CN110687173A - Electrochemical method for in-situ monitoring of membrane surface pollution condition and monitoring device - Google Patents
Electrochemical method for in-situ monitoring of membrane surface pollution condition and monitoring device Download PDFInfo
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- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/041—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/22—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating capacitance
Abstract
The invention relates to an electrochemical method for in-situ monitoring of the pollution condition of a membrane surface. The membrane to be measured is placed in a four-electrode system device to enable the membrane surface to be contacted with an electrolyte solution to form a series circuit, current or voltage signals obtained by an electrochemical impedance spectroscopy are reflected in electrochemical workstation software to form an impedance spectrum or an admittance spectrum, then an equivalent circuit model is selected to perform nonlinear least square fitting and analysis on the impedance spectrum or the admittance spectrum, and electrochemical parameters of a pollution layer and a membrane-solution interface layer in the measured membrane pollution process are obtained through fitting after electrochemical information of the system is obtained. The invention has the beneficial effects that: the method has the advantages of high accuracy, simplicity, practicability, non-damage to the measurement of the membrane, contribution to improving the test precision and reducing the errors caused by the nonuniformity of the membrane, and capability of effectively representing the change of the electrochemical characteristics of the membrane and the interface thereof in the membrane pollution process.
Description
Technical Field
The invention relates to the technical field of membranes, in particular to an electrochemical method for in-situ monitoring of membrane surface pollution condition and a monitoring device thereof.
Background
The membrane separation technology has been widely used in the fields of sewage treatment, seawater desalination, medicine, food processing, medical treatment, chemical industry, bionics and the like due to the characteristics of high efficiency, energy conservation, environmental protection, easy control and the like. However, membrane fouling is one of the main causes that restrict the application of membrane technology. Membrane fouling is the process of depositing contaminants on the membrane surface, where the contaminants in the water can adhere to the membrane surface and/or enter the membrane interior by electrostatic and chemical forces and form a fouling layer on the membrane surface. Membrane fouling causes a decrease in membrane performance such as flux and conductivity, and the phenomena of increased power consumption, shortened membrane life, etc. caused by membrane fouling have become major problems limiting the application and economic feasibility of membrane devices.
Membrane fouling is reported in many documents, most of which focuses on characterization of membrane physical properties and membrane material characteristics, and membrane fouling conditions cannot be monitored in real time. The development and application of a suitable nondestructive online membrane pollution monitoring technology have important application value for effectively quantifying the prevention and treatment of membrane pollution and the effect of membrane cleaning. The membrane pollution process is accompanied by the change of the electrochemical characteristics of the membrane surface, and the degree and the trend of the membrane pollution are related to the physical, chemical and electrochemical characteristics of the membrane surface and the types of pollutants. The pollution tendency and degree of the membrane can be evaluated through the change of electrochemical characteristics of the membrane and the interface thereof in the membrane pollution process.
Disclosure of Invention
The invention aims to provide a simple and reliable electrochemical method for in-situ monitoring of the membrane surface pollution condition and a monitoring device thereof.
In order to solve the technical problems, the invention adopts the technical scheme that: an electrochemical method for in-situ monitoring of the contamination of a membrane surface, comprising the steps of:
(1) preparing an electrolyte solution to be tested;
(2) putting a film to be tested into a film clamping part in a four-electrode testing device;
(3) connecting a four-electrode testing device with an electrochemical workstation and a gear pump, starting the gear pump, pumping the electrolyte solution prepared in the step (1) into the four-electrode testing device, and operating for a period of time to stabilize the condition of a testing membrane;
(4) applying a small-amplitude disturbance signal and sinusoidal alternating voltage or current to a monitoring device through an electrochemical workstation by adopting an electrochemical impedance spectroscopy method, collecting a response current or voltage signal by the electrochemical workstation, and reflecting the response current or voltage signal in Nova software carried by the electrochemical workstation to form an impedance spectrum EIS or an admittance spectrum;
(5) stopping the operation of the four-electrode testing device, disconnecting the four-electrode testing device from the electrochemical workstation and the gear pump, disassembling the four-electrode testing device and taking out the testing membrane;
(6) reassembling the four-electrode testing device, connecting the four-electrode testing device with an electrochemical workstation and a gear pump, and performing a blank experiment to obtain the resistance value of a blank solution;
(7) carrying out nonlinear least square fitting and analysis on the impedance spectrum or the admittance spectrum obtained in the step (4) by using an equivalent circuit model to obtain electrochemical characteristic information of the test membrane, wherein the calculation formula is
Where n is the number of data points selected for calculation, g'i，g″iRespectively the real part and the imaginary part of the admittance data;
the electrolyte solution in the step (1) is a NaCl solution, the purity level of inorganic salt used for preparing the electrolyte solution is superior purity, the used water is deionized water, and the electrolyte solution is added with typical pollutants (such as bovine serum albumin or sodium alginate) with different concentrations to simulate pollutants in natural water.
Soaking the membrane to be tested in the step (2) in 0.5M NaCl solution for 24h before testing, and replacing the solution for 4 times to remove the residual chemical solvent in the membrane.
The electrolyte solution in the step (3) is circulated.
The environmental temperature of the electrolyte solution prepared in the step (3) is 10-40 ℃.
The EIS testing frequency in the step (4) can be 1000000-0.01 Hz, wherein the testing frequency sections corresponding to different films are different, the amplitude of the alternating voltage is 0.01V, and 50 frequency points are taken in each test; the open circuit potential before the test was started was set to the initial potential of the device.
The equivalent circuit model in the step (7) is formed by the sum R of the resistances of the solution and the filmm+sThe test membrane is formed by connecting four parts of circuit elements of an electric double layer, a diffusion boundary layer and a pollution layer which are naturally formed in a solution from left to right in series, wherein the membrane and the solution are formed by a resistor Rm+sThe electric double layer is represented by a resistor RedlAnd phase angle constant element QdIn parallel, the diffusion boundary layer is represented by a resistor RdAnd phase angle constant element QdParallel, the contamination layer is represented by a resistor RfoulingAnd phase angle constant element QfoulingParallel representation; the fitting results in the sum of the resistances R of the solution and the membranem+sResistance value R of electric double layeredlCapacitance value C of the electric double layeredlResistance value R of diffusion boundary layerdCapacitance value C of diffusion boundary layerdResistance value R of the contamination layerfoulingAnd the capacitance C of the contamination layerfoulingThe resistance Rs of the solution is determined by a blank test, the resistance R of the pure filmmFrom the sum R of the resistances of the solution and the membranem+sMinus the resistance R of the solutionsAnd (6) obtaining.
The utility model provides a measuring device of electrochemistry method of in situ monitoring membrane surface pollution condition, includes test cell, double-layered membrane part, four electrode system and outside electrochemistry workstation, the gear pump of bilateral symmetry rotation setting, four electrode system includes working electrode, counter electrode and two reference electrodes, working electrode and counter electrode are the Ag AgCl electrode of disc form respectively, two reference electrodes are the Ag AgCl electrode of placing in lujin capillary.
The test tank is formed with four water passageways, and the gear pump is squeezed into electrolyte solution from the water passageway of test tank both sides lower limit respectively, and electrolyte solution then flows from the water passageway of test tank both sides upper limit respectively to guarantee that the test membrane both sides environment that awaits measuring is unanimous.
The diameter of the Ag/AgCl electrode is 10 mm; the effective membrane area of the membrane clamping part is 3.14cm2。
The invention has the beneficial effects that: the method and the device for acquiring the electrochemical characteristics of the membrane surface can measure the electrochemical properties of a test membrane, a surface interface layer and a pollution layer by an EIS method. The resistance value and the capacitance value in the equivalent circuit can reflect the structure of a testing membrane system, so that the equivalent circuit is utilized to fit impedance spectrum data, the conductivity value and the capacitance value of the interface layer and the pollution layer can be quantitatively analyzed, and the pollution tendency and degree of the membrane can be further evaluated. The device is accurate, reliable and simple to operate, and is suitable for in-situ monitoring of the surface pollution conditions of various films.
Drawings
FIG. 1 is a schematic diagram of an experimental setup for an electrochemical method of in situ monitoring of membrane surface contamination according to the present invention;
FIG. 2 is a schematic diagram of the overall structure of the four-electrode system test apparatus of the present invention;
FIG. 3 is a schematic structural diagram of a film clamping component of the four-electrode system testing device of the present invention;
FIG. 4 is an equivalent circuit model of the present invention for non-linear least squares fitting of impedance spectra;
FIG. 5 is electrochemical impedance spectroscopy data and fitted curves of the membrane of the invention after AEM-Type I contamination at a flow rate of 2cm/s, a temperature of 20. + -. 2 ℃, a solution of 0.5mol/LNaCl + 0.5% SA, and a time of 57.4 h;
FIG. 6 is a graph of AEM-Type II membranes of the invention subjected to S at various flow ratesA fouling membrane resistance (R)m) And total resistance (R) of the systemtotal) A change over time;
FIG. 7 is the membrane resistance (R) of the membrane AEM-Type II of the invention when contaminated with SA at different NaCl concentrationsm) And film fouling layer property changes;
FIG. 8 is the membrane resistance (R) of the membrane AEM-Type II of the inventionm) And the change in the nature of the fouling layer over time during the contamination by SA/BSA.
In the figure:
1. working electrode, counter electrode 2, reference electrode
3. Film clamping component 4 and electrochemical workstation
5. Computer 6, left side water outlet channel
7. Right side water outlet channel 8 and left side water inlet channel
9. Right water inlet channel
Detailed Description
The invention is described in further detail below with reference to the following figures and detailed description:
as shown in fig. 1, an electrochemical method for in-situ monitoring of the contamination condition of a membrane surface comprises the following steps:
(1) preparing an electrolyte solution to be tested;
(2) putting a film to be tested into a film clamping part in a four-electrode testing device;
(3) connecting a four-electrode testing device with an electrochemical workstation and a gear pump, starting the gear pump, pumping the electrolyte solution prepared in the step (1) into the four-electrode testing device, and operating for a period of time to stabilize the condition of a testing membrane;
(4) applying a small-amplitude disturbance signal and sinusoidal alternating voltage or current to a monitoring device through an electrochemical workstation by adopting an electrochemical impedance spectroscopy method, collecting a response current or voltage signal by the electrochemical workstation, and reflecting the response current or voltage signal in Nova software carried by the electrochemical workstation to form an impedance spectrum EIS or an admittance spectrum;
(5) stopping the operation of the four-electrode testing device, disconnecting the four-electrode testing device from the electrochemical workstation and the gear pump, disassembling the four-electrode testing device and taking out the testing membrane;
(6) reassembling the four-electrode testing device, connecting the four-electrode testing device with an electrochemical workstation and a gear pump, and performing a blank experiment to obtain the resistance value of a blank solution;
(7) and (4) carrying out nonlinear least square fitting and analysis on the impedance spectrum or the admittance spectrum obtained in the step (4) by using an equivalent circuit model to obtain electrochemical characteristic information of the test membrane.
An electrochemical measuring device for obtaining the contamination condition of the membrane surface, which implements the above method, is shown in fig. 2 and 3, and comprises a working electrode, a counter electrode, a reference electrode, and a membrane sandwiching member. And (4) placing the pretreated test membrane into a membrane clamping part, and fixing by using screws. And all the parts are connected in series and fixed by long screws. Electrolyte solution for testing is placed in the constant temperature water bath, two gear pump inlets are connected through rubber guide pipes, then the electrolyte solution is pumped into water inlets 8 and 9 of the testing device, and then returns to the constant temperature water bath from water outlets 6 and 7 of the testing device to flow circularly. The blank experiment is no film in the four-electrode testing device, and the rest steps are the same.
Specific example 1:
sodium Alginate (SA) is selected as a typical pollutant in membrane pollution research, and an AEM-TypeI-0.5 mol/L NaCl + 0.5% SA solution system is used. And putting the ion exchange membrane to be tested into a four-electrode system testing device, and then connecting the four-electrode system testing device with the electrochemical workstation and the two gear pumps. Pouring the prepared solution with the concentration of 0.5mol/LNaCl + 0.5% SA into a liquid storage tank, and placing the liquid storage tank into a constant temperature tank, wherein the set temperature is 20 ℃. Starting the gear pump, and adjusting the flow rate of the gear pump to ensure that the flow rate is 2 cm/s. And after the flow and the potential difference are stable, obtaining an impedance spectrogram by an electrochemical impedance spectroscopy method of an electrochemical workstation. The same measurement was carried out using AEM-TypeII-0.5 mol/L NaCl + 0.5% SA solution system, and then changing the flow rate of the gear pump to 2, 3, and 4cm/s, respectively, to examine the mechanism of influence of the flow rate on the contamination process. All the above experiments were performed under the same conditions as the above experiments.
The obtained impedance spectrum was fitted by the non-linear least squares method using the equivalent circuit model shown in fig. 4, and the obtained impedance spectrum and the fitting curve were shown in fig. 5. And obtaining electrochemical information such as the membrane resistance value, the total resistance value and the like of the measured ion exchange membrane according to the fitting result. The effect of flow rate on membrane resistance and interface characteristics after fouling is shown in figure 6.
Specific example 2:
sodium Alginate (SA) is selected as a typical pollutant in membrane pollution research, and an AEM-TypeII-0.1 mol/L NaCl + 0.5% SA solution system is used. And putting the ion exchange membrane to be tested into a four-electrode system testing device, and then connecting the four-electrode system testing device with the electrochemical workstation and the two gear pumps. Pouring the prepared NaCl solution with the concentration of 0.1mol/L into a liquid storage tank, and placing the liquid storage tank into a constant temperature tank, wherein the set temperature is 20 ℃. Starting a gear pump, and adjusting the flow rate of the gear pump to enable the flow rate to be 1 cm/s. And after the flow and the potential difference are stable, obtaining an impedance spectrogram by an electrochemical impedance spectroscopy method of an electrochemical workstation. Then, the same measurement was carried out while changing the concentration of the electrolyte (NaCl) solution to 0.3mol/L and 0.5mol/L, respectively, and the effect of the concentration of the electrolyte (NaCl) solution on the contamination of the anion exchange membrane was examined. Blank experiments were performed under the same conditions.
The obtained impedance spectrum was fitted by the non-linear least squares method using the equivalent circuit model shown in fig. 4, and the obtained impedance spectrum was shown in fig. 7.
Specific example 3:
sodium Alginate (SA) is selected as a typical pollutant in membrane pollution research, and an AEM-TypeII-0.1 mol/L NaCl + 0.5% SA solution system is used. And putting the ion exchange membrane to be tested into a four-electrode system testing device, and then connecting the four-electrode system testing device with the electrochemical workstation and the two gear pumps. Pouring the prepared NaCl solution with the concentration of 0.1mol/L into a liquid storage tank, and placing the liquid storage tank into a constant temperature tank, wherein the set temperature is 20 ℃. Starting a gear pump, and adjusting the flow rate of the gear pump to enable the flow rate to be 1 cm/s. And after the flow and the potential difference are stable, obtaining an impedance spectrogram by an electrochemical impedance spectroscopy method of an electrochemical workstation. Then, the same measurement was carried out by replacing the contaminant SA with bovine serum albumin BSA, and the influence of different contaminants on the contamination of the anion exchange membrane was examined. Blank experiments were performed under the same conditions.
The obtained impedance spectrum was fitted by the non-linear least squares method using the equivalent circuit model shown in fig. 4, and the obtained impedance spectrum was shown in fig. 5. The contamination conditions in FIG. 5 were a flow rate of 2cm/s, a temperature of 20. + -. 2 ℃, a solution of 0.5mol/LNaCl + 0.5% SA, a contamination time of 57.4h, and data results of a non-linear least squares fit using the equivalent circuit in FIG. 4 using NOVA software from Vanton, Switzerland were: rm+s＝5.863Ω，Rs＝5.068Ω，Rm＝0.795Ω,Redl＝0.0095Ω,Rd＝0.061Ω,Rfouling＝0.0056Ω,Cedl＝9.7087F,Cfouling＝0.96334F,Cd＝80.715F。
The technical solution of the present invention is not limited to the above-mentioned specific embodiments, and includes any combination of the specific embodiments, and all similar structures and similar variations thereof adopted by the present invention should be included in the scope of the present invention.
Claims (10)
1. An electrochemical method for in-situ monitoring of the contamination of a membrane surface, comprising the steps of:
(1) preparing an electrolyte solution to be tested;
(2) connecting a test device: connecting a four-electrode testing device with an electrochemical workstation and a gear pump;
(3) operating the membrane to be tested: putting the membrane to be tested into a membrane clamping part in a four-electrode testing device, driving the electrolyte solution prepared in the step (1) into the four-electrode testing device, and starting a gear pump;
(4) measuring current or voltage signals using electrochemical impedance spectroscopy: applying a small-amplitude disturbance signal and sinusoidal alternating voltage or current to the monitoring device through the electrochemical workstation, collecting a response current or voltage signal by the electrochemical workstation, and reflecting the response current or voltage signal in Nova software carried by the electrochemical workstation to form an impedance spectrum EIS or an admittance spectrum;
(5) taking out the test film: stopping the operation of the four-electrode testing device, disconnecting the four-electrode testing device from the electrochemical workstation and the gear pump, and disassembling the four-electrode testing device;
(6) measurement of resistance value of blank solution: reassembling the four-electrode testing device and connecting the four-electrode testing device with an electrochemical workstation and a gear pump, wherein the resistance value of the solution is obtained by a blank experiment, and the measured total resistance minus the resistance value of the blank solution is the resistance of the film, the double electric layers, the diffusion boundary layer and the pollution layer;
(7) performing nonlinear least square fitting and analysis on the impedance spectrum or admittance spectrum obtained in the step (4) by using an equivalent circuit model to obtain electrochemical characteristic information of the test membrane,
is calculated by the formula
Where n is the number of data points selected for calculation, g'i，g″iRespectively the real part and the imaginary part of the admittance data;
(8) the electrochemical characteristic information of step (7) includes resistance values of the solution and the membrane, an electric double layer naturally formed by the test membrane in the solution, a diffusion boundary layer, a resistance of a contamination layer, and a resistance value of the electric double layer, the greater the resistance value of the contamination layer, the more easily the membrane is contaminated, and the greater the resistance value of the contamination layer, the more seriously the membrane is contaminated.
2. The electrochemical method for in situ monitoring of membrane surface contamination according to claim 1, wherein: the electrolyte solution in the step (1) is NaCl solution, the purity level of inorganic salt used for preparing the electrolyte solution is superior purity, the used water is deionized water, and the electrolyte solution is added with typical pollutants of bovine serum albumin or sodium alginate with different concentrations to simulate pollutants in natural water.
3. The electrochemical method for in situ monitoring of membrane surface contamination according to claim 1, wherein: the membrane to be tested in the step (3) is an ion exchange membrane, an ultrafiltration membrane, a nanofiltration membrane, a reverse osmosis membrane or a forward osmosis membrane, and pretreatment is carried out before testing: soaking in 0.5M NaCl solution for 24 hr, and replacing the solution for 4 times to remove residual chemical solvent in the membrane.
4. The electrochemical method for in situ monitoring of membrane surface contamination according to claim 1, wherein: the electrolyte solution in the step (3) is circulated.
5. The electrochemical method for in situ monitoring of membrane surface contamination according to claim 1, wherein: the environmental temperature of the electrolyte solution prepared in the step (3) is 10-40 ℃.
6. The electrochemical method for in situ monitoring of membrane surface contamination according to claim 1, wherein: the EIS testing frequency in the step (4) can be 1000000-0.01 Hz, wherein the testing frequency sections corresponding to different films are different, the amplitude of the alternating voltage is 0.01V, and 50 frequency points are taken in each test; the open circuit potential before the test was started was set to the initial potential of the device.
7. The electrochemical method for in situ monitoring of membrane surface contamination according to claim 1, wherein: the equivalent circuit model in the step (7) is formed by the sum R of the resistances of the solution and the filmm+sThe test membrane is formed by connecting four parts of circuit elements of an electric double layer, a diffusion boundary layer and a pollution layer which are naturally formed in a solution from left to right in series, wherein the membrane and the solution are formed by a resistor Rm+sThe electric double layer is represented by a resistor RedlAnd phase angle constant element QdIn parallel, the diffusion boundary layer is represented by a resistor RdAnd phase angle constant element QdParallel, the contamination layer is represented by a resistor RfoulingAnd phase angle constant element QfoulingParallel representation; the fitting results in the sum of the resistances R of the solution and the membranem+sResistance value R of electric double layeredlCapacitance value C of the electric double layeredlResistance value R of diffusion boundary layerdCapacitance value C of diffusion boundary layerdResistance value R of the contamination layerfoulingAnd the capacitance C of the contamination layerfoulingThe resistance Rs of the solution is determined by a blank test, the intrinsic resistance R of the pure filmmFrom the sum R of the resistances of the solution and the membranem+sMinus the resistance R of the solutionsResult in that R ism＝Rm+s-Rs. The total resistance R of the film is measuredtotal＝Rm+Redl+Rd+Rfouling。
8. A measuring device for in-situ monitoring of the contamination of a membrane surface according to claim 1, wherein: including the rotatory test cell that sets up of bilateral symmetry, press from both sides membrane part (3), four electrode system and outside electrochemistry workstation, gear pump, four electrode system includes working electrode (1), counter electrode (1) and two reference electrode (2), working electrode (1) and counter electrode (1) are the Ag AgCl electrode of disc respectively, two reference electrode (2) are the Ag AgCl electrode of placing in the lujin capillary.
9. The apparatus for in-situ monitoring the contamination of a membrane surface according to claim 8, wherein: the test tank is formed with four water passageways, four water passageways correspond inhalant canal (8,9) that set up and play water passageway (6,7) that upper portion set up for the test tank lower part corresponds, and the gear pump is squeezed into electrolyte solution from inhalant canal (8,9) on test tank both sides lower limit respectively, and electrolyte solution then flows from play water passageway (8,9) on test tank both sides upper limit respectively to guarantee that test membrane both sides environment is unanimous.
10. The apparatus for in-situ monitoring the contamination of a membrane surface according to claim 8, wherein: the diameter of the Ag/AgCl electrode is 10 mm; the effective membrane area of the membrane clamping part (3) is 3.14cm2。
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| CN113340945B (en) * | 2021-04-30 | 2023-07-18 | 武汉工程大学 | Electrochemical detection method for structure and performance of extraction membrane and pervaporation membrane |
| CN115184417A (en) * | 2022-06-23 | 2022-10-14 | 同济大学 | Thin film mass transfer performance evaluation instrument and method |
| CN117558379A (en) * | 2024-01-08 | 2024-02-13 | 武汉工程大学 | Method, device, system and electronic equipment for characterizing membrane pollution of forward osmosis membrane |
| CN117558379B (en) * | 2024-01-08 | 2024-03-26 | 武汉工程大学 | Method, device, system and electronic equipment for characterizing membrane pollution of forward osmosis membrane |
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