CN110082394A - In-situ monitoring amberplex surface electrochemistry Characterization method and monitoring device - Google Patents
In-situ monitoring amberplex surface electrochemistry Characterization method and monitoring device Download PDFInfo
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- CN110082394A CN110082394A CN201910336541.4A CN201910336541A CN110082394A CN 110082394 A CN110082394 A CN 110082394A CN 201910336541 A CN201910336541 A CN 201910336541A CN 110082394 A CN110082394 A CN 110082394A
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- amberplex
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- resistance
- situ monitoring
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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
Abstract
The present invention relates to a kind of in-situ monitoring amberplex surface electrochemistry Characterization method, which includes four electrode system test devices, electrochemical workstation, temperature controlled water bath slot and gear pump.Amberplex to be measured, which is put into four electrode system devices, makes film surface and electrolyte solution contacts constitute series circuit.Electrochemical workstation collects the current or voltage signal of response to the disturbing signal that monitoring device applies a small amplitude, is reflected in the included Nova software of electrochemical workstation and forms impedance spectrum or Admittance Spectroscopy.Then Non-linear least-square curve fitting, analysis are carried out to impedance spectrum or Admittance Spectroscopy using equivalent-circuit model, passes through the electrochemical parameter value that fitting obtains amberplex boundary layer each section after obtaining the Electrochemistry Information of the system.It the beneficial effects of the present invention are: accuracy is high, simple and practical, and is non-damage to the measurement of amberplex, it helps improve measuring accuracy and reduce error caused by film inhomogeneities.
Description
Technical field
The present invention relates to a kind of ion exchange membrane technology field, in particular to a kind of in-situ monitoring ion exchange film surface electricity
Chemical characteristic method and its monitoring device.
Background technique
Electrodialysis reversal is a kind of pollution-free, sustainable production capacity method, the freedom generated when can mix two kinds of solution
It can be converted to electric energy, and this system can be applied in the place of any two difference salinity solution mixing, for example, river enters
Haikou etc..The electricity production technique device is simple and cleanliness without any pollution, has a good application prospect, thus have received widespread attention and
Research.
Core component of the amberplex as electrodialysis reversal device, performance can directly affect the electricity production of device
Energy.However, the polluter in water body can be adhered to by electrostatic force and chemisorption ion exchange film surface and/
Or enter inside film, and form pollution layer in film surface.Phenomena such as power consumption caused by fouling membrane increases, and membrane lifetime shortens is
As the application of limitation electrodialysis reversal electricity production device and the main problem of economic feasibility.It can be along with film during fouling membrane
The variation of surface electrochemistry characteristic.
About amberplex electrochemical properties evaluation method there are many, such as: chronpotentiometry, linear scan
Voltammetry and electrochemical impedance spectroscopy etc..However, evaluating the electricity of amberplex currently without a reliable and comprehensive method
Chemical property.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of simple and reliable electrochemical properties evaluation methods and its prison
Survey device.
In order to solve the above-mentioned technical problem, the technical solution adopted by the present invention is that: a kind of in-situ monitoring amberplex table
Face electrochemical properties method, it is characterised in that the following steps are included:
(1) test electrolyte solution is prepared；
(2) amberplex to be measured is put into be measured in the folder membrane element in four electrode testing devices；
(3) four electrode testing devices are connect with electrochemical workstation and gear pump, starter receiver pump matches step (1)
The electrolyte solution set is driven into four electrode testing devices, operation a period of time, amberplex balanced condition is made to get off；
(4) electrochemical impedance spectroscopy is used, applies the disturbance of a small amplitude to monitoring device by electrochemical workstation
Signal and sinusoidal voltage or electric current, and the current or voltage signal responded is collected by electrochemical workstation, it is reflected in electrification
It learns in the included Nova software of work station, forms impedance spectrum EIS or Admittance Spectroscopy；
(5) operation for stopping four electrode testing devices, disconnects four electrode testing devices and electrochemical workstation and gear pump
Connection, disassembly four electrode testing devices take out amberplex；
(6) four electrode testing devices have been re-assemblied and have been connect with electrochemical workstation and gear pump, blank assay has been done, obtains
To the resistance value of blank solution；
(7) non-linear least square is carried out to impedance spectrum obtained in step (4) or Admittance Spectroscopy using equivalent-circuit model
Method fitting, analysis, obtain the electrochemical characteristic information of the amberplex.
Electrolyte solution described in step (1) is the inorganic salt solution of NaCl solution or various concentration different component, is matched
The inorganic salts purity grade that electrolyte solution processed uses is excellent pure grade, and the water distribution used is deionized water.
It to be impregnated in the electrolyte solution of test concentrations for 24 hours, during which more before amberplex to be measured test in step (2)
4 solution are changed, to remove remaining chemical solvent in membrane removal.
Electrolyte solution in step (3) is circular flow.
The environment temperature of electrolyte solution obtained is 10 DEG C~40 DEG C in step (3).
The test frequency of EIS is 1000~0.01Hz in step (4), and the amplitude of alternating voltage is 0.01V, and test takes every time
50 Frequency points；The open circuit potential tested before starting is set as the initial potential of device.
Step (7) described equivalent-circuit model is by the sum of the resistance of solution and film Rm+s, amberplex in the solution from
The electric double layer and diffusion boundary layer three parts circuit element so formed is successively connected in series from left to right, wherein film itself and solution
By a resistance Rm+sIt indicates, electric double layer is by a resistance RedlWith normal phase angle original part QdParallel connection indicates that diffusion boundary layer is by one
Resistance RdWith normal phase angle original part QdParallel connection indicates；Fitting result obtains the sum of the resistance of solution and film Rm+s, electric double layer resistance value
Redl, electric double layer capacitance Cedl, diffusion boundary layer resistance value RdAnd the capacitance C of diffusion boundary layerd, the resistance Rs of solution
It is measured by blank test, the resistance R of pure filmmBy the sum of the resistance of solution and film Rm+sSubtract the resistance R of solutionsIt obtains.
Test pond, folder membrane element, four electrode systems and external electrochemical workstation, tooth including bilateral symmetry rotary setting
Wheel pump, four electrode system include working electrode, to electrode and two reference electrodes, the working electrode and to electrode point
Not Wei disc Ag/AgCl electrode, described two reference electrodes are located in the Ag/AgCl electrode in Luggin capillary.
The test pond is formed there are four aquaporin, and gear pump is by the electrolyte solution water following from test pond two sides respectively
Channel is squeezed into, and then electrolyte solution is flowed out from the aquaporin of test pond two sides top respectively, to guarantee ion exchange to be measured
Film film two sides environment is consistent.
The Ag/AgCl electrode diameter is 10mm；Effective membrane area of the folder membrane element is 3.14cm2。
The beneficial effects of the present invention are: the method and device energy provided by the invention for obtaining amberplex electrochemical properties
The electrical properties of amberplex and its boundary layer are determined by EIS method.Resistance value and capacitance in equivalent circuit can
To reflect the structure of ion exchange film system, therefore, impedance modal data energy quantitative analysis out-of-bounds are fitted using equivalent circuit
The electric conductivity value and capacitance of surface layer, while the thickness of diffusion boundary layer can also be calculated by its capacitance and resistance value.This
The device of invention is accurate, reliable and easy to operate, suitable for a variety of electrolyte solution intermediate ion exchange membrane electrochemical properties
Measurement.
Detailed description of the invention
Fig. 1 is the experimental provision schematic diagram of the electrochemical method of in-situ monitoring ion exchange membrane surface electrochemistry characteristic；
Fig. 2 is the general structure schematic diagram of four electrode system test devices；
Fig. 3 is the folder membrane element structural schematic diagram of four electrode system test devices；
Fig. 4 carries out the equivalent-circuit model of Non-linear least-square curve fitting to impedance spectrum；
The impedance spectra and matched curve that Fig. 5 flow velocity influences amberplex electrochemical properties；
Fig. 6 flow velocity schemes the rule that amberplex electrochemical properties influence；
The impedance spectra that Fig. 7 temperature influences amberplex electrochemical properties；
Fig. 8 temperature schemes the rule that amberplex electrochemical properties influence.
In figure:
1, working electrode 2, reference electrode 3, folder membrane element
4, electrochemical workstation 5, computer 6, working electrode
7, to electrode 8, reference electrode 9, reference electrode
10, membrane element 11, left side intake tunnel 12, left side exhalant canal are pressed from both sides
13, right side intake tunnel 14, right side exhalant canal；
Specific embodiment
Invention is further described in detail with reference to the accompanying drawings and detailed description:
As shown in Figure 1, a kind of electrochemical method of in-situ monitoring ion exchange membrane surface electrochemistry characteristic, including it is as follows
Step:
(1) test electrolyte solution is prepared；
(2) amberplex to be measured is put into the folder membrane element in four electrode testing devices, assembles the survey of four electrodes
Trial assembly is set；
(3) four electrode testing devices are connect with electrochemical workstation and gear pump, starter receiver pump matches step (1)
The electrolyte solution set is driven into four electrode testing devices, operation a period of time, amberplex balanced condition is made to get off；
(4) electrochemical impedance spectroscopy is used, applies the disturbance of a small amplitude to monitoring device by electrochemical workstation
Signal, that is, sinusoidal voltage or electric current, and the current or voltage signal responded is collected by electrochemical workstation, it is reflected in electrification
It learns in the included Nova software of work station, forms impedance spectrum or Admittance Spectroscopy；
(5) operation for stopping four electrode testing devices, disconnects four electrode testing devices and electrochemical workstation and gear pump
Connection, disassembly four electrode testing devices take out amberplex；
(6) four electrode testing devices have been re-assemblied and have been connect with electrochemical workstation and gear pump, blank assay is done, it is empty
The purpose of white experiment is to obtain the resistance value of blank solution；
(7) analytic function of the Nova software carried using electrochemical workstation to impedance spectrum obtained in step (4) or
Admittance Spectroscopy is handled, and building equivalent-circuit model carries out Non-linear least-square curve fitting, analysis automatically, obtains ion friendship
Change the Electrochemistry Information of film.
The measuring device for implementing the acquisition amberplex electrochemical properties of the above method is as shown in Figure 2 and Figure 3, the device
Containing working electrode, to electrode, reference electrode and folder membrane element.After pretreated amberplex is put into folder membrane element,
It is screwed.All components are connected with long screw again and are fixed.The electrolyte solution of test is placed in constant temperature water bath, is led to
Cross rubber conduit to be connected two gear pump inlets, then squeeze into 11,13 water inlets of test device, after from test device
12,14 water outlets return in rear constant temperature water bath, circulate.Blank assay is in four electrode testing devices without film, remaining step
It is identical.
Specific embodiment 1:
Use mono- NaCl solution system of AEM-TypeI.Amberplex to be measured is put into four electrode system test devices,
Then four electrode system test devices and electrochemical workstation and two gear pumps are connected.It is by the concentration of preparation
The NaCl solution of 0.1mol/L pours into reservoir, and reservoir is placed in thermostat, and set temperature is 25 DEG C.Starter receiver pump,
Gear flow rate pump is adjusted, flow velocity 1cm/s is made.After flow and potential difference are stablized, by the electrochemical impedance of electrochemical workstation
Spectrometry obtains impedance spectra.Then change the flow velocity of gear pump equally to be measured respectively for 2,3,4cm/s.Under the same conditions
Do blank assay.
Non-linear least-square curve fitting is carried out to obtained impedance spectra with equivalent-circuit model shown in Fig. 4,
Obtained impedance spectra and matched curve are as shown in Figure 5.Institute's measured ion exchange membrane can be obtained by fitting result
Film resistance value itself, electric double layer resistance capacitance value and diffusion boundary layer resistance capacitance value.Flow velocity is to amberplex electrochemical properties
Influence see Fig. 6.
Specific embodiment 2:
Use mono- NaCl solution system of CEM-TypeII.Amberplex to be measured is put into four electrode system test devices
In, then four electrode system test devices and electrochemical workstation and two gear pumps are connected.It is by the concentration of preparation
The NaCl solution of 0.5mol/L pours into reservoir, and reservoir is placed in thermostat, and set temperature is 10 DEG C.Starter receiver pump,
Gear flow rate pump is adjusted, flow velocity 1cm/s is made.After flow and potential difference are stablized, by the electrochemical impedance of electrochemical workstation
Spectrometry obtains impedance spectra.Then change thermostat equally to be measured respectively for 20,30,40 DEG C.Sky is done under the same conditions
White experiment.
Non-linear least-square curve fitting is carried out to obtained impedance spectra with equivalent-circuit model shown in Fig. 4,
Obtained impedance spectra is as shown in Figure 7.By fitting result can be obtained institute's measured ion exchange membrane film resistance value itself,
Electric double layer resistance capacitance value and diffusion boundary layer resistance capacitance value.Fig. 8 is shown in influence of the temperature to amberplex electrochemical properties.
Technical solution of the present invention is not limited to specific embodiment enumerated above, further includes between each specific embodiment
Any combination, it is all using similar structure and its similar variation of the invention, protection scope of the present invention should all be included in.
Claims (10)
1. a kind of in-situ monitoring amberplex surface electrochemistry Characterization method, it is characterised in that the following steps are included:
(1) test electrolyte solution is prepared；
(2) amberplex to be measured is put into be measured in the folder membrane element in four electrode testing devices；
(3) four electrode testing devices are connect with electrochemical workstation and gear pump, starter receiver pump, by step (1) configuration
Electrolyte solution is driven into four electrode testing devices, operation a period of time, amberplex balanced condition is made to get off；
(4) electrochemical impedance spectroscopy is used, applies the disturbing signal of a small amplitude to monitoring device by electrochemical workstation
And sinusoidal voltage or electric current, and the current or voltage signal of response is collected by electrochemical workstation, it is reflected in electrochemistry work
Make to form impedance spectrum EIS or Admittance Spectroscopy in the included Nova software in station；
(5) operation for stopping four electrode testing devices, disconnects the company of four electrode testing devices and electrochemical workstation and gear pump
It connects, four electrode testing devices of disassembly take out amberplex；
(6) four electrode testing devices have been re-assemblied and have been connect with electrochemical workstation and gear pump, blank assay has been done, obtains sky
The resistance value of white solution；
(7) nonlinear least square method is carried out to impedance spectrum obtained in step (4) or Admittance Spectroscopy using equivalent-circuit model to intend
Splitting or integrating analysis, obtains the electrochemical characteristic information of the amberplex.
2. in-situ monitoring amberplex surface electrochemistry Characterization method according to claim 1, it is characterised in that: step
(1) electrolyte solution described in is the inorganic salt solution of NaCl solution or various concentration different component, prepares electrolyte solution
The inorganic salts purity grade used is excellent pure grade, and the water distribution used is deionized water.
3. in-situ monitoring amberplex surface electrochemistry Characterization method according to claim 1, it is characterised in that: step
(2) it to be impregnated in the electrolyte solution of test concentrations for 24 hours before amberplex to be measured test in, during which replace 4 solution, with
Remove remaining chemical solvent in membrane removal.
4. in-situ monitoring amberplex surface electrochemistry Characterization method according to claim 1, it is characterised in that: step
(3) electrolyte solution in is circular flow.
5. in-situ monitoring amberplex surface electrochemistry Characterization method according to claim 1, it is characterised in that: step
(3) environment temperature of electrolyte solution obtained is 10 DEG C~40 DEG C in.
6. in-situ monitoring amberplex surface electrochemistry Characterization method according to claim 1, it is characterised in that: step
(4) test frequency of EIS is 1000~0.01Hz in, and the amplitude of alternating voltage is 0.01V, and test takes 50 Frequency points every time；
The open circuit potential tested before starting is set as the initial potential of device.
7. in-situ monitoring amberplex surface electrochemistry Characterization method according to claim 1, it is characterised in that: step
(7) equivalent-circuit model is by the sum of the resistance of solution and film Rm+s, amberplex self-assembling formation in the solution double electricity
Layer and diffusion boundary layer three parts circuit element are successively connected in series from left to right, and wherein film itself and solution are by a resistance
Rm+sIt indicates, electric double layer is by a resistance RedlWith normal phase angle original part QdParallel connection indicates that diffusion boundary layer is by a resistance RdWith normal phase
Angle original part QdParallel connection indicates；Fitting result obtains the sum of the resistance of solution and film Rm+s, electric double layer resistance value Redl, electric double layer
Capacitance Cedl, diffusion boundary layer resistance value RdAnd the capacitance C of diffusion boundary layerd, the resistance Rs of solution surveys by blank test
Out, the resistance R of pure filmmBy the sum of the resistance of solution and film Rm+sSubtract the resistance R of solutionsIt obtains.
8. a kind of measuring device of in-situ monitoring amberplex surface electrochemistry Characterization method according to claim 1,
It is characterized in that: test pond, folder membrane element (3), four electrode systems and external electrochemical operation including bilateral symmetry rotary setting
It stands, gear pump, four electrode system includes working electrode, to electrode (1) and two reference electrodes (2), the working electrode
With the Ag/AgCl electrode for electrode being respectively disc, described two reference electrodes are located in the Ag/ in Luggin capillary
AgCl electrode.
9. the measuring device of in-situ monitoring amberplex surface electrochemistry characteristic according to claim 8, it is characterised in that:
The test pond is formed there are four aquaporin, and gear pump by electrolyte solution, beat respectively by the aquaporin following from test pond two sides
Enter, then electrolyte solution is flowed out from the aquaporin of test pond two sides top respectively, to guarantee ion exchange membrane two to be measured
Side ring border is consistent.
10. the measuring device of in-situ monitoring amberplex surface electrochemistry characteristic, feature exist according to claim 8
In: the Ag/AgCl electrode diameter is 10mm；Effective membrane area of folder membrane element (3) is 3.14cm2。
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| CN110687173A (en) * | 2019-10-22 | 2020-01-14 | 天津城建大学 | Electrochemical method for in-situ monitoring of membrane surface pollution condition and monitoring device |
| CN111141953A (en) * | 2019-12-17 | 2020-05-12 | 武汉工程大学 | Alternating current impedance testing device and method for insulating hollow fiber membrane |
| CN111398683A (en) * | 2020-03-24 | 2020-07-10 | 苏州宇量电池有限公司 | Solid electrolyte ionic conductivity test fixture and test method |
| CN114965652A (en) * | 2022-04-27 | 2022-08-30 | 同济大学 | Device and method for measuring ion transmembrane potential barrier |
| CN115184417A (en) * | 2022-06-23 | 2022-10-14 | 同济大学 | Thin film mass transfer performance evaluation instrument and method |
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| CN115184417A (en) * | 2022-06-23 | 2022-10-14 | 同济大学 | Thin film mass transfer performance evaluation instrument and method |
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Application publication date: 20190802 |