CN114354708B - Regeneration electrode and preparation method thereof - Google Patents
Regeneration electrode and preparation method thereof Download PDFInfo
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- CN114354708B CN114354708B CN202111562089.7A CN202111562089A CN114354708B CN 114354708 B CN114354708 B CN 114354708B CN 202111562089 A CN202111562089 A CN 202111562089A CN 114354708 B CN114354708 B CN 114354708B
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
Abstract
The invention belongs to the technical field of biosensors, and particularly discloses a regeneration electrode and a preparation method thereof. The preparation method of the regenerated electrode comprises the following steps: cleaning the working electrode of the failure sensor by using a cleaning agent to obtain an electrode 1; the cleaning agent contains inorganic alkali and alcohol; the failure sensor comprises a working electrode, wherein the working electrode is covered with a mixture of a binder and at least one of chitosan, carbon nanotubes, carbon aerogel and Prussian blue; and sequentially carrying out cyclic voltammetry scanning on the electrode 1 in KCl/PBS buffer solution and inorganic alkali solution to obtain a regenerated electrode. The method can effectively remove materials such as Nafion film, chitosan, carbon nano tube, carbon aerogel, prussian blue and the like attached to the failure sensor, does not need to use dangerous reagents with strong corrosivity such as hydrochloric acid, sulfuric acid and the like, can recycle the electrode, and is used for preparing the sensor again.
Description
Technical Field
The invention relates to the technical field of biosensors, in particular to a regeneration electrode and a preparation method thereof.
Background
The wearable flexible glucose sensor can realize noninvasive detection of blood glucose, so that a blood glucose detector is free from the pain of needle insertion. Gold has the advantages of strong stability, high conductivity, good biocompatibility and the like, and can be combined with polyethylene terephthalate PET and silver/silver chloride to prepare a flexible gold three-electrode which takes a gold electrode as a working electrode and a reference electrode and silver/silver chloride as a reference electrode. Further, prussian blue, chitosan, glucose oxidase, carbon nanotubes, carbon aerogel and other materials are used for modifying the flexible gold three-electrode, so that the flexible gold three-electrode glucose sensor for noninvasive detection of blood sugar can be obtained. For example, the related art discloses a preparation method and application of a PET substrate film gold electrode glucose sensor, wherein a PET substrate film gold electrode is obtained by using electroless gold plating, silver paste is coated on a reference electrode, prussian blue is deposited on a working electrode, glucose oxidase/chitosan/carbon nanotube solution is dripped for modification, and perfluorinated sulfonic polymer Nafion solution is dripped for encapsulation, so that the flexible glucose sensor is obtained.
After the flexible gold three-electrode glucose sensor is prepared, the sensor cannot be used continuously due to pollution of a detection sample, inactivation of glucose oxidase and the like, and is disabled. The preparation cost of the flexible gold three electrode is higher, and the undamaged flexible gold three electrode can be used for preparing the flexible gold three electrode glucose sensor again after being treated, so that the flexible gold three electrode has higher recycling treatment and recycling value.
The treatment and recycling of the flexible gold three electrode need to solve the following problems: 1. the surface layer of the flexible gold three-electrode glucose sensor is generally embedded and encapsulated by Nafion solution, and the Nafion embedded film on the surface of the electrode needs to be removed first. However, no related art has disclosed how to remove the Nafion embedded membrane. 2. The materials such as chitosan, carbon nano tube, carbon aerogel and Prussian blue have strong adhesion, and the materials need to be removed cleanly without damaging the gold electrode, and the current method inevitably damages the gold electrode when removing the materials such as chitosan, carbon nano tube, carbon aerogel and Prussian blue. 3. The use of ultrasonic cleaning results in silver/silver chloride shedding as a reference electrode. 4. Cleaning the electrodes with hydrochloric acid, sulfuric acid, or the like easily causes corrosion of the electrodes, and polarization phenomenon easily occurs when using cyclic voltammetry. The strong hydrochloric acid and sulfuric acid solutions have certain operational safety risks in the process of using and preparing the reagents.
Disclosure of Invention
The present invention aims to solve at least one of the technical problems existing in the prior art. Therefore, a first object of the present invention is to provide a method for preparing a regenerated electrode, which can effectively remove materials such as Nafion membrane, chitosan, carbon nanotube, carbon aerogel, prussian blue attached to a dead sensor such as a flexible gold three-electrode glucose sensor, and can reuse the electrode for preparing the sensor without using highly corrosive hazardous reagents such as hydrochloric acid and sulfuric acid.
A second object of the present invention is to provide a regeneration electrode.
Specifically, the invention relates to the following technical scheme:
a method for preparing a regenerated electrode, comprising the steps of:
cleaning the working electrode of the failure sensor by using a cleaning agent to obtain an electrode 1; the cleaning agent contains inorganic alkali and alcohol; the failure sensor comprises a working electrode, wherein the working electrode is covered with a mixture of a binder and at least one of chitosan, carbon nanotubes, carbon aerogel and Prussian blue;
and sequentially carrying out cyclic voltammetry scanning on the electrode 1 in KCl/PBS buffer solution and inorganic alkali solution to obtain a regenerated electrode.
In the preparation method, a working electrode of the failure sensor is cleaned by adopting a cleaning agent composed of inorganic alkali and alcohol, wherein the alcohol can dissolve an adhesive for fixing modified materials such as chitosan, carbon nano tubes, carbon aerogel, prussian blue and the like on the working electrode, so that the adhesive is removed.
The chitosan in the sensor is generally dissolved in an acidic solution such as acetic acid, and then uniformly mixed and dispersed with carbon nanotubes, carbon aerogel and the like, and then glucose oxidase and the like are adsorbed for preparing the corresponding sensor. The chitosan has viscosity and can be adhered to the surface of the electrode material after air drying. Namely, chitosan, carbon nanotubes and carbon aerogel in the failure sensor show certain acidity. After inorganic alkali is added into the cleaning agent, the inside of chitosan and the connection with carbon nano tubes, carbon aerogel and other materials can be destroyed by acid-base neutralization, so that the chitosan is dispersed and further removed from the working electrode.
Prussian blue, i.e., ferric ferrocyanide, is a substance that can be synthesized by coordination of potassium ferrocyanide and ferric chloride in a slightly acidic environment. In the sensor preparation process, prussian blue can be adhered to the surface of the electrode through dyeing and electrochemical deposition. Ethanol has poor dissolution effect on Prussian blue, but the structure of Prussian blue can be destroyed by adding inorganic alkali and neutralizing by acid and alkali, ferric hydroxide and ferricyanide are formed, and the Prussian blue has good dissolution and cleaning effects.
Therefore, the working electrode of the failure sensor is cleaned by adopting a cleaning agent consisting of inorganic alkali and alcohol, and materials such as a binder, chitosan, carbon nano tube, carbon aerogel, prussian blue and the like adhered on the working electrode can be well dissolved and shed.
Meanwhile, by performing cyclic voltammetry scanning in KCl/PBS buffer solution and inorganic alkali solution, sediment and oxide on the working electrode can be removed, and polarization phenomenon of the working electrode can be improved.
In some embodiments of the invention, the cleaning agent comprises 1-4 parts by volume of an inorganic alkaline solution and 1-2 parts by volume of alcohol; preferably, the cleaning agent comprises 1-4 parts of inorganic alkali solution and 1 part of alcohol by volume; more preferably, the cleaning agent comprises 1 to 2 parts by volume of an inorganic alkali solution and 1 part by volume of alcohol.
In some embodiments of the invention, the inorganic alkaline solution in the cleaning agent is an aqueous solution of an inorganic base at a concentration of 1 to 3mol/L, preferably 1.5 to 2.5mol/L. After the inorganic alkali solution with the concentration is mixed with alcohol in proportion, the pH value of the cleaning agent can reach 10 or above.
In some embodiments of the invention, the inorganic base in the cleaning agent comprises at least one of sodium hydroxide, potassium hydroxide, magnesium hydroxide, sodium carbonate, potassium carbonate. In order to avoid bringing unnecessary ions, the inorganic base in the cleaning agent is preferably sodium hydroxide.
In some embodiments of the invention, the alcohol in the cleaning agent comprises at least one of ethanol, methanol, isopropanol. Ethanol is preferred because it is less expensive, has high volatility, is less likely to remain, and has low toxicity and irritation than other alcohols such as isopropanol and methanol.
In some embodiments of the invention, the step of cleaning the working electrode of the failed sensor with a cleaning agent is specifically to apply the cleaning agent to the working electrode of the failed sensor and agitate the mixture overlying the working electrode. The agitation may be performed by using a purge rod. The cleaning agent is combined with mechanical stirring, so that the binding agent, chitosan, carbon nano tube, carbon aerogel, prussian blue and other modified materials adhered on the working electrode can be well dissolved and fall off.
In some embodiments of the invention, the step of cleaning the working electrode of the failed sensor with a cleaning agent is followed by a step of washing with water and drying. The cleaning agent is removed from the surface of the working electrode by washing with water and drying, and the influence on the subsequent cyclic voltammetry scanning step is avoided.
In some embodiments of the invention, the binder comprises a perfluorosulfonic acid-based polymer Nafion membrane. The perfluorinated sulfonic acid polymer is dissolved by volatile alcohols such as isopropanol, ethanol and the like to prepare Nafion solution, and after air drying, a polymer film (Nafion film) with selective permeability can be formed, and the electrode modification material can be encapsulated and embedded and adhered to the surface of an electrode. Ethanol is added into the cleaning agent to dissolve the polymer film formed by the Nafion solution.
In some embodiments of the invention, the working electrode is a gold electrode.
In some embodiments of the invention, the cyclic voltammetry scan is performed in KCl/PBS buffer at a voltage ranging from 300mV to 650mV; preferably, the sweep rate is from 100 to 200mV/s, preferably about 150mV/s; preferably, the number of scanning turns is 3-9. Deposit and oxide on the working electrode can be removed by cyclic voltammetry scanning in KCl/PBS buffer.
In some embodiments of the invention, the KCl/PBS buffer has a concentration of KCl of 0.05 to 0.2mol/L, preferably 0.1 to 0.15mol/L. The KCl concentration has an influence on the current of the electrode, and when the KCl concentration is too high for cyclic voltammetry scanning, the generated current is too high, so that the electrode can be burnt out; too low a current is insufficient and good effects of removing adherents and activating electrodes cannot be achieved.
In some embodiments of the invention, the cyclic voltammetry scan is performed in a KCl/PBS buffer, which is applied to the working electrode, followed by cyclic voltammetry scan.
In some embodiments of the invention, the voltage range of the cyclic voltammetry sweep in the inorganic alkaline solution is from-250 mV to 300mV; preferably, the sweep rate is from 30 to 80mV/s, preferably about 50mV/s; preferably, the number of scanning turns is 1-3. By performing the second cyclic voltammetry scan in an inorganic alkaline solution, deposits and oxides on the working electrode can be further removed, improving the polarization phenomenon of the working electrode.
In some embodiments of the invention, the inorganic base solution used for cyclic voltammetry scanning is an aqueous solution of an inorganic base at a concentration of 0.05 to 1mol/L, preferably 0.1 to 0.5mol/L. The inorganic base used for cyclic voltammetry scanning may include at least one of sodium hydroxide, potassium hydroxide, magnesium hydroxide, sodium carbonate, potassium carbonate, sodium bicarbonate, and potassium bicarbonate, and may be the same as or different from the inorganic base in the cleaning agent. Preferably, the inorganic base used for cyclic voltammetry scanning is sodium hydroxide. Preferably, the inorganic base used for cyclic voltammetry scanning is the same as the inorganic base in the cleaning agent.
In some embodiments of the invention, the specific step of performing the cyclic voltammetry scan in an inorganic base solution is to apply the inorganic base solution to the working electrode and then perform the cyclic voltammetry scan.
In some embodiments of the invention, the step of performing the cyclic voltammetry scan in PBS buffer is further included after performing the cyclic voltammetry scan in an inorganic base solution. By cyclic voltammetry scanning in PBS buffer, a stable repeated scan curve can be obtained, and the stability of the regenerated electrode can be checked.
In some embodiments of the invention, the voltage range of the cyclic voltammetry scan in PBS buffer is-250 mV to 300mV; preferably, the sweep rate is from 30 to 80mV/s, preferably about 50mV/s; preferably, the number of turns of the scan can be determined as needed until a stable and repeated scan curve is obtained. As an example, the number of scanning turns may be 3 to 6 turns.
In some embodiments of the invention, the PBS buffer used for cyclic voltammetry scanning has a pH of 6 to 8, preferably 7 to 7.5, more preferably 7 to 7.2.
In some embodiments of the invention, the specific step of performing the cyclic voltammetry scan in a PBS buffer is to apply the PBS buffer to the working electrode, followed by the cyclic voltammetry scan.
The failure sensor further comprises a counter electrode and a reference electrodeWhen the counter electrode, the reference electrode and the working electrode form a three-electrode, and when cleaning is performed by adopting a cleaning agent and cyclic voltammetry scanning is performed in KCl/PBS buffer solution, inorganic alkali solution and PBS buffer solution, the adding amount of the cleaning agent, KCl/PBS buffer solution, inorganic alkali solution and PBS buffer solution can generally cover the three-electrode area. As an example, the detergent, the KCl/PBS buffer for cyclic voltammetry scanning, an inorganic base solution or PBS buffer is added in an amount to the working electrode area ratio of not less than 7. Mu.L/mm 2 Preferably 7 to 15. Mu.L/mm 2 More preferably 7.5 to 10. Mu.L/mm 2 . For example, 30 to 40. Mu.L of a cleaning agent, KCl/PBS buffer, inorganic alkaline solution or PBS buffer may be added to a circular working electrode having a diameter of 4 mm.
After cyclic voltammetry scanning in PBS buffer solution, the regenerated electrode is washed with water and dried, and the regenerated electrode can be used for manufacturing various sensors or other electronic elements again.
A regenerated electrode is prepared by the preparation method.
Compared with the prior art, the invention has the following beneficial effects:
the invention uses alcohol and inorganic alkali to prepare the cleaning agent, the cleaning agent is simple to prepare, the cost is low, the dosage is small, the cleaning agent has good dissolving and removing effects on materials such as nafion membrane, chitosan, carbon nano tube, carbon aerogel, prussian blue and the like attached to a failure sensor, and the cleaning agent does not need to use dangerous reagents with strong corrosivity such as hydrochloric acid, sulfuric acid and the like.
And the KCl/PBS buffer solution is adopted for cyclic voltammetry scanning, so that sediment and oxide on the gold electrode are removed, and the operation is simple, safe and efficient.
And (3) adopting inorganic alkali solution to carry out cyclic voltammetry scanning, further removing residual sediment and oxide on the gold electrode, and obviously improving the polarization phenomenon of the electrode.
The method provided by the invention is used for processing the failure sensor, and the obtained regenerated anode has very good electrical stability and can be applied to manufacturing various sensors or other electronic components.
Drawings
FIG. 1 is a photograph of a real object of the dead gold three-electrode glucose sensor of example 1 during cleaning;
FIG. 2 is a cyclic voltammetry scan (CV) curve of the spent gold three-electrode glucose sensor of example 1 and comparative example 1 after regeneration treatment;
FIG. 3 is a photograph of a real object during the cleaning process of the dead gold three-electrode glucose sensor of example 2 and comparative example 2;
fig. 4 is a flexible gold three electrode cleaner formulated in different proportions for example 2 and comparative example 2.
Detailed Description
The technical scheme of the invention is further described below with reference to specific examples. The starting materials used in the examples below, unless otherwise specified, are all commercially available from conventional sources; the processes used, unless otherwise specified, are all conventional in the art.
Example 1
In the following, a flexible gold three-electrode glucose sensor having a working electrode diameter of 4mm and an overall width of 10mm is exemplified, and as shown in fig. 1A1, the flexible gold three-electrode glucose sensor includes a flexible PET substrate on which gold three electrodes including a gold electrode as a working electrode (circular area in fig. 1) and a counter electrode and silver/silver chloride as a reference electrode are plated, wherein the working electrode is covered with a mixture of chitosan, carbon nanotubes, carbon aerogel, prussian blue and Nafion.
The regeneration treatment method of the invalid flexible gold three-electrode glucose sensor comprises the following steps:
(1) Preparing 2mol/L sodium hydroxide solution, and then mixing 1 part of the 2mol/L sodium hydroxide solution and 1 part of absolute ethyl alcohol to prepare the flexible gold three-electrode cleaner. A40. Mu.L flexible gold three-electrode cleaner was dropped on the gold three-electrode, stirred with a plastic rod having a diameter of 1mm, and Nafion film for encapsulating the electrode was dissolved and removed, and materials such as chitosan, carbon nanotube, carbon aerogel, prussian blue, etc., adhered to the surface of the working electrode were adhered, as shown in FIG. 1A 2. Then, the gold three electrode is rinsed by ultrapure water, and is dried by cold air, so that the cleaned three electrode is obtained, as shown in fig. 1A 3.
(2) mu.L of 0.1M KCl/PBS buffer was added dropwise to the gold triad electrode, and cyclic voltammetry was performed at a rate of 150mV/s for 6 cycles at 300mV to 650mV to remove deposits and oxides on the gold triad electrode.
(3) 40 mu L of 0.5mol/L sodium hydroxide solution is dripped on the gold three electrode, cyclic voltammetry scanning is carried out for 1 circle at the speed of 50mV/s from minus 250mV to 300mV, residual sediment and oxide on the gold three electrode are further removed, and the polarization phenomenon of the electrode is improved.
(4) mu.L of PBS buffer at pH 7.2 was added dropwise to the gold triplex electrode, and cyclic voltammetry was run at a rate of 50mV/s for 3 cycles at-250 mV to 300mV to give a stable repeated CV curve, as shown in FIG. 2.
(5) And (3) flushing the gold three electrodes by using ultrapure water, and drying by cold air.
Example 2
In this embodiment, the dead flexible gold three-electrode glucose sensor is subjected to regeneration treatment, wherein the structure of the dead flexible gold three-electrode glucose sensor is the same as that of embodiment 1, the physical photo is shown in fig. 3A1, and the regeneration treatment method comprises the following steps:
(1) 2mol/L sodium hydroxide solution is prepared, and then 2 parts of the 2mol/L sodium hydroxide solution and 1 part of absolute ethyl alcohol are mixed to prepare the clear and transparent flexible gold three-electrode cleaner, as shown in figure 4A. 30 mu L of the flexible gold three-electrode cleaner was dropped on the gold three-electrode, stirred with a plastic rod with a diameter of 1mm, and Nafion film for encapsulating the electrode was dissolved and removed, and materials such as chitosan, carbon nanotube, carbon aerogel, prussian blue and the like adhered to the surface of the working electrode were adhered, as shown in FIG. 3A 2. Then, the gold three electrode is rinsed by ultrapure water, and is dried by cold air, so that the cleaned gold three electrode is obtained, as shown in fig. 3A 3.
(2) mu.L of 0.1M KCl/PBS buffer was added dropwise to the gold triad electrode, and cyclic voltammetry was run at a rate of 150mV/s for 3 cycles at 300mV to 650mV to remove deposits and oxides on the gold triad electrode.
(3) 30 mu L of 0.1mol/L sodium hydroxide is dripped on the gold three electrode, cyclic voltammetry scanning is carried out for 2 circles at the speed of 50mV/s from minus 250mV to 300mV, residual sediment and oxide on the gold three electrode are further removed, and the polarization phenomenon of the electrode is improved.
(4) mu.L of PBS buffer at pH 7.2 was added dropwise to the gold triplex electrode, and cyclic voltammetry was run at a rate of 50mV/s for 3 cycles at-250 mV to 300mV to give a stable repeated CV curve similar to that of example 1.
(5) And (5) flushing the gold electrode by using ultrapure water, and drying by cold air.
Comparative example 1
The difference between this comparative example and example 1 is that: no cyclic voltammetry scans were performed in 0.5mol/L sodium hydroxide solution. The method specifically comprises the following steps:
(1) Preparing 2mol/L sodium hydroxide solution, and then mixing 1 part of the 2mol/L sodium hydroxide solution and 1 part of absolute ethyl alcohol to prepare the flexible gold three-electrode cleaner. And (3) dripping 40 mu L of the flexible gold three-electrode cleaner onto the gold three-electrode, stirring with a plastic rod with the diameter of 1mm, dissolving and removing Nafion films for packaging the electrodes, and adhering chitosan, carbon nano tubes, carbon aerogel, prussian blue and other materials on the surfaces of the gold electrodes. And then the gold three electrode is washed by ultrapure water, and is dried by cold air, so that the cleaned gold three electrode is obtained.
(2) mu.L of 0.1M KCl/PBS buffer was added dropwise to the electrode, and cyclic voltammetry was performed at a rate of 150mV/s for 6 cycles at 300mV to 650mV to remove the deposit and oxide on the gold electrode.
(3) mu.L of PBS buffer at pH 7.2 was added dropwise to the gold triplex electrode, and cyclic voltammetry was run at a rate of 50mV/s for 3 cycles at-250 mV to 300mV, and the CV curve obtained was shown in FIG. 2. As can be seen from comparison with the CV curve of example 1, the electrode polarization could not be improved by omitting the cyclic voltammetry scanning step in 0.5mol/L sodium hydroxide solution, and stable and repeated CV curve could not be obtained.
Comparative example 2
This comparative example was performed on a dead flexible gold three-electrode glucose sensor having the same structure as that of example 2, and a physical photograph as shown in fig. 3B1, and the regeneration processing method was different from that of example 2 in that: the composition of the flexible gold three-electrode cleaner is changed into: 1 part of 2mol/L sodium hydroxide solution and 9 parts of absolute ethyl alcohol.
The method comprises the following specific steps:
2mol/L sodium hydroxide solution is prepared, and then 1 part of 2mol/L sodium hydroxide solution and 9 parts of absolute ethyl alcohol are mixed to obtain the flexible gold three-electrode cleaner, and the flexible gold three-electrode cleaner has obvious turbidity, as shown in fig. 4B. A30 mu L flexible gold three-electrode cleaner is dripped on the gold three-electrode, a plastic rod with the diameter of 1mm is used for stirring, and an electrode physical diagram after stirring is shown in a figure 3B2, so that materials such as Nafion films for packaging the electrodes, chitosan, carbon nano tubes, carbon aerogel, prussian blue and the like adhered to the surface of the working electrode cannot be dissolved and removed. Then the gold three electrode is rinsed with ultrapure water and dried by cold air, as shown in fig. 3B 3.
Fig. 4B, fig. 3B2 and fig. 3B3 reflect that when the formulation ratio of the flexible gold three-electrode cleaner is incorrect, not only the solution is turbid, but also the cleaning effect on the invalid gold three-electrode is poor, and materials such as Nafion film of the encapsulated electrode, chitosan adhered to the surface of the working electrode, carbon nano tube, carbon aerogel, prussian blue and the like cannot be effectively dissolved and removed.
The sensor (FIG. 3C 1) cleaned with a flexible gold three-electrode cleaner prepared from 1 part of 2mol/L sodium hydroxide solution and 9 parts of absolute ethyl alcohol was cleaned again as in example 2, with the following steps:
2 parts of 2mol/L sodium hydroxide solution and 1 part of absolute ethyl alcohol are mixed to prepare the clear and transparent flexible gold three-electrode cleaner. 30 mu L of the flexible gold three-electrode cleaner was dropped on the gold three-electrode, stirred with a plastic rod with a diameter of 1mm, and Nafion film for encapsulating the electrode was dissolved and removed, and materials such as chitosan, carbon nanotube, carbon aerogel, prussian blue and the like adhered to the surface of the working electrode were adhered, as shown in FIG. 3C 2. Then, the gold three electrode is rinsed by ultrapure water, and is dried by cold air, so that the cleaned three electrode is obtained, as shown in fig. 3C 3. It can be seen that the finishing material attached to the electrode can be well dissolved and washed by using a suitable cleaning agent.
The above examples are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above examples, and any other changes, modifications, substitutions, combinations, and simplifications that do not depart from the spirit and principle of the present invention should be made in the equivalent manner, and the embodiments are included in the protection scope of the present invention.
Claims (8)
1. A preparation method of a regenerated electrode is characterized by comprising the following steps: the method comprises the following steps:
cleaning the working electrode of the failure sensor by using a cleaning agent to obtain an electrode 1; the cleaning agent contains inorganic alkali and alcohol; the failure sensor comprises a working electrode, wherein the working electrode is covered with a mixture of a binder and at least one of chitosan, carbon nanotubes, carbon aerogel and Prussian blue;
sequentially carrying out cyclic voltammetry scanning on the electrode 1 in KCl/PBS buffer solution and inorganic alkali solution to obtain a regenerated electrode; the cleaning agent comprises 1-4 parts of inorganic alkali solution and 1-2 parts of alcohol by volume; the concentration of the inorganic alkali solution in the cleaning agent is 1-3 mol/L; the binder is a perfluorinated sulfonic acid based polymer Nafion film.
2. The method for producing a regenerated electrode according to claim 1, wherein: the inorganic base in the cleaning agent comprises at least one of sodium hydroxide, potassium hydroxide, magnesium hydroxide, sodium carbonate and potassium carbonate.
3. The method for producing a regenerated electrode according to claim 1, wherein: the alcohol in the cleaning agent comprises at least one of ethanol, methanol and isopropanol.
4. A method for producing a regeneration electrode according to any one of claims 1 to 3, characterized in that: the voltage range for cyclic voltammetry scanning in KCl/PBS buffer was 300-650 mV.
5. The method for producing a regenerated electrode according to claim 4, wherein: the concentration of the KCl/PBS buffer solution is 0.05-0.2 mol/L.
6. The method for producing a regenerated electrode according to claim 4, wherein: the voltage range of the cyclic voltammetry scanning in the inorganic alkali solution is-250 mV to 300 mV.
7. The method for producing a regenerated electrode according to claim 6, wherein: the concentration of the inorganic alkali solution used for cyclic voltammetry scanning is 0.05-1 mol/L.
8. A regenerated electrode produced by the production method according to any one of claims 1 to 7.
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| US8840775B2 (en) * | 2011-12-16 | 2014-09-23 | Utc Fire & Security Corporation | Regenerative gas sensor |
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| EP0326632A1 (en) * | 1988-02-02 | 1989-08-09 | The Dow Chemical Company | Method for the preparation of perfluorosulfonate ionomer films |
| KR20100022165A (en) * | 2008-08-19 | 2010-03-02 | 한남대학교 산학협력단 | Method for preparing enzyme-free glucose sensor and enzyme-free glucose sensor thereby |
| CN111474222A (en) * | 2020-04-22 | 2020-07-31 | 中国药科大学 | Renewable electrochemical sensor for simultaneously detecting epinephrine and uric acid and preparation method and application thereof |
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