CN108172758B - New application of recovered expired tetracycline antibiotic medicine - Google Patents
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- CN108172758B CN108172758B CN201711249274.4A CN201711249274A CN108172758B CN 108172758 B CN108172758 B CN 108172758B CN 201711249274 A CN201711249274 A CN 201711249274A CN 108172758 B CN108172758 B CN 108172758B
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
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- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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- H01M10/058—Construction or manufacture
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/04—Processes of manufacture in general
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- H01M4/0404—Methods of deposition of the material by coating on electrode collectors
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
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- 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
- Y02E60/10—Energy storage using batteries
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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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention discloses an application method of expired tetracycline antibiotic drugs, and belongs to the technical field of new energy materials. Grinding expired tetracycline antibiotic drugs into powder, mixing the powder with a conductive agent and a binder to obtain an electrode material mixture, adding the electrode material mixture into an N-methylpyrrolidone solvent, and uniformly stirring to obtain electrode slurry; uniformly coating the electrode slurry on the surface of the current collector, and performing vacuum drying to obtain an electrode plate; the lithium ion rechargeable battery or the sodium ion rechargeable battery is assembled by taking an electrode plate as a working electrode, a lithium foil or a sodium foil as a counter electrode and a reference electrode and a porous polypropylene film, a polyethylene film, glass fiber or non-woven fabric as a diaphragm under the anhydrous and anaerobic conditions. The invention has the advantages of environmental protection, strong practicability and low cost, firstly uses the overdue tetracycline antibiotic medicines in the field of new energy materials, and provides a new way and a new scheme for recycling and applying the overdue antibiotic medicines.
Description
Technical Field
The invention relates to an application method of expired tetracycline antibiotic drugs, and belongs to the technical field of new energy materials.
Background
With the rapid development of the socioeconomic level and the rapid improvement of the health consciousness of people, the production amount of the medicine is gradually increased year by year. Once the supply exceeds the demand, it is easy to produce large amounts of expired drugs. However, the improper treatment of overdue drugs can cause the residual effective components to enter the environment and cause negative effects on the ecosystem, and especially the problems of environmental pollution and ecological toxicity of antibiotic drugs have attracted much attention. Among them, tetracycline antibiotics have the advantages of broad-spectrum antibacterial, high quality and low price, have the effect of inhibiting the synthesis of bacterial proteins, are commonly used for treating various bacterial infections, and are a class of antibiotics which are widely applied at present. The classes include mainly natural tetracyclines (such as tetracycline, oxytetracycline, chlortetracycline and demeclocycline) and semi-synthetic tetracyclines (such as methacycline, doxycycline and minocycline). Researches show that the tetracycline antibiotics not only have adverse effects on animals and plants (such as causing severe DNA damage of fishes or inhibiting the root growth of plants, but also cause the reduction of microbial diversity in soil and finally cause the deterioration of soil ecology), and in addition, bacterial drug resistance caused by antibiotics is one of the main problems facing the treatment of a large number of clinical infectious diseases, and seriously threatens public health safety.
Although the organisms in the environment can spontaneously produce antibiotics, most antibiotic contamination is still a result of human factors. In addition to the metabolic residues after administration to humans or livestock, improper handling of expired drugs is a major route for such drugs to enter the ecological environment. Overdue drugs are mainly from medical units or household reserves, and for overdue drugs of medical units, a common strategy is to burn or bury the overdue drugs at high temperature after being uniformly recovered by related departments. The high-temperature incineration can effectively degrade active ingredients in the medicine, but has high energy consumption and is easy to cause secondary pollution to the environment; the landfill method is difficult to biodegrade the stable effective components in the overdue drugs, and is not beneficial to protecting the ecological environment. As for overdue drugs generated by household storage, due to the reasons of relatively dispersed distribution, low social environmental awareness of people, high recovery cost and the like, the overdue drugs are usually directly discarded as conventional garbage, and residual effective ingredients are easier to enter the ecological environment. In a word, no effective and systematic recovery and application system is formed for expired tetracycline antibiotics at present, which not only seriously affects the ecological environment, but also wastes resources, and a new application approach in the aspect of tetracycline drug recovery is urgently needed to be developed.
Disclosure of Invention
The invention provides a new application method of overdue tetracycline antibiotic medicines for the first time aiming at the recycling problem of the overdue tetracycline antibiotic medicines, and particularly mainly aims to use the overdue tetracycline antibiotic medicines as electrode materials of rechargeable batteries and construct a novel association between the overdue antibiotic medicines and the electrode materials of the batteries.
An application method of an overdue tetracycline antibiotic medicine comprises the following specific steps:
(1) grinding expired tetracycline antibiotic drugs into powder, mixing the powder with a conductive agent and a binder to obtain an electrode material mixture, adding the electrode material mixture into an N-methylpyrrolidone solvent, and uniformly stirring to obtain electrode slurry; wherein the conductive agent is acetylene black, Ketjen black, conductive graphite, conductive carbon black or carbon nano tube, and the binder is polyvinyl alcohol, polytetrafluoroethylene, carboxymethyl cellulose or polyvinylidene fluoride;
(2) uniformly coating the electrode slurry obtained in the step (1) on the surface of a current collector, and drying in vacuum to obtain an electrode slice;
(3) assembling a lithium ion rechargeable battery or a sodium ion rechargeable battery by taking the electrode slice obtained in the step (2) as a working electrode, a lithium foil or a sodium foil as a counter electrode and a reference electrode and a PP (polypropylene) film, a PE (polyethylene) film, glass fiber or non-woven fabric as a diaphragm under the anhydrous and oxygen-free conditions;
the tetracycline antibiotic medicines in the step (1) comprise tetracycline, tetracycline hydrochloride, oxytetracycline hydrochloride, chlortetracycline hydrochloride, demeclocycline hydrochloride, methacycline hydrochloride tablets, doxycycline hydrochloride, minocycline or minocycline hydrochloride; by mass percentage, the electrode material mixture comprises 60-85% of traditional Chinese medicine powder, 10-30% of conductive agent and 5-10% of binder;
the dosage forms of the tetracycline antibiotic medicines in the step (1) comprise tablets, capsules, pills or granules, powder and the like;
the tetracycline antibiotic medicine in the step (1) can be an antibiotic medicine for human, or an antibiotic medicine for poultry, livestock and fish;
the current collector in the step (2) is copper, iron or nickel, and the shape of the current collector is net-shaped, foil-shaped or foam-shaped.
The invention has the beneficial effects that:
(1) the invention applies the expired tetracycline antibiotics to the field of new energy materials for the first time, which not only can relieve the influence of the tetracycline antibiotics on the ecological environment, but also can give full play to the utilization value of waste resources;
(2) the recycling application process is simple and practical, the operability is strong, and secondary pollution which may occur in the resource recycling application process can be effectively avoided;
(3) the invention explores the application feasibility of the electrode based on the expired tetracycline antibiotic drugs in the lithium ion rechargeable battery or the sodium ion rechargeable battery, and constructs a novel association between the expired antibiotic drugs and the battery electrode material.
Drawings
FIG. 1 is a schematic diagram of the molecular structure of a tetracycline antibiotic;
FIG. 2 is an SEM photograph of the expired tetracycline drug powder of example 1;
FIG. 3 is an FTIR spectrum of the expired tetracycline drug powder of example 2;
fig. 4 is a charge/discharge curve of a simulated sodium ion battery prepared in example 3;
FIG. 5 is a cycle stability curve for a simulated lithium ion battery prepared in example 4;
FIG. 6 is a graph of rate capability of a simulated lithium ion battery prepared in example 5;
fig. 7 is a charge/discharge curve of a simulated lithium ion battery prepared in example 6.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments, but the scope of the present invention is not limited to the description.
The chemical structure of the tetracycline antibiotic in the embodiment of the invention is shown in fig. 1, and as can be seen from fig. 1, the basic chemical structure of the tetracycline antibiotic drug is formed by connecting four benzene rings, and functional groups such as carbonyl, hydroxyl, amide, tertiary amine, methyl and the like are connected to the benzene rings, and are collectively called as "polycyclic benzamide derivatives".
Example 1: an application method of an overdue tetracycline antibiotic medicine comprises the following specific steps:
(1) after the overdue tetracycline tablets are ground into powder, the microscopic morphology of the overdue tetracycline tablets is tested, as shown in fig. 2, as can be seen from fig. 2, the tetracycline medicine powder presents a random particle morphology, and the particle size is not more than 10 μm; then uniformly mixing the overdue tetracycline powder, the conductive graphite and the polyvinyl alcohol to obtain an electrode material mixture, adding the electrode material mixture into an N-methylpyrrolidone solvent, and uniformly stirring to obtain electrode slurry; wherein, the overdue tetracycline powder accounts for 60 percent, the conductive agent (conductive graphite) accounts for 30 percent and the binder (polyvinyl alcohol) accounts for 10 percent in the electrode material mixture in percentage by mass;
(2) uniformly coating the electrode slurry obtained in the step (1) on the surface of a copper foil current collector, and carrying out vacuum drying for 24 hours at the temperature of 60 ℃ to obtain an electrode slice;
(3) assembling a button type simulated sodium ion battery in a glove box filled with high-purity argon, namely assembling the sodium ion battery by taking a sodium sheet as a counter electrode and a reference electrode, taking the electrode sheet obtained in the step (2) as a working electrode, taking porous non-woven fabric as a diaphragm and taking solution A as electrolyte under the anhydrous and oxygen-free conditions, wherein the solute in the solution A is 1 mol/L NaClO4The solvent is a mixed solvent of ethylene carbonate and propylene carbonate, the volume ratio of the ethylene carbonate to the propylene carbonate is 1:1, and 5% of ethylene carbonate in the ethylene carbonate is fluorinated.
Example 2: an application method of an overdue tetracycline antibiotic medicine comprises the following specific steps:
(1) after the particles in the expired tetracycline capsule were further ground, the microstructure was examined by Fourier transform infrared spectroscopy as shown in FIG. 3, which shows that at 3421 cm-1、1257 cm-1、740 cm-1The left and the right respectively correspond to the stretching vibration, the in-plane bending vibration and the out-of-plane bending vibration of the N-H bond; at 3676 cm-1、1398 cm-1And 670 cm-1The positions of (a) are respectively corresponding to the stretching vibration, the in-plane bending vibration and the out-of-plane bending vibration of the O-H bond; at 2922 cm-1、1327 cm-1And 860 cm-1The nearby peak corresponds to-CH3The stretching vibration, the in-plane bending vibration and the out-of-plane bending vibration of (1); c = O expansion vibration at 1640cm-1And 1609 cm-1The left and right peaks correspond to 1508 cm-1、1457 cm-1、1045 cm-1And 949 cm-1Corresponding to the stretching vibration of C = C, C-C in the aromatic ring and the in-plane and out-of-plane bending vibration of C-H bond on the ring, at 1185 cm-1And 1109 cm-1The main component in the tetracycline medicine powder is still 6-methyl-4- (dimethylamino) -3,6,10,12,12 α -pentahydroxyl-1, 11-dioxo-1, 4,4 α,5,5 α,6,11,12 α -octahydro-2-tetracene formamide, the overdue tetracycline medicine powder, the carbon nano tube and the polytetrafluoroethylene are uniformly mixed to obtain an electrode material mixture, the electrode material mixture is added into an N-methyl pyrrolidone solvent, and the electrode material mixture is uniformly stirred to obtain electrode slurry, wherein the overdue tetracycline medicine powder accounts for 85 percent, the conductive agent (the carbon nano tube) accounts for 10 percent and the binder (the polytetrafluoroethylene) accounts for 5 percent by mass;
(2) uniformly coating the electrode slurry obtained in the step (1) on the surface of a nickel foil current collector, and carrying out vacuum drying for 24 hours at the temperature of 60 ℃ to obtain an electrode slice;
(3) assembling a button type simulated sodium ion battery in a glove box filled with high-purity argon, namely assembling the sodium ion battery by taking sodium sheets as a counter electrode and a reference electrode, taking electrode sheets obtained in the step (2) as working electrodes, taking glass fiber as a diaphragm and taking solution A as electrolyte under the anhydrous and oxygen-free conditions, and testing the electrochemical performance of the sodium ion battery by using a constant current charge/discharge method, wherein the solute in the solution A is 1 mol/L NaClO4The solvent is a mixed solvent of ethylene carbonate and propylene carbonate, the volume ratio of the ethylene carbonate to the propylene carbonate is 1:1, and 5% of ethylene carbonate in the ethylene carbonate is fluorinated.
Example 3: an application method of an overdue tetracycline antibiotic medicine comprises the following specific steps:
(1) further grinding particles in the expired tetracycline capsule, uniformly mixing the particles with acetylene black and sodium carboxymethylcellulose to obtain an electrode material mixture, adding the electrode material mixture into an N-methylpyrrolidone solvent, and uniformly stirring to obtain electrode slurry; wherein, the overdue tetracycline medicine powder accounts for 70 percent, the conductive agent (acetylene black) accounts for 20 percent and the binder (sodium carboxymethylcellulose) accounts for 10 percent in the electrode material mixture in percentage by mass;
(2) uniformly coating the electrode slurry obtained in the step (1) on the surface of a nickel foil current collector, and performing vacuum drying at 60 ℃ for 12 hours to obtain an electrode slice;
(3) assembling a button type simulated sodium ion battery in a glove box filled with high-purity argon, namely assembling the sodium ion battery by taking sodium sheets as a counter electrode and a reference electrode, taking the electrode sheets obtained in the step (2) as working electrodes, taking a porous glass fiber membrane as a diaphragm and taking a solution A as electrolyte under the anhydrous and oxygen-free conditions, and testing the electrochemical performance of the sodium ion battery by using a constant current charge/discharge method, wherein the solute in the solution A is 1 mol/L NaClO4The solvent is a mixed solvent of ethylene carbonate and propylene carbonate, the volume ratio of the ethylene carbonate to the propylene carbonate is 1:1, and 5% of ethylene carbonate in the ethylene carbonate is fluorinated;
the electrochemical performance of the sodium-ion battery of this example is shown in fig. 4, and it can be seen from fig. 4 that after 50 cycles of charge/discharge test, the battery capacity is stabilized at 38 mAh/g, and the curves of the 25 th and 50 th cycles are substantially overlapped, which indicates that the electrode sheet of the simulated sodium-ion battery in this example has better charge/discharge cycle stability.
Embodiment 4, an application method of an overdue tetracycline antibiotic drug comprises the following specific steps:
(1) grinding overdue oxytetracycline tablets into powder, uniformly mixing with Ketjen black and polyvinylidene fluoride to obtain an electrode material mixture, adding the electrode material mixture into an N-methylpyrrolidone solvent, and uniformly stirring to obtain electrode slurry; wherein the expired oxytetracycline drug powder accounts for 60 percent, the conductive agent (Keqin black) accounts for 30 percent and the binder (polyvinylidene fluoride) accounts for 10 percent in the electrode material mixture in percentage by mass;
(2) uniformly coating the electrode slurry obtained in the step (1) on the surface of an iron foil current collector, and carrying out vacuum drying for 24 hours at the temperature of 60 ℃ to obtain an electrode slice;
(3) assembling a button type simulated lithium ion battery in a glove box filled with high-purity argon, namely assembling the lithium ion battery in the glove box filled with the high-purity argon by taking a lithium sheet as a counter electrode and a reference electrode, taking an electrode slice obtained in the step (2) as a working electrode, taking a Porous Polypropylene (PP) membrane as a diaphragm and taking a solution B as an electrolyte, and testing the electrochemical performance of the lithium ion battery by using a constant current charge/discharge method, wherein the solute in the solution B is L iPF of 1 mol/L6The solvent is a mixed solvent of ethylene carbonate and propylene carbonate, and the volume ratio of the ethylene carbonate to the propylene carbonate is 1: 1;
the electrochemical performance of the lithium ion battery of the embodiment is shown in fig. 5, and as can be seen from fig. 5, after 50 cycles of charge/discharge test, the battery capacity is stabilized at 150mAh/g, the battery has better cycle stability and the coulombic efficiency is close to 100%, which indicates that the electrode sheet for simulating the lithium ion battery in the embodiment has higher electrochemical reaction reversibility.
Example 5: an application method of an overdue tetracycline antibiotic medicine comprises the following specific steps:
(1) grinding the overdue tetracycline tablets into powder, uniformly mixing the powder with acetylene black and polyvinylidene fluoride to obtain an electrode material mixture, adding the electrode material mixture into an N-methyl pyrrolidone solvent, and uniformly stirring to obtain electrode slurry; wherein, the overdue tetracycline medicine powder accounts for 60 percent, the conductive agent (acetylene black) accounts for 30 percent and the binder (polyvinylidene fluoride) accounts for 10 percent in the electrode material mixture in percentage by mass;
(2) uniformly coating the electrode slurry obtained in the step (1) on the surface of a foam copper current collector, and performing vacuum drying at the temperature of 60 ℃ for 24 hours to obtain an electrode slice;
(3) assembling a button type simulated lithium ion battery in a glove box filled with high-purity argon, namely assembling the lithium ion battery in the glove box filled with the high-purity argon by taking a lithium sheet as a counter electrode and a reference electrode, taking an electrode sheet obtained in the step (2) as a working electrode, taking a Porous Polypropylene (PP) membrane as a diaphragm and taking a solution B as an electrolyte, and testing the electrochemical performance of the lithium ion battery by using a constant current charge/discharge method, wherein the solute in the solution B is 1 mol/LLiPF6The solvent is a mixed solvent of ethylene carbonate and propylene carbonate, and the volume ratio of the ethylene carbonate to the propylene carbonate is 1: 1;
as shown in fig. 6, it can be seen from fig. 6 that when the current densities are 100 mA/g, 200 mA/g, 400 mA/g, 800 mA/g and 1600 mA/g, the specific capacities of the lithium ion batteries of the present embodiment can be respectively maintained at about 230mAh/g, 195 mAh/g, 150mAh/g, 80 mAh/g and 50mAh/g, and when the current density is restored to 50 mA/g, the specific capacity is increased from the initial 250 mAh/g to 280 mAh/g, which illustrates that the electrode material for simulating the lithium ion batteries of the present embodiment has high tolerance to large current changes.
Example 6: an application method of an overdue tetracycline antibiotic medicine comprises the following specific steps:
(1) further grinding the medicine powder in the overdue doxycycline hydrochloride capsule, uniformly mixing the medicine powder with conductive carbon black and polyvinylidene fluoride to obtain an electrode material mixture, adding the electrode material mixture into an N-methyl pyrrolidone solvent, and uniformly stirring to obtain electrode slurry; wherein, the overdue doxycycline hydrochloride powder accounts for 60 percent, the conductive agent (conductive carbon black) accounts for 30 percent and the binder (polyvinylidene fluoride) accounts for 10 percent in the electrode material mixture in percentage by mass;
(2) uniformly coating the electrode slurry obtained in the step (1) on the surface of a foam copper current collector, and performing vacuum drying for 24 hours at the temperature of 60 ℃ to obtain an electrode plate;
(3) assembling a button type simulated lithium ion battery in a glove box filled with high-purity argon, namely assembling the lithium ion battery in the glove box filled with the high-purity argon by taking a lithium sheet as a counter electrode and a reference electrode, taking the electrode slice obtained in the step (2) as a working electrode, taking a PE (polyethylene) membrane as a diaphragm and taking a solution B as electrolyte, and testing the electrochemical performance of the lithium ion battery by using a constant current charge/discharge method, wherein the solute in the solution B is L iPF mol/L6The solvent is a mixed solvent of ethylene carbonate and propylene carbonate, and the volume ratio of the ethylene carbonate to the propylene carbonate is 1: 1;
as shown in fig. 7, it can be seen from fig. 7 that, in the case of the lithium ion battery of the present example having a current density of 50 mA/g,the specific discharge capacity of the first circle reaches 310 mAh/g, and in the subsequent circulation, the specific discharge capacity is close to 175 mAh/g, which shows that the electrode material of the simulated lithium ion battery in the embodiment enters stable reversible de/intercalation L i+The stage (2) shows better electrochemical performance.
Claims (2)
1. An application method of an overdue tetracycline antibiotic medicine is characterized by comprising the following specific steps:
(1) grinding expired tetracycline antibiotic drugs into powder, mixing the powder with a conductive agent and a binder to obtain an electrode material mixture, adding the electrode material mixture into an N-methylpyrrolidone solvent, and uniformly stirring to obtain electrode slurry; wherein the conductive agent is acetylene black, Ketjen black, conductive graphite or carbon nano tube, and the binder is polyvinyl alcohol, polytetrafluoroethylene, carboxymethyl cellulose or polyvinylidene fluoride; by mass percentage, the electrode material mixture comprises 60-85% of traditional Chinese medicine powder, 10-30% of conductive agent and 5-10% of binder; tetracycline antibiotic drugs include tetracycline, tetracycline hydrochloride, oxytetracycline hydrochloride, chlortetracycline hydrochloride, demeclocycline hydrochloride, methacycline hydrochloride tablets, doxycycline hydrochloride, minocycline, or minocycline hydrochloride;
(2) uniformly coating the electrode slurry obtained in the step (1) on the surface of a current collector, and drying in vacuum to obtain an electrode slice;
(3) and (3) assembling the lithium ion battery or the sodium ion battery by taking the electrode slice obtained in the step (2) as a working electrode, a lithium foil or a sodium foil as a counter electrode and a reference electrode and a PP (polypropylene) film, a PE (polyethylene) film, glass fiber or non-woven fabric as a diaphragm under the anhydrous and oxygen-free conditions.
2. The method of using an expired tetracycline antibiotic drug as in claim 1, wherein: and (3) the current collector in the step (2) is made of copper, iron or nickel, and the shape of the current collector is net-shaped, foil-shaped or foam-shaped.
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锂离子电池负极材料对苯二甲酸的电化学性能;邹崴等;《中国化学会第29届学术年会摘要集-第24分会:化学电源》;20141231;摘要 * |
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