CN114906996A - Method for recovering phosphorus in sludge and synchronously generating electricity by using bluestone generated by microbial fuel cell - Google Patents
Method for recovering phosphorus in sludge and synchronously generating electricity by using bluestone generated by microbial fuel cell Download PDFInfo
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- CN114906996A CN114906996A CN202210630274.3A CN202210630274A CN114906996A CN 114906996 A CN114906996 A CN 114906996A CN 202210630274 A CN202210630274 A CN 202210630274A CN 114906996 A CN114906996 A CN 114906996A
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- sludge
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- fuel cell
- cathode
- anode
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- C—CHEMISTRY; METALLURGY
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F11/00—Treatment of sludge; Devices therefor
- C02F11/02—Biological treatment
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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
- C02F11/00—Treatment of sludge; Devices therefor
- C02F11/006—Electrochemical treatment, e.g. electro-oxidation or electro-osmosis
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/06—Combination of fuel cells with means for production of reactants or for treatment of residues
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/16—Biochemical fuel cells, i.e. cells in which microorganisms function as catalysts
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Health & Medical Sciences (AREA)
- Molecular Biology (AREA)
- Micro-Organisms Or Cultivation Processes Thereof (AREA)
Abstract
The invention discloses a method for recovering phosphorus in sludge and synchronously generating electricity by using cyanite generated by a microbial fuel cell, belonging to the field of residual sludge phosphorus recovery and resource utilization. The method comprises the following steps: a double-chamber microbial fuel cell is adopted, anaerobic sludge is inoculated on an anode, so that electricity-generating microorganisms are enriched on an anode carbon brush, the electricity-generating microorganisms are utilized to degrade organic matters in the sludge to generate electrons and are captured by an electrode, ferric citrate is used as an electron acceptor at a cathode, an oxidation-reduction potential difference is generated to enable the electrons on the anode to spontaneously reach the cathode through an external circuit, and the electrons reduce the ferric citrate and ferric iron in the sludge at the cathode to generate ferrocyanite so as to achieve the purposes of recovering phosphorus in the sludge and synchronously generating electricity. The method newly generates the vivianite in the sludge, and the recovery rate of the soluble phosphorus in the sludge can reach 98.94 percent by controlling the reaction conditions.
Description
Technical Field
The invention relates to the field of residual sludge phosphorus recovery and resource utilization, in particular to a method for recovering phosphorus in sludge and synchronously generating electricity by using bluestone generated by a microbial fuel cell.
Background
Phosphorus is one of the basic elements of life activities in nature, and 90 percent of phosphorus is derived from nonrenewable phosphate ores. However, with the continuous exploitation and utilization of phosphorite resources and the natural sedimentation of phosphorus cycle, phosphorus resources become more and more scarce, and China is facing a severe energy crisis and a phosphorus depletion crisis, so that the recovery of phosphorus resources from wastes becomes a hot spot of current research.
Compared with developed countries, the research on phosphorus recovery in China starts late, and the phenomenon of 'heavy water and light mud' exists, and in fact, the total amount of the generated urban excess sludge is greatly increased along with the rapid increase of domestic sewage treatment capacity in China. According to research, 20-50% of organic carbon compounds and 90% of phosphorus are converted into sludge in the sewage treatment process. The excess sludge is a byproduct of sewage treatment and is the final destination of phosphorus in sewage treatment plants, and if the excess sludge is directly discharged without being treated or is treated as waste, not only resource waste is caused, but also environmental pollution is caused. At present, sludge treatment methods in China mainly comprise incineration, direct landfill, land utilization, electric fermentation, anaerobic digestion and the like, and the methods have the defects of large energy consumption, secondary pollution risk, low phosphorus resource recovery rate, long treatment period and the like. Therefore, the development of a new sludge treatment technology with low energy consumption, high resource recovery rate, short treatment period, safety and reliability is imperative.
Vivianite (Fe) 3 (PO 4 ) 2 ·8H 2 O) is used as a ferric phosphate salt compound with stable property, is a good slow-release fertilizer, and has higher economic value of phosphorus (P) in unit weight compared with other phosphate compounds. However, because the generation of the phosphorus is required to be carried out under the anaerobic reducing condition, the operation requirement is higher, and the phosphorus recovery research mainly appears in the anaerobic digestion of the sludge in recent years, but the anaerobic digestion reaction time is longer, the phosphorus recovery efficiency in a short period is not high, and how to carry out the sludge phosphorus recovery in the form of vivianite with high efficiency has very important meaningAnd (5) defining.
Disclosure of Invention
Aiming at the problems of high energy consumption, secondary pollution risk, low phosphorus resource recovery rate, long treatment period and the like in the prior art, the invention provides a method for recovering phosphorus in sludge and synchronously generating electricity by using a microbial fuel cell to generate vivianite.
The invention firstly provides a method for recovering phosphorus in sludge and synchronously generating electricity, which comprises the following steps: anaerobic sludge is inoculated on an anode by adopting a double-chamber microbial fuel cell, so that electricity-producing microorganisms are enriched on an anode carbon brush, organic matters in the sludge are degraded by the electricity-producing microorganisms to generate electrons and are captured by an electrode, ferric citrate is used as an electron acceptor at the cathode, an oxidation-reduction potential difference is generated to ensure that the electrons on the anode spontaneously reach the cathode through an external circuit, and the electrons reduce the ferric citrate and ferric iron in the sludge at the cathode and generate ferrocyanite, so that the aims of recovering phosphorus in the sludge and synchronously producing electricity are fulfilled.
The electrogenic microorganisms are mainly one or more of Proteobacteria, Theobromobacteria, Acidobacterium and Actinomycetes, specifically can be Geobacter, Shewanella and the like, are mostly facultative anaerobes, take anaerobic respiration and fermentation as main metabolic modes, and generate CO by oxidizing organic matters 2 And obtains the energy required by the growth of the electron in the process of electron transfer.
The anaerobic sludge is anaerobic sludge discharged by an anaerobic bioreactor which stably runs for a long time in a laboratory or a sewage treatment plant.
The method specifically comprises the following steps:
(1) inoculating anaerobic sludge in the anode chamber of the double-chamber microbial fuel cell, and starting the cell;
(2) adding sludge to be treated into the anode chamber of the started double-chamber microbial fuel cell; adding sludge to be treated and ferric citrate solution into the cathode chamber; and operating the double-chamber microbial fuel cell to achieve the purposes of recovering phosphorus in the sludge and synchronously generating electricity.
The method, step (1), for starting the dual-chamber microbial fuel cell, comprises the following steps: anaerobic sludge is inoculated in the anode chamber, a culture solution is added, a ferric citrate solution is added in the cathode chamber, nitrogen is used for aerating the anode chamber and the cathode chamber to ensure that the whole reaction process is in an anaerobic state, a lead is used for connecting the anode and the cathode, the double-chamber microbial fuel cell is operated, when the voltage is close to zero, the solution in the cathode chamber and the anode chamber is replaced, and when the electricity generation time and the maximum voltage of each period tend to be stable, the starting is completed.
In the method, the volume ratio of the anaerobic sludge to the culture solution is 1: 5-1: 10, and specifically can be 1: 5;
the culture solution comprises the following components: ammonium chloride, potassium chloride, sodium bicarbonate, sodium dihydrogen phosphate, sodium acetate, trace element solution and vitamin solution;
specifically, in the culture solution, the concentration of sodium acetate is 5.0-25.0 mM; specifically 10 mM;
more specifically, the culture solution comprises the following components: 0.25g/L NH 4 Cl、0.1g/L KCl、2.5g/L NaHCO 3 、0.6g/L NaH 2 PO 4 5.0-25.0 mM sodium acetate, 10mL/L of trace element solution and 10mL/L of vitamin solution;
the trace element solution comprises the following components: nitrilotriacetic acid trisodium, MgSO 4 ·7H 2 O、MnSO 4 ·H 2 O、NaCl、FeSO 4 ·7H 2 O、CaCl 2 ·2H 2 O、CoCl 2 ·6H 2 O、ZnCl 2 、CuSO 4 ·5H 2 O、AlK(SO 4 ) 2 ·12H 2 O、H 3 BO 3 、Na 2 MoO 4 ·2H 2 O、NiCl 2 ·6H 2 O and Na 2 WO 4 ·2H 2 O; the solvent is water;
specifically, the composition of the trace element solution is as follows: 1.5g/L trisodium nitrilotriacetate, 3g/L MgSO 4 ·7H 2 O、0.5g/L MnSO 4 ·H 2 O、1g/L NaCl、0.1g/L FeSO 4 ·7H 2 O、0.1g/L CaCl 2 ·2H 2 O、0.1g/L CoCl 2 ·6H 2 O、0.13g/L ZnCl 2 、0.01g/L CuSO 4 ·5H 2 O、0.01g/L AlK(SO 4 ) 2 ·12H 2 O、0.01g/L H 3 BO 3 、0.025g/L Na 2 MoO 4 ·2H 2 O、0.024g/L NiCl 2 ·6H 2 O and 0.025g/L Na 2 WO 4 ·2H 2 O；
The vitamin solution comprises the following components: pyridoxine hydrochloride, vitamin B12, biotin, folic acid, pantothenic acid, thiamine, riboflavin, nicotinic acid, p-aminobenzoic acid, and lipoic acid; the solvent is water;
specifically, the vitamin solution comprises the following components: pyridoxine hydrochloride 10mg/L, vitamin B12 0.1mg/L, biotin 2mg/L, folic acid 2mg/L, pantothenic acid 5mg/L, thiamine 5mg/L, riboflavin 5mg/L, nicotinic acid 5mg/L, p-aminobenzoic acid 5mg/L, and lipoic acid 5 mg/L.
In the step (1), the concentration of the ferric citrate solution is 25-50 mM; specifically, the concentration of the active ingredient can be 50 mM;
the aeration time is 15-30 min;
in the step (1), the temperature for operating the double-chamber microbial fuel cell is 25-35 ℃; specifically, it may be 30 ℃.
In the method, in the step (2), the initial SCOD concentration of the solution in the anode chamber is 200-2000 mg/L; specifically, the concentration may be 500 mg/L.
In the method, in the step (2), the initial pH of the solution in the cathode chamber is 6-9; specifically, the number of the carbon atoms can be 6-8; more specifically, it can be 7 or 7.5;
the initial Fe/P molar ratio of the solution in the cathode chamber is 0.6-2.5; specifically, it may be 1.5.
In the method, in the step (2), the operating temperature of the dual-chamber microbial fuel cell is 25-35 ℃; specifically, the temperature can be 30 ℃;
the two-chamber microbial fuel cell is operated under anaerobic conditions.
In the method, the sludge to be treated is at least one of excess sludge of a municipal sewage treatment plant, secondary sedimentation tank sludge, return sludge, concentrated sludge and dewatered sludge.
The water content of the sludge to be treated is 98 wt% -99 wt%.
The sludge is the excess sludge of the municipal sewage plant, the cathode chamber and the anode chamber are the same sludge in practical application, including but not limited to secondary sedimentation tank sludge, return sludge, concentrated sludge, dehydrated sludge and the like, and the return pump is used for internal circulation, thereby being beneficial to large-scale phosphorus recovery.
The anode of the double-chamber microbial fuel cell is an electrode which is easy to attach microorganisms and has a large specific surface area, and the electrode comprises but is not limited to a carbon brush, a carbon felt, a carbon cloth or a graphite felt, and the like, so that the anode microorganisms can continuously and stably generate electricity.
The cathode of the double-chamber microbial fuel cell is an electrode with good conductivity and corrosion resistance, and the electrode comprises but is not limited to a stainless steel net, a carbon rod or graphene and the like, so that the continuous conductivity of the reactor is facilitated.
The cathode and the anode of the double-chamber microbial fuel cell are connected by a lead when in operation and are connected with a resistor; specifically, the resistance is 1000 Ω.
In the above method, step (2) further includes a step of pretreating the sludge to be treated; the method specifically comprises the following steps: the sludge is sieved by a 100-mesh sieve, naturally settled at 4 ℃ (the step is not required for dewatering sludge), and the supernatant and impurities are discarded and stored at 4 ℃ for later use.
The principle of the invention is as follows: anaerobic sludge is inoculated on the anode of the microbial fuel cell, electricity-producing microorganisms are enriched on an anode carbon brush, the organic matters in the sludge are consumed by the electricity-producing microorganisms at the anode and generate electrons, the electrons are captured by the carbon brush, ferric citrate is used as an electron acceptor at the cathode, an oxidation-reduction potential difference is formed, the electrons can spontaneously reach the cathode through an external circuit to generate current, after the electrons reach the cathode, on one hand, free ferric iron is reduced into divalent iron, on the other hand, iron phosphate in the sludge can be excited to be activated, and the divalent iron generated by reduction can fix free phosphate radicals in the sludge to form iron cyanite, so that the purposes of synchronously generating electricity and producing the iron cyanite are achieved.
The invention has the following beneficial effects:
(1) the invention generates new blue in the sludgeThe recovery rate of soluble phosphorus in the sludge can reach 98.94% by controlling the reaction conditions, the iron-phosphorus content in the sludge including the vivianite is 70%, the iron-phosphorus content is increased by about 9% compared with that before the reaction, and the vivianite crystal form in the sludge is obviously enhanced; (2) the invention can generate electricity spontaneously without external voltage, reduces energy consumption investment, and has average current density of 300mA/m 3 (ii) a (3) The reactor of the invention has simple structure, short reaction period and no secondary pollution.
Drawings
FIG. 1 is a schematic view of the structure of a microbial fuel cell according to the present invention; in the figure, 1 anode chamber, 2 cathode chambers, 3 cation exchange membranes, 4 carbon fiber brush anodes, 5 stainless steel mesh cathodes, 6 platinum sheet electrode clamps, 7 sampling ports, 8 water inlets, 9 water outlets, 10 gas collecting ports, 11 leads, 12 resistors and 13 multimeters.
Fig. 2 is a schematic view of the operation principle of the microbial fuel cell of the present invention.
FIG. 3 is an XRD pattern of sludge before and after reaction in the microbial fuel cell in example 1.
FIG. 4 is a graph showing the ratio of each phosphorus component in the solid phase of sludge before and after the reaction in the microbial fuel cell in example 1.
FIG. 5 is a graph showing changes in phosphorus concentration in example 1 of the present invention and in comparative example 1.
FIG. 6 is a graph showing the effect of iron reduction in example 1 of the present invention and comparative example 1.
FIG. 7 is a graph showing the change in phosphorus concentration in example 2 of the present invention.
FIG. 8 is a graph showing the ratio of phosphorus components in the solid phase of sludge before and after the reaction in example 2 of the present invention.
FIG. 9 is a graph of the average current density of example 2 of the present invention.
Detailed Description
The present invention is described in further detail below with reference to specific embodiments, which are given for the purpose of illustration only and are not intended to limit the scope of the invention.
The experimental procedures in the following examples are conventional unless otherwise specified.
Materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
In the following examples, the percentages are by weight unless otherwise specified.
The following experiments were all set up in triplicate and the results averaged.
Fig. 1 shows a schematic structural diagram of a microbial fuel cell used in the following embodiments, the microbial fuel cell is a two-chamber microbial fuel cell, and mainly includes: anode chamber 1, cathode chamber 2, cation exchange membrane 3, carbon fiber brush anode 4, stainless steel mesh cathode 5, platinum sheet electrode holder 6, sample connection 7, water inlet 8, delivery port 9, gas collection mouth 10, wire 11, resistance 12, universal meter 13. The anode chamber 1 and the cathode chamber 2 are separated by a cation exchange membrane 3, a carbon fiber brush anode 4 is fixed in the anode chamber 1, and a stainless steel mesh cathode 5 is fixed in the cathode chamber 2 by a platinum sheet electrode clamp 6; the two chambers are fixed by stainless steel screws; the sampling needle is inserted into the sampling port 7, and the switch is controlled by the two-way valve; the water inlet 8 and the water outlet 9 are arranged at two sides of the anode chamber 1 and the cathode chamber 2, the water inlet 8 is arranged above the water outlet 9, and the water outlet 9 is arranged below the water inlet 8 and is tightly sealed by a rubber sleeve when not in use; the air bag is connected with the air collecting port 10 and is used for storing gas generated by decomposing organic matters by anode microorganisms; the cathode and the anode are connected by a copper wire 11, and a resistor 12 is connected in the middle; multimeter 13 is connected in parallel in the circuit for measuring the circuit voltage and is connected with a computer for recording data in real time.
FIG. 2 is a schematic view of the operation of the microbial fuel cell of the present invention; the working principle of the microbial fuel cell of the invention is as follows: anaerobic sludge is inoculated to the anode of the microbial fuel cell, electricity-producing microorganisms are enriched on an anode carbon brush, the organic matters in the sludge are consumed by the electricity-producing microorganisms at the anode, electrons are generated and captured by the carbon brush, ferric citrate is used as an electron acceptor at the cathode, an oxidation-reduction potential difference is formed, so that the electrons can spontaneously reach the cathode through an external circuit, current is generated, after the electrons reach the cathode, free ferric iron is reduced into ferrous iron, on the other hand, ferric phosphate activation in the sludge can be excited, and the reduced ferrous iron can fix free phosphate radicals in the sludge to form iron cyanite, so that the aims of synchronously generating electricity and producing the iron cyanite are fulfilled.
Example 1 Effect of microbial Fuel cell on Power Generation and phosphorus recovery from excess sludge from Water works
The residual sludge is the dewatered sludge from the Yongfeng reclaimed water plant in Beijing, wherein the water content of the sludge is 84.77 percent, the organic matter content is 53.46 percent, the pH value is 7.05, the Fe/P molar ratio is 0.56, the impurities attached to the sludge are removed, and the sludge is stored at the temperature of 4 ℃. For convenience of experiment, the sludge with the water content of 98% is prepared by uniformly mixing the sludge and water according to a certain sludge-water ratio before reaction.
The microbial fuel cell is constructed as shown in fig. 1, a reactor shell of the microbial fuel cell is made of polymethyl methacrylate material, the outer part of the reactor shell is of a cubic structure, the inner part of a chamber is of a cylindrical structure, and the effective volume of a single chamber is 118 mL. The size of the carbon fiber brush anode is 2.5cm in diameter and 2.0cm in length; the stainless steel mesh cathode is a 60 × 60-mesh 304 stainless steel mesh, and is 4cm long and 3cm wide; the two chambers are fixed by stainless steel screws.
Inoculating an effluent from a stably-operated anaerobic membrane bioreactor (sludge obtained by anaerobic fermentation of dewatered sludge of a certain reclaimed water plant in Beijing through a laboratory anaerobic membrane bioreactor) in the anode chamber, and mixing the effluent and a culture solution according to a volume ratio of 1:5 for inoculation; the culture solution is composed of 2.5g/L NaHCO 3 、0.25g/L NH 4 Cl、0.1g/L KCl、0.6g/L NaH 2 PO 4 Composition, 10mM sodium acetate as a supplementary carbon source, and trace element solution (10mL/L) and vitamin solution (10mL/L) are added to promote the growth of microorganisms. Wherein the composition of the trace element solution is as follows: 1.5g/L nitrilotriacetic acid trisodium (NTA), 3g/L MgSO 4 ·7H 2 O、0.5g/L MnSO 4 ·H 2 O、1g/L NaCl、0.1g/L FeSO 4 ·7H 2 O、0.1g/L CaCl 2 ·2H 2 O、0.1g/L CoCl 2 ·6H 2 O、0.13g/L ZnCl 2 、0.01g/L CuSO 4 ·5H 2 O、0.01g/L AlK(SO 4 ) 2 ·12H 2 O、0.01g/L H 3 BO 3 、0.025g/L Na 2 MoO 4 ·2H 2 O、0.024g/L NiCl 2 ·6H 2 O、0.025g/L Na 2 WO 4 ·2H 2 O; the composition of the vitamin solution was as follows: pyridoxine hydrochloride (vitamin B6) 10mg/L, vitamin B12 0.1mg/L, biotin 2mg/L, folic acid 2mg/L (vitamin B9), pantothenic acid 5mg/L (vitamin B5), thiamine 5mg/L (vitamin B1), riboflavin 5mg/L (vitamin B2), nicotinic acid 5mg/L, p-aminobenzoic acid 5mg/L, and lipoic acid 5 mg/L. The solvent of the culture solution is deionized water. The cathode solution was 50mM ferric citrate solution. After the cathode solution and the anode solution are added, the cathode and the anode need to be aerated for 20min by using a nitrogen bottle, and the whole reaction process is ensured to be in an anaerobic state. The cathode and the anode are connected by copper wires and are externally connected with a 1000 omega resistor. The MFC reactor has to be run at a constant temperature of 30 ℃. And monitoring the voltage change in real time by using a universal meter, and replacing the cathode solution and the anode solution when the voltage is close to zero (the anode only replaces the culture solution and does not inoculate anaerobic sludge). When the power generation time and the maximum voltage tend to be stable in each period, the starting is considered to be successful.
After the MFC is successfully started, the reactor is formally operated for an experiment. 100mL of the treated excess sludge was added to the cathode chamber and the anode chamber, respectively. Wherein, the sludge in the cathode chamber needs to be prepared together with ferric citrate with certain concentration before being added, specifically, the initial iron-phosphorus molar ratio of the sludge is 1.5, and the initial pH of the sludge is adjusted to be about 7 by using 2M NaOH solution or HCl solution. In the experimental process, a magnetic stirrer is adopted to stir the sludge so as to uniformly mix the sludge, the reaction temperature is controlled at 30 ℃, and other conditions are the same as those in the starting stage. Sampling every 2h during the operation, centrifuging, passing through the membrane and measuring the concentration of soluble P, soluble total iron (TFe) and soluble ferrous iron (Fe) in the cathode chamber 2+ ) Concentration and anode compartment SCOD concentration, wherein Fe is prevented 2+ And (4) oxidation, and a cathode chamber sample needs to be measured in time. And monitoring the voltage change in real time by using a universal meter, and when the voltage is close to zero, determining that a periodic reaction is finished. Taking out the sludge after reaction, centrifuging, and placing the solid phase in a vacuum drying oven at 35 deg.CDrying at low temperature, grinding after drying, sieving with a 100-mesh sieve, and storing in a vacuum-dried sealed bag for later use. And (3) measuring various phosphorus components in the sludge solid phase before and after the reaction by adopting a seven-step phosphorus grading method.
Fig. 3 is an XRD representation of sludge samples before and after reaction, and compared with a ferrocyanide standard card, the characteristic diffraction peaks of the sludge after the reaction are 11.16 degrees, 13.18 degrees, 18.10 degrees, 23.08 degrees, 23.60 degrees and 30.04 degrees, which can be seen to be matched with the ferrihydrite standard card PDF #75-1186, the peaks of the sludge before the reaction at the angles have certain deviation, and the intensity of the peaks after the reaction is higher than that of the peaks before the reaction, and the peak shapes are sharper, so that the content of the ferrihydrite in the sludge after the reaction is higher, and the crystal form is better.
FIG. 4 IS a graph showing the ratio of phosphorus components at each stage in sludge before reaction (IS) and after Reaction (RS), wherein weakly bound phosphorus (Loosely-P) IS phosphorus physically adsorbed to metal oxides, hydroxides, and carbonates; ferrous-bound phosphorus (Fe (II) -P) represents phosphorus in the non-oxidized vivianite; aluminum-bound phosphorus (Al-P) is phosphorus in aluminum phosphate and hydrated aluminum phosphate; the ferric iron combined phosphorus (Fe (III) -P) is phosphorus in the oxidized vivianite and phosphorus in a ferric iron phosphorus compound; extracting phosphorus (Reductant-P) by using a reducing agent refers to phosphorus which is coated by a precipitate or a colloid formed by metal oxide and exists in an adsorption form; calcium-binding phosphorus (Ca-P) is phosphorus in calcium phosphate; organophosphorus (Organic-P) is nucleic acid, inositol phosphate, polyphosphate and phosphorus complexed with Organic matter in biological cells. As can be seen from FIG. 4, the Loosely-P content after the reaction is reduced from 5% to less than 1%, the Loosely-P content is basically fixed, the Al-P content is also reduced to a certain extent, and the iron-phosphorus content of the sludge after the reaction, including vivianite, is 70%, and is increased by about 9% compared with that before the reaction, so that the method can be shown to mainly fix the phosphorus in the sludge in a weak binding state to form stable vivianite.
Comparative example 1
Since the composition of the sludge is complex, the following comparative experiments for the non-MFC group were set up to ensure that the reaction at the cathode of the MFC was due to an electrochemical reaction rather than a reaction caused by microorganisms in the sludge under anaerobic conditions.
The experiment of the non-MFC group is carried out by adopting a 250mL conical flask, and 100mL of the mixture is added into the conical flask to be mixed with ferric citrateThe remaining sludge, all parameter settings were the same as in the cathode compartment in MFC operation in example 1. Sealing the opening of the conical flask with a sealing film after anaerobic aeration for 20min, inserting a sampling needle to sample every 2h, centrifuging, passing through the film, and measuring the soluble P concentration, TFe and Fe in the cathode 2+ Concentration of Fe to prevent 2+ And (4) oxidation, wherein the sample needs to be measured in time, and the reaction time is the same as that of MFC.
Wherein the phosphorus concentration change and the iron reduction rate are shown in figures 5 and 6, and the figure shows that the recovery rate of the soluble phosphorus in 12h in example 1 can reach 98.9 percent, and the iron reduction rate is 97.4 percent; in contrast, in comparative example 1, the iron reduction rate was only 8.5% even in 12 hours under anaerobic conditions, and the phosphorus concentration in the supernatant did not decrease or increase.
Example 2 Simultaneous excess sludge Generation and iron pyrite production in microbial Fuel cells at different cathode initial pH
The implementation steps 1, 2, and 3 are the same as those in embodiment 1, and are not described herein.
After the MFC is successfully started, the reactor is formally operated for an experiment. 100mL of the treated excess sludge was added to the cathode chamber and the anode chamber, respectively. Sodium acetate is added to regulate and control the initial SCOD concentration of the anode sludge in each experiment, and the specific setting is 500 mg/L; the cathode sludge needs to be prepared together with ferric citrate with a certain concentration before being added, specifically, the initial iron-phosphorus molar ratio of the sludge is 1.5, and the initial pH of the sludge is adjusted by 2M NaOH solution or HCl solution, specifically, the initial pH is set to be 6, 7, 7.5, 8 and 9. In the experimental process, a magnetic stirrer is adopted to stir the sludge so as to uniformly mix the sludge, the reaction temperature is controlled at 30 ℃, and other conditions are the same as those in the starting stage. Taking a sample for 2h for each experiment, centrifuging, passing through a membrane, and measuring the concentration of soluble P in the cathode, TFe and Fe 2+ Concentration and anode SCOD concentration, wherein to prevent Fe 2+ And (4) oxidation, and a cathode chamber sample needs to be measured in time. And monitoring the voltage change in real time by using a multimeter, and when the voltage is close to zero, determining that a periodic reaction is finished. Taking out the sludge after reaction, centrifuging, placing the solid phase in a vacuum drying oven for drying at the low temperature of 35 ℃, grinding after drying and sieving with a 100-mesh sieveAnd storing in a vacuum-dried sealed bag for testing. And (3) measuring various phosphorus components in the sludge solid phase after reaction by adopting a seven-step phosphorus grading method.
Wherein the sludge phosphorus recovery effect and the generated average current density are shown in figures 7-9, when the pH of the sludge is close to neutral, the phosphorus recovery effect and the electricity generation effect are better, the phosphorus recovery rate of the sludge supernatant is 98.94% at most, the content of the bioavailable phosphorus in the pyrite in the solid phase is 75%, and the maximum average current density is 300mA/m 3 。
Claims (10)
1. A method for recovering phosphorus in sludge and synchronously generating electricity comprises the following steps: anaerobic sludge is inoculated on an anode by adopting a double-chamber microbial fuel cell, so that electricity-producing microorganisms are enriched on an anode carbon brush, organic matters in the sludge are degraded by the electricity-producing microorganisms to generate electrons and are captured by an electrode, ferric citrate is used as an electron acceptor at the cathode, an oxidation-reduction potential difference is generated to ensure that the electrons on the anode spontaneously reach the cathode through an external circuit, and the electrons reduce the ferric citrate and ferric iron in the sludge at the cathode and generate ferrocyanite, so that the aims of recovering phosphorus in the sludge and synchronously producing electricity are fulfilled.
2. The method of claim 1, wherein: the method comprises the following steps:
(1) inoculating anaerobic sludge in the anode chamber of the double-chamber microbial fuel cell, and starting the cell;
(2) adding sludge to be treated into the anode chamber of the started double-chamber microbial fuel cell; adding sludge to be treated and ferric citrate solution into the cathode chamber; and operating the double-chamber microbial fuel cell to achieve the purposes of recovering phosphorus in the sludge and synchronously generating electricity.
3. The method of claim 2, wherein: in the step (1), the starting of the dual-chamber microbial fuel cell comprises the following steps: anaerobic sludge is inoculated in the anode chamber, a culture solution is added, a ferric citrate solution is added in the cathode chamber, nitrogen is used for aerating the anode chamber and the cathode chamber to ensure that the whole reaction process is in an anaerobic state, a lead is used for connecting the anode and the cathode, the double-chamber microbial fuel cell is operated, when the voltage is close to zero, the solution in the cathode chamber and the anode chamber is replaced, and when the electricity generation time and the maximum voltage of each period tend to be stable, the starting is completed.
4. The method of claim 3, wherein: the volume ratio of the anaerobic sludge to the culture solution is 1: 5-1: 10, and specifically can be 1: 5;
the culture solution comprises the following components: ammonium chloride, potassium chloride, sodium bicarbonate, sodium dihydrogen phosphate, sodium acetate, trace element solution and vitamin solution;
specifically, in the culture solution, the concentration of sodium acetate is 5.0-25.0 mM;
more specifically, the culture solution comprises the following components: 0.25g/L NH 4 Cl、0.1g/L KCl、2.5g/L NaHCO 3 、0.6g/L NaH 2 PO 4 5.0-25.0 mM sodium acetate, 10mL/L microelement solution and 10mL/L vitamin solution.
5. The method according to claim 3 or 4, characterized in that: in the step (1), the concentration of the ferric citrate solution is 25-50 mM;
the aeration time is 15-30 min;
in the step (1), the temperature for operating the double-chamber microbial fuel cell is 25-35 ℃.
6. The method according to any one of claims 2-5, wherein: in the step (2), the initial SCOD concentration of the solution in the anode chamber is 200-2000 mg/L.
7. The method according to any one of claims 2-6, wherein: in the step (2), the initial pH of the solution in the cathode chamber is 6-9, specifically 6-8;
the initial Fe/P molar ratio of the solution in the cathode chamber is 0.6-2.5.
8. The method according to any one of claims 2-7, wherein: in the step (2), the operating temperature of the double-chamber microbial fuel cell is 25-35 ℃;
the two-chamber microbial fuel cell is operated under anaerobic conditions.
9. The method according to any one of claims 2-8, wherein: the sludge to be treated is at least one of excess sludge of a municipal sewage plant, secondary sedimentation tank sludge, return sludge, concentrated sludge and dewatered sludge.
10. The method according to any one of claims 2-9, wherein: the water content of the sludge to be treated is 98 wt% -99 wt%.
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| CN117361810B (en) * | 2023-12-04 | 2024-03-29 | 中国环境科学研究院 | Non-medicament Fenton treatment system based on microbial electrolytic cell |
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