A loaded MXene ionic liquid gel microsphere composite electrode, a preparation method thereof and application thereof in electrochemical detection of p-aminophenol
By modifying the electrode with PMMA/BMIMPF6/MXene composite material, a PMMA/BMIMPF6 gel microsphere composite electrode loaded with MXene was constructed, which solved the shortcomings of existing methods for detecting p-aminophenol and achieved high-sensitivity and rapid-response electrochemical detection.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- LIAONING UNIVERSITY
- Filing Date
- 2026-03-09
- Publication Date
- 2026-05-29
AI Technical Summary
Existing methods for detecting p-aminophenol suffer from problems such as long sample preparation time, high cost, and insufficient sensitivity, making it difficult to achieve efficient, rapid, and economical electrochemical detection.
Electrodes were modified with PMMA/BMIMPF6/MXene composite materials to construct PMMA/BMIMPF6 gel microsphere composite electrodes loaded with MXene. The regular spherical structure and large specific surface area of PMMA, the high ionic conductivity of BMIMPF6, and the high conductivity and abundant surface functional groups of MXene were used to synergistically enhance the electrocatalytic activity and detection signal of the electrode.
It achieves high sensitivity, rapid response and good selectivity for the detection of p-aminophenol, is suitable for detection needs in complex media, and provides an efficient and economical detection solution.
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Figure CN122109237A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of electrochemical sensor technology, specifically to an ionic liquid gel microsphere composite electrode loaded with MXene, its preparation method, and its application in the electrochemical detection of p-aminophenol. Background Technology
[0002] p-Aminophenol (4-AP) is a typical organic phenolic environmental pollutant, widely used in medicine, cosmetics, antioxidants, dyes, and petroleum additives. 4-AP has teratogenic and carcinogenic effects and can accumulate in aquatic environments and soil, producing persistent toxicity. If 4-AP accidentally enters the body and accumulates excessively, it can cause allergies, dermatitis, and acute kidney and liver failure, even leading to death. Therefore, finding an accurate and sensitive method for analyzing 4-AP is crucial. Phenolic compounds are detected using various techniques, such as high-performance liquid chromatography (HPLC) and fluorescent probes; however, these techniques have drawbacks, such as long sample preparation time and relatively high cost. The electrochemical detection of p-aminophenol offers advantages such as portability, low power consumption, and high sensitivity. Polymethyl methacrylate (PMMA), a hydrophobic polymer with excellent mechanical strength and good chemical stability, forms gel microspheres with a regular spherical structure, controllable particle size distribution, and large specific surface area. These microspheres can serve as loading carriers for functional components, effectively inhibiting nanomaterial aggregation. Simultaneously, they provide unique micro / nano channels for the adsorption and mass transfer of 4-aminophenol, meeting the interfacial requirements of electrochemical detection. 1-Butyl-3-methylimidazolium hexafluorophosphate (BMIMPF6), a typical hydrophobic ionic liquid, possesses ultra-high ionic conductivity, a wide electrochemical stability window, excellent thermal stability, and chemical inertness. It not only optimizes the charge transfer efficiency at the electrode / electrolyte interface and accelerates the redox reaction kinetics of 4-aminophenol on the electrode surface but also enhances the enrichment capacity for target analytes. Hydrophilic MXene nanosheets, with their high conductivity, abundant surface functional groups, and large specific surface area, can effectively amplify detection signals and improve sensing sensitivity. The hydroxyl groups on the surface of MXene form hydrogen bonds with the carbonyl oxygen and alkoxy oxygen in the PMMA ester group, which can be uniformly dispersed on the surface of PMMA / BMIMPF6 gel microspheres. At the same time, the introduction of BMIMPF6 can construct continuous ion transport channels, synergistically improving the conductivity, mechanical stability and specific response to p-aminophenol of the composite system. Summary of the Invention
[0003] The purpose of this invention is to provide a PMMA / BMIMPF6 / MXene / CC composite electrode for the detection of p-aminophenol. Therefore, this invention uses a PMMA / BMIMPF6 / MXene composite material to modify the electrode, constructing a sensitive composite electrode for the detection of p-aminophenol. This composite electrode exhibits excellent electrocatalytic activity, a wide linear range, and a low detection limit for p-aminophenol.
[0004] To achieve the above objectives, the technical solution adopted by the present invention is: a PMMA / BMIMPF6 gel microsphere composite electrode loaded with MXene, the preparation method of which includes the following steps:
[0005] 1) Preparation of PMMA / BMIMPF6 / MXene / CC composite electrode: A few layers of MXene were added to deionized water, and PMMA / BMIMPF6 gel microsphere powder was dispersed in deionized water. The PMMA / BMIMPF6 gel microsphere dispersion was added to the MXene aqueous solution, and stirred and ultrasonically vibrated under a nitrogen atmosphere. The mixture was filtered, washed with deionized water, and the filter cake was collected and freeze-dried to obtain PMMA / BMIMPF6 / MXene powder. The powder was dispersed in anhydrous ethanol, ultrasonically vibrated, and dropped onto carbon cloth. It was then dried at room temperature to obtain the PMMA / BMIMPF6 / MXene / CC composite electrode.
[0006] 2) Place the PMMA / BMIMPF6 / MXene / CC composite electrode obtained in step 1) at room temperature for 2-3 hours to allow the electrode material and carbon cloth to fully bond together, thus obtaining the PMMA / BMIMPF6 / MXene / CC composite electrode.
[0007] The above-mentioned PMMA / BMIMPF6 / MXene / CC composite electrode, wherein the few-layer MXene is prepared by the following steps:
[0008] LiF was added to hydrochloric acid and stirred until fully dissolved to obtain an etchant. Ti3AlC2 was gradually added to the etchant over 30 min and stirred at 40 °C for 48 h to obtain a mixture. The mixture was washed several times with dilute hydrochloric acid and deionized water. After each wash, when the pH of the supernatant was ≥5, the precipitate was collected, dissolved in deionized water, and under a nitrogen-protected atmosphere, sonicated, centrifuged, and the supernatant was collected and freeze-dried to obtain a few-layer MXene.
[0009] In the aforementioned PMMA / BMIMPF6 / MXene / CC composite electrode, the concentration of the hydrochloric acid is 6 M, and the concentration of the dilute hydrochloric acid is 1 M.
[0010] The PMMA / BMIMPF6 / MXene / CC composite electrode described above, wherein the PMMA / BMIMPF6 gel microspheres are prepared by the following steps:
[0011] PVP was ultrasonically dispersed in anhydrous ethanol, and then BMIMPF6, MMA, and AIBN were mixed evenly and ultrasonically dispersed dropwise into the PVP dispersion. The reaction was sealed under a nitrogen atmosphere. After centrifugation and washing with deionized water, the precipitate was collected and freeze-dried to obtain PMMA / BMIMPF6 gel microspheres.
[0012] The PMMA / BMIMPF6 / MXene / CC composite electrode described above has a mass ratio of PVP:BMIMPF6:MMA:AIBN of 4:2:5:0.1.
[0013] The aforementioned PMMA / BMIMPF6 / MXene / CC composite electrode was reacted at 70°C for 24 hours.
[0014] The above-mentioned PMMA / BMIMPF6 / MXene / CC composite electrode is used in the electrochemical detection of p-aminophenol.
[0015] The above application is performed as follows: using the above-mentioned PMMA / BMIMPF6 / MXene / CC composite electrode as the working electrode, the Ag / AgCl electrode as the reference electrode, and the platinum wire as the counter electrode, the three-electrode system is placed in a phosphate buffer solution containing p-aminophenol for electrochemical testing.
[0016] The composite electrode described in this invention achieves synergistic performance and structural complementarity among its components. PMMA gel microspheres, with their regular spherical structure, provide a stable loading substrate for MXene, effectively inhibiting nanosheet aggregation and constructing micro / nano mass transfer channels. BMIMPF6 ionic liquid, with its high ionic conductivity and enrichment characteristics, optimizes the charge transfer efficiency at the electrode / electrolyte interface, accelerating the redox kinetics of p-aminophenol. MXene, with its high conductivity and abundant surface functional groups, significantly amplifies the detection signal. The synergistic effect of these three components endows the electrode with excellent electrocatalytic activity and specific recognition capabilities. This invention not only provides a novel electrochemical sensing scheme for the efficient, rapid, and economical detection of phenolic pollutants such as p-aminophenol in aquatic environments, but also offers new ideas for the design and development of functional composite electrochemical electrode materials.
[0017] The beneficial effects of this invention are:
[0018] 1. This invention cleverly utilizes the structural advantages and characteristics of PMMA. The resulting gel microspheres have a regular spherical structure, controllable particle size distribution, and large specific surface area. They can not only serve as a high-quality support to effectively inhibit the aggregation of MXene nanosheets, but also construct unique micro-nano channels, ensuring the efficient adsorption and rapid mass transfer of 4-AP. They perfectly meet the interface requirements of electrochemical detection and lay a stable structural foundation.
[0019] 2. This invention achieves complementary and synergistic performance through the synergistic composite design of PMMA, BMIMPF6, and MXene: Hydrophobic BMIMPF6 possesses advantages such as ultra-high ionic conductivity and a wide electrochemical stability window, which can optimize the charge transfer efficiency at the electrode / electrolyte interface, accelerate the kinetics of 4-AP redox reaction, and enhance the enrichment ability of target analytes; Hydrophilic MXene, with its high conductivity, abundant surface functional groups, and large specific surface area, amplifies the detection signal and improves sensing sensitivity; Furthermore, the hydroxyl groups on the surface of MXene form hydrogen bonds with the carbonyl oxygen and alkoxy oxygen in the ester group of PMMA, making it uniformly dispersed on the surface of gel microspheres. Combined with the continuous ion transport channels constructed by BMIMPF6, this synergistically improves the conductivity, mechanical stability, and specific response capability to 4-AP of the composite system.
[0020] 3. This invention successfully fabricates a high-performance composite electrode through the rational proportioning of the three components and the precise design of the composite system. This electrode fully leverages the synergistic advantages of each component, exhibiting excellent comprehensive performance in 4-AP detection. It not only demonstrates high detection sensitivity and fast response speed but also good stability and selectivity, making it suitable for detection requirements in complex media. Its fabrication process is simple and controllable, providing a novel solution for the efficient, accurate, and economical detection of phenolic pollutants such as 4-AP in the environment, while also offering new insights for the design and development of high-performance electrochemical sensing materials. Attached Figure Description
[0021] Figure 1 These are SEM images of MAX, MXene, PMMA / BMIMPF6, and PMMA / BMIMPF6 / MXene.
[0022] Figure 2 These are the infrared spectra of BMIMPF6, MXene, PMMA / BMIMPF6, and PMMA / BMIMPF6 / MXene.
[0023] Figure 3 These are XRD patterns of MAX, MXene, PMMA / BMIMPF6, and PMMA / BMIMPF6 / MXene.
[0024] Figure 4 Different modified electrodes in [Fe(CN)6] 3- / 4-Electrochemical impedance spectroscopy in solution;
[0025] These are CC, BMIMPF6 / CCi, PMMA / BMIMPF6 / CC, and PMMA / BMIMPF6 / MXene / CC, respectively.
[0026] Figure 5 The CV curves for detecting p-aminophenol using CC, BMIMPF6 / CC, PMMA / BMIMPF6 / CC, and PMMA / BMIMPF6 / MXene / CC modified electrodes in PBS solution at pH 6.5 are shown.
[0027] Figure 6 The image shows the CV curves of 1 mM p-aminophenol measured in PBS at pH 6.5 using a PMMA / BMIMPF6 / MXene / CC composite electrode at different scan rates.
[0028] Figure 7 It is a linear graph of scan rate versus the peak current of p-aminophenol reduction.
[0029] Figure 8 It is a differential pulse voltammogram at different concentrations of p-aminophenol.
[0030] Figure 9 This is a calibration graph showing the peak current as a function of p-aminophenol concentration. Detailed Implementation
[0031] To enable those skilled in the art to better understand the technical solution of the present invention, the present invention will be further described in detail below with reference to the accompanying drawings and embodiments.
[0032] All raw materials used in the examples were commercially available.
[0033] Example 1: Fabrication of a PMMA / BMIMPF6 / MXene / CC composite electrode
[0034] (a) The preparation method is as follows
[0035] 1. Preparation of few-layer MXene
[0036] 2.0 g of lithium fluoride was slowly dissolved in 40 mL of 9 M hydrochloric acid and stirred for 10 min to ensure complete dissolution. Then, 1.0 g of Ti3AlC2 was slowly added over 30 min, and the mixture was stirred at 40 °C for 48 h. After the reaction was complete, the mixture was first washed twice with dilute hydrochloric acid (1 M) to remove excess lithium fluoride, then washed with deionized water and centrifuged at 3500 rpm for 5 min each time, until the pH of the supernatant was >5. The precipitate was then collected. The mixture was dissolved in 100 mL of water and sonicated for 2.5 h under a nitrogen atmosphere. Finally, it was centrifuged at 3500 rpm for 1 h, and the supernatant was collected and freeze-dried to obtain a few-layer MXene.
[0037] 2. Preparation of PMMA / BMIMPF6 gel microspheres
[0038] 4 g PVP was ultrasonically dispersed in 50 mL of anhydrous ethanol. Then, 2 g BMIMPF6, 5 g MMA, and 0.1 g AIBN were mixed evenly and ultrasonically dispersed dropwise into the PVP dispersion. The mixture was sealed and reacted at 70 °C for 24 h under a nitrogen atmosphere. After centrifugation and washing with deionized water, the precipitate was collected and freeze-dried to obtain PMMA / BMIMPF6 gel microspheres.
[0039] 3. Fabrication of PMMA / BMIMPF6 / MXene / CC composite electrode
[0040] 50 mg of few-layer MXene was added to 50 mL of deionized water, and 200 mg of PMMA / BMIMPF6 gel microsphere powder was dispersed in 50 mL of deionized water. The above gel microsphere dispersion was added to 50 mL of MXene aqueous solution, and stirred for 30 min under a nitrogen atmosphere, followed by ultrasonic vibration for 10 min. The mixture was then filtered, washed with deionized water, and the filter cake was collected and freeze-dried to obtain PMMA / BMIMPF6 / MXene. 2 mg of PMMA / BMIMPF6 / MXene powder was dispersed in 1 mL of anhydrous ethanol, ultrasonicated for 10 min, and then dropped onto a 1.0 cm × 1.5 cm piece of carbon cloth. The mixture was then dried at room temperature to obtain the PMMA / BMIMPF6 / MXene / CC composite electrode.
[0041] (II) Testing
[0042] Figure 1The SEM image of the MAX phase (Ti3AlC2) in Figure A shows a dense three-dimensional layered structure. The structure of the MAX phase etched with LiF and HCl exhibits a transformation from blocky to lamellar. Figure B shows the thin lamellar structure of MXene. Figure C shows that the prepared ionic liquid gel microspheres PMMA / BMIMPF6 are monodisperse spherical particles. Figure D clearly shows that the gel microspheres were successfully intercalated between the MXene sheets; the elemental distribution provides a direct visual indication of the successful preparation of PMMA / BMIMPF6 / MXene.
[0043] Figure 2 These are the infrared spectra of BMIMPF6, PMMA / BMIMPF6, PMMA / BMIMPF6 / MXene, and MXene. MXene is located at 3445 cm⁻¹ in the spectra. -1 The absorption band observed nearby belongs to the absorption peak of -OH at 620 cm⁻¹. -1 The characteristic peak at 835 cm⁻¹ indicates Ti-O. -1 The PF characteristic peak at 1732 cm⁻¹ confirms the presence of BMIMPF₆. -1 The C=O stretching vibration in the region is a characteristic absorption peak of PMMA, and at 3448 cm⁻¹... -1 The peak corresponds to the stretching vibration of OH formed by the hydrolysis of ester bonds, which also proves the existence of hydrogen bonds. These results show that the spectrum of the PMMA / BMIMPF6 / MXene composite material exhibits the characteristic absorption peaks of MXene and BMIMPF6.
[0044] Figure 3 These are XRD patterns of different materials. Figure 3 As can be seen, the (104) diffraction peak (JCPDS no. 52-0875) corresponding to Ti3AlC2 at 39.0° completely disappears in MXene, indicating a significant etching effect on the Al layer inside Ti3AlC2. This indicates that MXene preparation was successful. In addition, the (002) diffraction peak shifts to the left, the interlayer spacing increases, and PMMA / BMIMPF6 gel microspheres are successfully intercalated between the MXene sheets.
[0045] Example 2: Application of PMMA / BMIMPF6 / MXene / CC composite electrode in the detection of phenolic contaminants
[0046] The method is as follows: Using the PMMA / BMIMPF6 / MXene / CC composite electrode prepared in Example 1 as the working electrode, the Ag / AgCl electrode as the reference electrode, and a platinum wire as the counter electrode, the three-electrode system was placed in 10 ml of p-nitrophenol phosphate buffer solution. Electrochemical measurements were performed using a CHI760e electrochemical workstation, employing cyclic voltammetry, differential pulse voltammetry, and electrochemical impedance spectroscopy. A standard electrochemical curve was plotted based on the electrochemical signal data measured.
[0047] Working electrode selection: The PMMA / BMIMPF6 / MXene / CC composite electrode prepared in Example 1 was replaced with a CC electrode, a BMIMPF6 / CC composite electrode, and a PMMA / BMIMPF6 / CC composite electrode, respectively.
[0048] (a) PMMA / BMIMPF6 / MXene / CC composite electrode, CC electrode, BMIMPF6 / CC composite electrode, PMMA / BMIMPF6 / CC composite electrode in [Fe(CN)6] 3- / 4- Electrochemical response in KCl solution
[0049] Take 10 mL containing 5 mM [Fe(CN)6] 3- / 4- The 0.1 M KCl solution was placed in a beaker. A three-electrode system was used, with the Ag / AgCl electrode as the reference electrode, the platinum wire as the counter electrode, and the working electrodes being a PMMA / BMIMPF6 / MXene / CC composite electrode, a CC electrode, a BMIMPF6 / CC composite electrode, and a PMMA / BMIMPF6 / CC composite electrode, respectively. Electrochemical impedance spectroscopy was performed using a CHI760e electrochemical workstation. The test results are as follows: Figure 4 As shown.
[0050] Figure 4 These are PMMA / BMIMPF6 / MXene / CC composite electrodes, CC electrodes, BMIMPF6 / CC composite electrodes, and PMMA / BMIMPF6 / CC composite electrodes in [Fe(CN)6]. 3- / 4- Electrochemical impedance spectroscopy in solution. Figure 4 It is evident that the charge transfer resistance of the BMIMPF6 / CC and PMMA / BMIMPF6 / MXene / CC composite electrodes is much lower than that of CC and PMMA / BMIMPF6 / CC. This is because the high conductivity of MXene and BMIMPF6 promotes electron transfer and reduces the Rct value.
[0051] (II) Detection performance of PMMA / BMIMPF6 / MXene / CC composite electrode, CC electrode, BMIMPF6 / CC composite electrode, and PMMA / BMIMPF6 / CC composite electrode
[0052] Take 10 mL of 0.2 mol / L phosphate buffer solution with pH 6.5 and place it in a beaker. Then add p-aminophenol to the beaker to make its concentration 1 mM and mix well.
[0053] A three-electrode system was used, with the Ag / AgCl electrode as the reference electrode and the platinum wire as the counter electrode. The working electrodes were a PMMA / BMIMPF6 / MXene / CC composite electrode, a CC electrode, a BMIMPF6 / CC composite electrode, and a PMMA / BMIMPF6 / CC composite electrode, respectively. Electrochemical measurements were performed using a CHI760e electrochemical workstation with a potential scan range of -0.4–0.8 V. p-Aminophenol was detected, and the results are as follows: Figure 5 As shown.
[0054] Figure 5 This is a CV graph showing the detection of p-aminophenol using different modified electrodes in PBS solution at pH 6.5. Figure 5 It is evident that the PMMA / BMIMPF6 / MXene / CC composite electrode exhibits the strongest current response, demonstrating that the addition of PMMA / BMIMPF6 and MXene can effectively enhance the detection signal of this electrode.
[0055] (III) Catalytic performance of PMMA / BMIMPF6 / MXene / CC composite electrode for the detection of different concentrations of p-aminophenol
[0056] The effect of scan rate on peak current was investigated using cyclic voltammetry in the range of 25–400 mV / s. Figure 6 As shown, the reduction peak current of p-aminophenol increases with increasing scan rate from 25 mV / s to 400 mV / s. The results obtained after linear fitting are as follows: Figure 7 As shown, the reduction peak current of p-aminophenol is linearly related to the scan rate. The equation shows that the reduction peak current of p-aminophenol is proportional to the first power of the scan rate. The results indicate that the typical mechanism controlling the kinetics of p-aminophenol on the PMMA / BMIMPF6 / MXene / CC composite electrode surface is diffusion-controlled electrochemical process.
[0057] p-Aminophenol was added to a phosphate buffer solution at pH 6.5 to achieve concentrations of 0, 2, 4, 6, 8, 10, 50, 90, 130, 170, 210, and 250 μM. The PMMA / BMIMPF6 / MXene / CC composite electrode prepared in Example 1 was used as the working electrode, the Ag / AgCl electrode as the reference electrode, and a platinum wire as the counter electrode. Electrochemical measurements were performed using a CHI760e electrochemical workstation with a potential scan range of -0.2–0.4 V. p-Aminophenol was then detected.
[0058] Figure 8 It is a differential pulse voltammogram at different concentrations of p-aminophenol. Figure 9 This is a calibration graph showing the peak current as a function of p-aminophenol concentration. (From...) Figure 8 As shown, the oxidation peak current of the composite electrode increases with the gradual increase in the concentration of p-nitrophenol in the phosphate buffer solution, proving that the PMMA / BMIMPF6 / MXene / CC composite electrode prepared in this invention has good catalytic recognition performance for p-aminophenol. Figure 9 As shown, the DPV oxidation current gradually increases with increasing p-aminophenol concentration. A good linear relationship exists between the oxidation peak current and the p-aminophenol concentration in the range of 0 μM–250 μM, and the linear equation is I(A) = 2.0774 × 10⁻⁶ in the range of 0 μM–10 μM. -5 C(M) + 4.151 × 10 -5 (R 2 =0.994), and the linear equation in the range of 10 μM-250 μM is I(A)=2.59733×10 -6 C(M) + 2.38648 × 10 -4 (R 2 =0.998), and the detection limit is 108.3 nM.
Claims
1. A PMMA / BMIMPF6 gel microsphere composite electrode loaded with MXene, characterized in that, The preparation method includes the following steps: 1) Preparation of PMMA / BMIMPF6 / MXene / CC composite electrode: A few layers of MXene were added to deionized water, and PMMA / BMIMPF6 gel microsphere powder was dispersed in deionized water. The PMMA / BMIMPF6 gel microsphere dispersion was added to the MXene aqueous solution, and stirred and ultrasonically vibrated under a nitrogen atmosphere. The mixture was filtered, washed with deionized water, and the filter cake was collected and freeze-dried to obtain PMMA / BMIMPF6 / MXene powder. The powder was dispersed in anhydrous ethanol, ultrasonically vibrated, and dropped onto carbon cloth. It was then dried at room temperature to obtain the PMMA / BMIMPF6 / MXene / CC composite electrode. 2) Place the PMMA / BMIMPF6 / MXene / CC composite electrode obtained in step 1) at room temperature for 2-3 hours to allow the electrode material and carbon cloth to fully bond together, thus obtaining the PMMA / BMIMPF6 / MXene / CC composite electrode.
2. The PMMA / BMIMPF6 gel microsphere composite electrode loaded with MXene as described in claim 1, characterized in that, The preparation method of the few-layer MXene includes the following steps: LiF was added to hydrochloric acid and stirred until fully dissolved to obtain an etchant. Ti3AlC2 was gradually added to the etchant over 30 min and stirred at 40 °C for 48 h to obtain a mixture. The mixture was washed several times with dilute hydrochloric acid and deionized water. After each wash, when the pH of the supernatant was ≥5, the precipitate was collected, dissolved in deionized water, and under a nitrogen-protected atmosphere, sonicated, centrifuged, and the supernatant was collected and freeze-dried to obtain a few-layer MXene.
3. The PMMA / BMIMPF6 gel microsphere composite electrode loaded with MXene as described in claim 2, characterized in that, The concentration of the hydrochloric acid is 6 M, and the concentration of the dilute hydrochloric acid is 1 M.
4. The PMMA / BMIMPF6 gel microsphere composite electrode loaded with MXene as described in claim 1, characterized in that, The preparation method of the PMMA / BMIMPF6 gel microspheres includes the following steps: PVP was ultrasonically dispersed in anhydrous ethanol, and then BMIMPF6, MMA, and AIBN were mixed evenly and ultrasonically dispersed dropwise into the PVP dispersion. The reaction was sealed under a nitrogen atmosphere. After centrifugation and washing with deionized water, the precipitate was collected and freeze-dried to obtain PMMA / BMIMPF6 gel microspheres.
5. The PMMA / BMIMPF6 gel microsphere composite electrode loaded with MXene as described in claim 4, characterized in that, The mass ratio of PVP:BMIMPF6:MMA:AIBN is 4:2:5:0.
1.
6. The PMMA / BMIMPF6 gel microsphere composite electrode loaded with MXene as described in claim 4, characterized in that, The reaction was carried out at 70°C for 24 hours.
7. The application of the PMMA / BMIMPF6 gel microsphere composite electrode loaded with MXene as described in claim 1 in the electrochemical detection of p-aminophenol.
8. The application as described in claim 7, characterized in that, The method is as follows: using the PMMA / BMIMPF6 / MXene / CC composite electrode as described in claim 1 as the working electrode, the Ag / AgCl electrode as the reference electrode, and the platinum wire as the counter electrode, the three-electrode system is placed in a phosphate buffer solution containing p-aminophenol for electrochemical testing.