparative example 13 is subjected to a scanning electron microscope test, and the test result is shown in fig. 5-b; the surface of 304 stainless steel treated by wastewater for 48 hours in example 33 was subjected to scanning electron microscope test, and the test results are shown in FIG. 5-c; after the surface precipitates of the 304 stainless steel treated by the wastewater in the example 33 for 48 hours are removed, the surface thereof is tested by a scanning electron microscope, and the test result is shown in FIG. 5-d.
As can be seen from fig. 5-a, the unused 304 stainless steel has a smoother surface.
As can be seen from fig. 5-b, the unprotected 304 stainless steel surface had severe surface corrosion after long-term experiments.
As can be seen from FIG. 5-c, the surface of the 304 stainless steel treated for 48 hours in the wastewater of example 30 showed a large amount of copper powder, and as can be seen from FIG. 5-d, the surface of the 304 stainless steel was substantially free from corrosion after the surface precipitates were removed.
According to the photoelectrochemical system disclosed by the invention, by introducing the photoproduction cathodic protection concept, the corrosion of the cathode surface is inhibited under the photoproduction cathodic protection effect in the process of treating wastewater for a long time, the stability of the system is effectively improved, and the photoelectrochemical system can stably run for a long time in a high-salt environment.
The invention has been described in detail with reference to specific embodiments and illustrative examples, but the description is not intended to be construed in a limiting sense. Those skilled in the art will appreciate that various equivalent substitutions, modifications or improvements may be made to the technical solution of the present invention and its embodiments without departing from the spirit and scope of the present invention, which fall within the scope of the present invention. The scope of the invention is defined by the appended claims.

Claims (10)

1. A flow-type photoelectrochemical system having a resource recovery function, comprising: photoelectrochemical reactor (9) and water circulation system (3), photoelectrochemical reactor (9) are including light source (2), photoanode (6), metal cathode (7), external circuit (8) and water cooling circulation system (10).
2. The flow-type photoelectrochemical system according to claim 1, wherein the photoelectrochemical system is a flow-type photoelectrochemical system,
the photo-anode (6), the metal cathode (7) and the water-cooling circulation system (10) are positioned inside the photoelectrochemical reactor (9), one end of an external circuit (8) is connected with the photo-anode (6), the other end of the external circuit is connected with the metal cathode (7), and the water-cooling circulation system (10) is arranged along the inner wall of the side edge of the photoelectrochemical reactor (9) to form a loop;
the water circulation system (3) is positioned outside the photoelectrochemical reactor (9) and is communicated with two ends of the photoelectrochemical reactor (9).
3. The flow-type photoelectrochemical system according to claim 1, wherein the photoelectrochemical system is a flow-type photoelectrochemical system,
the photoelectrochemical system also comprises a light-transmitting quartz window (4), and the light-transmitting quartz window (4) is positioned on one side of the photo anode (6);
the photo-anode is selected from one or more of titanium dioxide, carbon quantum dots, ferric oxide, tungsten oxide, molybdenum disulfide, vanadium bismuth tetroxide and Mxene.
4. The flow-type photoelectrochemical system according to claim 1, wherein the photoelectrochemical system is a flow-type photoelectrochemical system,
the metal cathode is selected from stainless steel, aluminum alloy, carbon steel, brass, nickel-based materials or a platinum sheet;
the length of the lead is 1-30 cm.
5. The flowing photoelectrochemical system with the resource recovery function is used for treating wastewater.
6. A method of wastewater treatment and electrical energy recovery, the method comprising the steps of:
step 1, placing wastewater to be treated in a photoelectrochemical system;
and 2, setting treatment conditions for treatment.
7. The wastewater treatment and electric energy recovery method according to claim 6, wherein, in step 1,
the photoelectrochemical system is the photoelectrochemical system of one of claims 1 to 4;
the concentration of organic matters in the wastewater to be treated is 0.1-20 mol/L.
8. The wastewater treatment and electric energy recovery method according to claim 6, wherein, in step 1,
the concentration of the heavy metal ions is 0.01-5 mol/L.
9. The wastewater treatment and electric energy recovery method according to claim 6, wherein, in step 1,
the salinity of the wastewater is 0.05-5%.
10. The wastewater treatment and electric energy recovery method according to claim 6, wherein, in the step 2,
treating the substrate under the illumination condition that: 1-3 sunlight rays;
the flow rate of the wastewater in the photoelectrochemical system is 1-10 mL/min.
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