CN110993963A - Phosphomolybdic acid/reduced graphene oxide/polyaniline composite material and preparation method and application thereof - Google Patents
Phosphomolybdic acid/reduced graphene oxide/polyaniline composite material and preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to the technical field of microbial fuel cells, and particularly discloses a phosphomolybdic acid/reduced graphene oxide/polyaniline composite material and a preparation method and application thereof. The preparation method comprises the following steps: mixing the graphene oxide suspension with a phosphomolybdic acid solution, adding isopropanol, and performing a photocatalytic reaction to obtain phosphomolybdic acid/reduced graphene oxide suspension; and mixing the aniline prepolymerization solution with the phosphomolybdic acid/reduced graphene oxide turbid liquid, and stirring for reaction to obtain the phosphomolybdic acid/reduced graphene oxide/polyaniline composite turbid liquid. The preparation method provided by the invention has the characteristics of simple process, convenience in operation, low energy consumption and low cost, and the obtained composite material is used for the microbial fuel cell, so that the electricity generation performance and the perchlorate removal performance of the microbial fuel cell are improved.
Description
Technical Field
The invention relates to the technical field of microbial fuel cells, in particular to a phosphomolybdic acid/reduced graphene oxide/polyaniline composite material and a preparation method and application thereof.
Background
In the face of the dual pressure of energy shortage and environmental pollution, the traditional energy-intensive sewage treatment technology cannot meet the requirement of sustainable development in the 21 st century, and the problem of how to solve energy development and utilization and environmental pollution becomes a hot spot of concern to human beings. In recent years, attention has been paid to Microbial Fuel Cell (MFC) technology, which utilizes microorganisms to oxidize and decompose organic substances and generate electricity, and has a certain prospect in terms of wastewater treatment and electricity generation.
Currently, the practical application of MFC technology is mainly limited by poor electricity generation performance and high cost, and the electrode material is a determinant factor of electricity generation performance and cost. In particular, the anode material directly affects the amount of bacteria attached, the degree of substrate oxidation, and the electron transfer rate. Therefore, it is important to develop research on the development and utilization of novel anode materials.
Disclosure of Invention
Aiming at the problems of poor electricity generation performance, high cost and the like in the prior MFC technology, the invention provides a phosphomolybdic acid/reduced graphene oxide/polyaniline composite material and a preparation method and application thereof.
In order to achieve the purpose of the invention, the embodiment of the invention adopts the following technical scheme:
a preparation method of phosphomolybdic acid/reduced graphene oxide/polyaniline composite material comprises the following steps:
s1: dispersing graphene oxide in deionized water to prepare a graphene oxide turbid liquid; dissolving phosphomolybdic acid in deionized water to prepare phosphomolybdic acid solution; adding aniline into an oxidant solution to prepare an aniline prepolymerization solution;
s2: mixing the graphene oxide suspension with the phosphomolybdic acid solution, adding isopropanol, and performing photocatalytic reaction to obtain phosphomolybdic acid/reduced graphene oxide suspension;
s3: and mixing the aniline prepolymerization solution with the phosphomolybdic acid/reduced graphene oxide turbid liquid, and stirring for reaction to obtain the phosphomolybdic acid/reduced graphene oxide/polyaniline composite turbid liquid.
Compared with the prior art, the preparation method of the phosphomolybdic acid/reduced graphene oxide/polyaniline composite material provided by the invention uses phosphomolybdic acid (PMo)12) And Graphene Oxide (GO) serving as a raw material, carrying out a photocatalytic reaction in the presence of isopropanol, reducing phosphomolybdic acid into heteropoly blue (phosphomolybdic blue) after photocatalysis, contacting graphene oxide, oxidizing phosphomolybdic acid into oxidation state phosphomolybdic acid, reducing graphene oxide into reduced graphene oxide (rGO), wherein the phosphomolybdic acid and the reduced graphene oxide have strong attraction due to electron transfer and electrostatic interaction, and the phosphomolybdic acid and the reduced graphene oxide are combined to form PMo12/rGO；PMo12Mixing rGO with pre-polymerized solution of aniline, polymerizing aniline to form Polyaniline (PAN) and simultaneously mixing with PMo12the/rGO is compounded, and the reduced graphene oxide is negatively charged, while the polyaniline is positively charged, so that PMo is formed through electrostatic interaction12a/rGO/PAN composite. The preparation method has the advantages of simple process, convenient operation, low energy consumption and low cost.
Further, the mass ratio of the graphene oxide to the phosphomolybdic acid to the aniline is 0.10-0.30: 1.00-3.00: 1.00-3.00, and the PMo with high specific surface area, high catalytic activity and high conductivity is ensured to be obtained by controlling the dosage of each component12a/rGO/PAN composite; the dosage ratio of the phosphomolybdic acid to the isopropanol is 1.00-3.00 g: and adding sufficient isopropanol into the solution of 30-90 mu L, wherein the isopropanol can react with hydroxyl radicals generated in the reaction process, so that the hydroxyl radicals are prevented from reducing phosphomolybdic acid, the excited electrons are used for reducing phosphomolybdic acid into phosphomolybdic blue, and the subsequent reaction with graphene oxide is facilitated.
Further, the mass ratio of the aniline to the oxidant is 11-33: and 5-15, ensuring that the aniline monomer is fully reacted into polyaniline.
Further, the mass concentration of the phosphomolybdic acid solution is 16-50 mg/mL-1(ii) a The mass concentration of the graphene oxide turbid liquid is 1.00-3.00 mg/mL-1(ii) a The oxidant is ammonium persulfate, and the mass concentration of the oxidant solution is 0.20-0.60 mmol/mL-1。
Further, the time of the photocatalytic reaction is 8-12 h, so that the full reaction is ensured, and PMo is formed12a/rGO suspension; in the step S3, the temperature of the reaction is 30-40 ℃, the time is 5-7 h, and PMo is guaranteed12Sufficient contact of/rGO with PAN and formation of PMo by electrostatic interaction12a/rGO/PAN composite.
The invention also provides a phosphomolybdic acid/reduced graphene oxide/polyaniline composite material prepared by the preparation method. The space structure of phosphomolybdic acid anions is similar to a cage-shaped spherical structure, the charge density of the surface of the phosphomolybdic acid anions is low, protons can move freely and can be subjected to reversible oxidation reduction without influencing the structure of the phosphomolybdic acid anions, but phosphomolybdic acid is easy to gather in water, so that the specific surface area of the phosphomolybdic acid anions is reduced; the reduced graphene oxide has large specific surface area, good conductivity and certain toxicity to microorganisms; polyaniline has good conductivity and biocompatibility. According to the composite material provided by the invention, the reduced graphene oxide is used as a carrier to load phosphomolybdic acid, so that the phosphomolybdic acid is highly dispersed on the surface of the reduced graphene oxide, the specific surface area and the active site of the composite material are increased, and then the phosphomolybdic acid is combined with polyaniline to effectively improve the conductivity of the composite material, reduce the toxicity of the reduced graphene oxide, improve the biocompatibility and enable the composite material to have excellent bioelectrocatalysis performance.
The invention also provides application of the phosphomolybdic acid/reduced graphene oxide/polyaniline composite material in a microbial fuel cell.
The invention also provides a microbial fuel cell anode material which comprises a base material and the phosphomolybdic acid/reduced graphene oxide/polyaniline composite material deposited on the base material.
The invention also provides a preparation method of the anode material, which comprises the following steps: and (3) depositing the composite material on the surface of a base material by adopting a cyclic voltammetry, and washing and drying to obtain the anode material of the microbial fuel cell.
Further, the substrate is a carbon-based material, specifically, the carbon-based material is carbon cloth, the potential of the cyclic voltammetry is-1.50-0.50V, and the sweep rate is 40-60 mV · s-1The number of scanning turns is 30-50 turns.
The phosphomolybdic acid/reduced graphene oxide/polyaniline composite material provided by the invention modifies a carbon-based material to form a microbial fuel cell anode material, so that the growth environment of bacteria on the surface of an anode is improved. Due to the positive charge of the polyaniline and the good hydrophilicity, conductivity and biocompatibility of the polyaniline, negatively charged bacteria can be attracted to the surface of the electrode to form a biological membrane, the attachment amount of microorganisms is increased, and the electron transfer between the electrogenic microorganisms and the electrode is facilitated, so that the electrogenic performance and the pollutant removal performance of the MFC are improved.
Drawings
FIG. 1 is a blank anode SEM image;
FIG. 2 shows an embodiment PMo of the present invention12SEM image of/rGO/PAN anode;
FIG. 3 is a non-photocatalytic PMo of a comparative example of the present invention12SEM image of/rGO/PAN anode;
FIG. 4 is a graph of the power generation performance of MFCs for different anode materials;
fig. 5 is a graph of perchlorate removal rates of MFC for different anode materials.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
A preparation method of phosphomolybdic acid/reduced graphene oxide/polyaniline composite material comprises the following steps:
s1: dispersing 0.20g of graphene oxide in 100mL of deionized water, stirring and ultrasonically dispersing for 90min to prepare a graphene oxide suspension; dissolving 2g of phosphomolybdic acid in 60mL of deionized water to prepare a phosphomolybdic acid solution; dissolving 2.20g (9.60mmol) of ammonium persulfate in 25mL of deionized water, stirring to prepare an ammonium persulfate solution, dropwise adding 2mL (21.90mmol) of aniline into the ammonium persulfate solution, and stirring to prepare an aniline prepolymerization solution;
s2: mixing the graphene oxide turbid liquid with a phosphomolybdic acid solution, adding 60 mu L of isopropanol, and reacting in a photocatalytic reactor for 10 hours to obtain phosphomolybdic acid/reduced graphene oxide turbid liquid;
s3: and mixing the aniline prepolymerization solution with a phosphomolybdic acid/reduced graphene oxide turbid liquid, and stirring at 35 ℃ for 6 hours to obtain a phosphomolybdic acid/reduced graphene oxide/polyaniline composite turbid liquid.
The phosphomolybdic acid/reduced graphene oxide/polyaniline composite material is applied to the microbial fuel cell, and is used for preparing the anode material of the microbial fuel cell, and the preparation method of the anode material comprises the following steps: adopting a three-electrode system, taking carbon cloth pretreated by nitric acid as a working electrode, a platinum electrode as a counter electrode and a saturated calomel electrode as a reference electrode, placing the three electrodes in turbid liquid of phosphomolybdic acid/reduced graphene oxide/polyaniline composite material, adopting a cyclic voltammetry method, setting the potential to be-1.50-0.50V and the sweep rate to be 50mV s-1Sensitivity of 10-3And performing electro-deposition on the composite material on the surface of the carbon cloth with the number of scanning turns of 40, washing with deionized water, and drying at room temperature to obtain the carbon cloth with the surface modified by phosphomolybdic acid/reduced graphene oxide/polyaniline, namely the MFC anode material.
Example 2
A preparation method of phosphomolybdic acid/reduced graphene oxide/polyaniline composite material comprises the following steps:
s1: dispersing 0.10g of graphene oxide in 100mL of deionized water, stirring and ultrasonically dispersing for 90min to prepare a graphene oxide suspension; dissolving 1.00g of phosphomolybdic acid in 60mL of deionized water to prepare a phosphomolybdic acid solution; dissolving 3.42g (15.00mmol) of ammonium persulfate in 25mL of deionized water, stirring to prepare an ammonium persulfate solution, dropwise adding 3mL (32.90mmol) of aniline into the ammonium persulfate solution, stirring and reacting to prepare an aniline prepolymerization solution;
s2: mixing the graphene oxide turbid liquid with a phosphomolybdic acid solution, adding 30 mu L of isopropanol, and reacting in a photocatalytic reactor for 8 hours to obtain phosphomolybdic acid/reduced graphene oxide turbid liquid;
s3: and mixing the aniline prepolymerization solution with a phosphomolybdic acid/reduced graphene oxide turbid liquid, and stirring for 5 hours at 40 ℃ to obtain a phosphomolybdic acid/reduced graphene oxide/polyaniline composite turbid liquid.
The phosphomolybdic acid/reduced graphene oxide/polyaniline composite material is applied to the microbial fuel cell, and is used for preparing the anode material of the microbial fuel cell, and the preparation method of the anode material comprises the following steps: the method comprises the following steps of (1) adopting a three-electrode system, taking carbon cloth pretreated by nitric acid as a working electrode, a platinum electrode as a counter electrode and a saturated calomel electrode as a reference electrode, placing the three electrodes in turbid liquid of phosphomolybdic acid/reduced graphene oxide/polyaniline composite material, and setting the potential to be-1.50-0.50V by adopting a cyclic voltammetry; the sweeping speed is 60mV s-1(ii) a Sensitivity of 10-3(ii) a And (3) scanning for 50 circles, electrodepositing the composite material on the surface of the carbon cloth, washing with deionized water, and drying at room temperature to obtain the carbon cloth with the surface modified by phosphomolybdic acid/reduced graphene oxide/polyaniline, namely the MFC anode material.
Example 3
A preparation method of phosphomolybdic acid/reduced graphene oxide/polyaniline composite material comprises the following steps:
s1: dispersing 0.30g of graphene oxide in 100mL of deionized water, stirring and ultrasonically dispersing for 90min to prepare a graphene oxide suspension; dissolving 3.00g of phosphomolybdic acid in 60mL of deionized water to prepare a phosphomolybdic acid solution; dissolving 1.14g (5.00mmol) of ammonium persulfate in 25mL of deionized water, stirring to prepare an ammonium persulfate solution, dropwise adding 1mL (11.00mmol) of aniline into the ammonium persulfate solution, stirring and reacting to prepare an aniline prepolymerization solution;
s2: mixing the graphene oxide turbid liquid with a phosphomolybdic acid solution, adding 90 mu L of isopropanol, and reacting in a photocatalytic reactor for 12 hours to obtain phosphomolybdic acid/reduced graphene oxide turbid liquid;
s3: and mixing the aniline prepolymerization solution with a phosphomolybdic acid/reduced graphene oxide turbid liquid, and stirring for 7 hours at 30 ℃ to obtain a phosphomolybdic acid/reduced graphene oxide/polyaniline composite turbid liquid.
The phosphomolybdic acid/reduced graphene oxide/polyaniline composite material is applied to the microbial fuel cell, and is used for preparing the anode material of the microbial fuel cell, and the preparation method of the anode material comprises the following steps: the method comprises the following steps of (1) adopting a three-electrode system, taking carbon cloth pretreated by nitric acid as a working electrode, a platinum electrode as a counter electrode and a saturated calomel electrode as a reference electrode, placing the three electrodes in turbid liquid of phosphomolybdic acid/reduced graphene oxide/polyaniline composite material, and setting the potential to be-1.5-0.5V by adopting a cyclic voltammetry; the sweeping speed is 40mV s-1(ii) a Sensitivity of 10-3(ii) a And (3) performing electro-deposition on the composite material on the surface of the carbon cloth with the number of scanning turns of 30 turns, washing the carbon cloth with deionized water, and drying the carbon cloth at room temperature to obtain the carbon cloth with the surface modified by phosphomolybdic acid/reduced graphene oxide/polyaniline, namely the MFC anode material.
In order to better illustrate the technical solution of the present invention, further comparison is made below by means of a comparative example and an example of the present invention.
Comparative example 1
A preparation method of a non-photocatalytic phosphomolybdic acid/reduced graphene oxide/polyaniline composite material comprises the following steps:
s1: dispersing 0.20g of graphene oxide in 100mL of deionized water, stirring and ultrasonically dispersing for 90min to prepare a graphene oxide suspension; dissolving 2g of phosphomolybdic acid in 60mL of deionized water to prepare a phosphomolybdic acid solution; dissolving 2.20g (9.6mmol) of ammonium persulfate in 25mL of deionized water, stirring to prepare an ammonium persulfate solution, dropwise adding 2mL (21.9mmol) of aniline into the ammonium persulfate solution, stirring and reacting to prepare an aniline prepolymerization solution;
s2: mixing the graphene oxide turbid liquid with a phosphomolybdic acid solution, and reacting at room temperature for 10 hours to obtain non-photocatalytic phosphomolybdic acid/reduced graphene oxide turbid liquid;
s3: and mixing the aniline prepolymerization solution with the suspension of the non-photocatalytic phosphomolybdic acid/reduced graphene oxide, and stirring for 6 hours at 35 ℃ to obtain the suspension of the non-photocatalytic phosphomolybdic acid/reduced graphene oxide/polyaniline composite material.
The application of the non-photocatalytic phosphomolybdic acid/reduced graphene oxide/polyaniline composite material in the microbial fuel cell is used for preparing an anode material of the microbial fuel cell, and the preparation method of the anode material comprises the following steps: the method comprises the following steps of (1) adopting a three-electrode system, taking carbon cloth pretreated by nitric acid as a working electrode, a platinum electrode as a counter electrode and a saturated calomel electrode as a reference electrode, placing the three electrodes in turbid liquid of a non-photocatalytic phosphomolybdic acid/reduced graphene oxide/polyaniline composite material, and setting the potential to be-1.5-0.5V by adopting a cyclic voltammetry; the sweeping speed is 50mV s-1(ii) a Sensitivity of 10-3(ii) a And (3) performing electro-deposition on the composite material on the surface of the carbon cloth with the number of scanning turns of 40 turns, washing the carbon cloth with deionized water, and drying the carbon cloth at room temperature to obtain the carbon cloth with the surface which is not modified by photocatalytic phosphomolybdic acid/reduced graphene oxide/polyaniline, namely the MFC anode material.
To better illustrate the characteristics of the phosphomolybdic acid/reduced graphene oxide/polyaniline composite material provided by the embodiments of the present invention, the MFC anode material (PMo) prepared in example 1 is described below12/rGO/PAN anode), MFC anode material prepared in comparative example 1 (non-photocatalytic PMo)12/rGO/PAN anode) and carbon cloth pretreated with nitric acid (blank anode) were subjected to SEM analysis. Blank anode, PMo12A/rGO/PAN anode and a non-photocatalytic PMo12SEM results for/rGO/PAN anodes are shown in FIGS. 1, 2 and 3, respectively, with the unmodified blank anode surface being clean and smooth, and the PMo anode surface being modified12The surface of the/rGO/PAN modified carbon cloth is loaded with lamellar, granular and cauliflower-like substances, PMo12the/rGO/PAN material is distributed more uniformly, covered more comprehensively and has no photocatalysis PMo12PerGO/PAN Anode vs. PMo12the/rGO/PAN anode is loaded with more lamellar, granular and cauliflower-like substances on the surface and provides larger specific surface area.
In addition, a blank anode, PMo12A/rGO/PAN anode and a non-photocatalytic PMo12/rGO/PAN anodeAn anode for a single-chamber air cathode MFC was incubated with microorganisms, growth medium and contaminants, and the microbial fuel cell output voltage (as shown in FIG. 4) and perchlorate (ClO) were measured4 -) Removal rate (as shown in fig. 5). In ClO4 -The concentration is 420 mg.L-1Under the conditions of (1), PMo12A/rGO/PAN anode, non-photocatalytic PMo12The maximum voltages generated by the/rGO/PAN anode and the blank anode MFC were 156.57mV, 78.92mV and 61.33mV, respectively; ClO of hollow anode MFC in 10h4 -The removal rate is 93.5 percent at most, and the PMo is not photo-catalyzed12ClO of/rGO/PAN anode MFC4 -The removal rate is 99.46% at the maximum, and PMo12ClO of/rGO/PAN anode MFC at 9h4 -The removal rate reaches 100 percent.
The data show that the anode modified by the composite material provided by the embodiment of the invention has effectively increased conductivity and effectively increased surface area, is beneficial to the adhesion of microorganisms on the surface of the anode, and improves the power generation and ClO of MFC4 -The performance is removed. The phosphomolybdic acid/reduced graphene oxide/polyaniline composite materials provided in embodiments 2 and 3 of the present invention have comparable performance and effect to those in embodiment 1.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents or improvements made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (10)
1. A preparation method of phosphomolybdic acid/reduced graphene oxide/polyaniline composite material is characterized by comprising the following steps: the method comprises the following steps:
s1: dispersing graphene oxide in deionized water to prepare a graphene oxide turbid liquid; dissolving phosphomolybdic acid in deionized water to prepare phosphomolybdic acid solution; adding aniline into an oxidant solution to prepare an aniline prepolymerization solution;
s2: mixing the graphene oxide suspension with the phosphomolybdic acid solution, adding isopropanol, and performing photocatalytic reaction to obtain phosphomolybdic acid/reduced graphene oxide suspension;
s3: and mixing the aniline prepolymerization solution with the phosphomolybdic acid/reduced graphene oxide turbid liquid, and stirring for reaction to obtain the phosphomolybdic acid/reduced graphene oxide/polyaniline composite turbid liquid.
2. The method of preparing phosphomolybdic acid/reduced graphene oxide/polyaniline composite material according to claim 1, wherein: the mass ratio of the graphene oxide to the phosphomolybdic acid to the aniline is 0.10-0.30: 1.00-3.00: 1.00-3.00; the dosage ratio of the phosphomolybdic acid to the isopropanol is 1.00-3.00 g: 30-90 mu L.
3. The method of preparing phosphomolybdic acid/reduced graphene oxide/polyaniline composite material according to claim 1, wherein: the mass ratio of the aniline to the oxidant is 11-33: 5 to 15.
4. The method of preparing phosphomolybdic acid/reduced graphene oxide/polyaniline composite material according to claim 3, wherein: the mass concentration of the phosphomolybdic acid solution is 16-50 mg/mL-1(ii) a The mass concentration of the graphene oxide turbid liquid is 1.00-3.00 mg/mL-1(ii) a The oxidant is ammonium persulfate, and the mass concentration of the oxidant solution is 0.2-0.6 mmol/mL-1。
5. The method of preparing phosphomolybdic acid/reduced graphene oxide/polyaniline composite material according to claim 1, wherein: the time of the photocatalytic reaction is 8-12 h; in the step S3, the reaction temperature is 30-40 ℃ and the reaction time is 5-7 h.
6. A phosphomolybdic acid/reduced graphene oxide/polyaniline composite material is characterized in that: prepared by the preparation method of any one of claims 1 to 5.
7. The use of the phosphomolybdic acid/reduced graphene oxide/polyaniline composite material according to claim 6 in a microbial fuel cell.
8. A microbial fuel cell anode material, characterized in that: comprising a substrate and the phosphomolybdic acid/reduced graphene oxide/polyaniline composite of claim 6 deposited on the substrate.
9. The method for preparing an anode material for a microbial fuel cell according to claim 8, wherein: and (3) depositing the composite material on the surface of a base material by adopting a cyclic voltammetry, and washing and drying to obtain the anode material of the microbial fuel cell.
10. The method of preparing a microbial fuel cell anode material of claim 9, wherein: the substrate is a carbon-based material, the potential of cyclic voltammetry is-1.50-0.50V, and the sweep rate is 40-60 mV · s-1The number of scanning turns is 30-50 turns.
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