CN111874938A - Preparation method of magnesium-copper hydroxy sulfate nano flower-like material - Google Patents
Preparation method of magnesium-copper hydroxy sulfate nano flower-like material Download PDFInfo
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- CN111874938A CN111874938A CN202010777241.2A CN202010777241A CN111874938A CN 111874938 A CN111874938 A CN 111874938A CN 202010777241 A CN202010777241 A CN 202010777241A CN 111874938 A CN111874938 A CN 111874938A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G3/00—Compounds of copper
- C01G3/10—Sulfates
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G3/00—Compounds of copper
- C01G3/006—Compounds containing, besides copper, two or more other elements, with the exception of oxygen or hydrogen
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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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- 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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
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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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/30—Particle morphology extending in three dimensions
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
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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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive electrodes
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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
- Y02E60/10—Energy storage using batteries
Abstract
The invention provides a preparation method of a magnesium-copper hydroxy sulfate nano flower-shaped material, which comprises the following steps: the first step is as follows: dissolving magnesium salt, copper salt and sulfonate in ethanol solution, and magnetically stirring until the magnesium salt, the copper salt and the sulfonate are completely dissolved to form blue solution marked as solution A; the second step is that: adding an alkali metal base solution to the solution, wherein the molar weight ratio of the magnesium salt, the copper salt, the sulfonate and the alkali metal base is as follows: 1: 1: 2: 2, labeled as solution B; the third step: transferring the solution B into a reaction kettle, reacting for 36-48 h at 160-180 ℃, and naturally cooling to room temperature; the fourth step: and centrifuging the blue product, and drying the blue product in an oven at the temperature of 60-80 ℃ to obtain the final product, namely the magnesium-copper hydroxy sulfate nano flower-like material. The invention utilizes an alkaline induction auxiliary solvothermal method to prepare the magnesium-copper hydroxy sulfate nano flower-like material. The preparation method has the advantages of simple method, easy realization of process conditions, low energy consumption and no pollution in preparation.
Description
Technical Field
The invention relates to the technical field of magnesium batteries, in particular to a preparation method of a magnesium-copper hydroxy sulfate nano flower-shaped material.
Background
With the development of human society, the contradiction between the global shortage of energy resources and the increasing demand of people for energy is more and more acute. The development of battery systems with high energy density is a major goal of current power supply systems. Although lithium ion batteries having high specific energy and being environmentally friendly have been widely used in portable mobile appliances such as mobile phones and notebook computers, and in power sources for electric bicycles and electric vehicles. However, because the safety of the lithium ion battery is not well solved, the application of the lithium ion battery as a power battery still has much work to be done.
Magnesium, one of the most abundant light metal elements on earth, is widely used in many fields due to its good physical and chemical properties. Much research is now done on secondary magnesium batteries, all based on secondary lithium ion batteries. Since magnesium and lithium are located diagonally in the periodic table of elements, the melting point of magnesium (648.8 ℃) is much higher than that of lithium (180.5 ℃) and there is no metal mobility of lithium, in addition to having similar atomic radius and chemical properties, so that the secondary magnesium battery is better in safety. Although the specific mass capacity was not as high as lithium (3862mAh/g), it was also quite considerable (2205 mAh/g). In addition, the magnesium resource is very rich in China, the price of magnesium is far lower than that of lithium, and the magnesium is environment-friendly, so that secondary magnesium batteries are more and more concerned by people.
Magnesium copper hydroxy sulfate is often used as a wide band gap semiconductor, and is considered as a promising magnesium ion positive electrode material as a magnesium ion battery positive electrode material. However, magnesium copper hydroxy sulfate is easy to agglomerate, collapse and pulverize during circulation, resulting in poor electrochemical performance of the material. Therefore, the preparation method of the magnesium-copper hydroxy sulfate nano flower-shaped material is provided to solve the problems in the prior art.
Disclosure of Invention
The invention aims to provide a method for preparing a magnesium-copper hydroxy sulfate nano flower-shaped material, which prepares the magnesium-copper hydroxy sulfate nano flower-shaped material by using an alkaline induction auxiliary solvothermal method. The structure has larger specific surface area, and further can improve the electrochemical performance of the material. The problem that the specific capacity is attenuated relatively fast and the electrochemical performance is relatively poor in the circulation process of the magnesium ion battery is solved. And the preparation method is simple, the process conditions are easy to realize, the energy consumption is low, and the preparation is pollution-free.
In order to achieve the purpose, the invention provides the following technical scheme: a method for preparing magnesium-copper hydroxy sulfate nano flower-like material comprises the following steps,
the first step is as follows: dissolving magnesium salt, copper salt and sulfonate in ethanol solution, and magnetically stirring until the magnesium salt, the copper salt and the sulfonate are completely dissolved to form blue solution marked as solution A;
the second step is that: adding an alkali metal base solution to the solution, wherein the molar weight ratio of the magnesium salt, the copper salt, the sulfonate and the alkali metal base is as follows: 1: 1: 2: 2, labeled as solution B;
the third step: transferring the solution B into a reaction kettle, reacting for 36-48 h at 160-180 ℃, and naturally cooling to room temperature;
the fourth step: and centrifuging the blue product, and drying the blue product in an oven at the temperature of 60-80 ℃ to obtain the final product, namely the magnesium-copper hydroxy sulfate nano flower-like material.
Preferably, in the first step, the magnesium salt is one or a combination of magnesium acetate, magnesium citrate and magnesium formate.
Preferably, in the first step, the copper salt is one or a combination of copper acetate, copper citrate and copper formate.
Preferably, in the first step, the sulfonate is one or a combination of sodium dodecyl sulfonate, sodium sulfonate or dioctyl sodium sulfosuccinate.
Preferably, in the second step, the alkali metal base is one or a combination of potassium hydroxide or sodium hydroxide.
Compared with the prior art, the invention has the following beneficial effects:
the invention utilizes an alkaline induction auxiliary solvothermal method to prepare the magnesium-copper hydroxy sulfate nano flower-like material. The structure has larger specific surface area, and further can improve the electrochemical performance of the material. The problem that the specific capacity is attenuated relatively fast and the electrochemical performance is relatively poor in the circulation process of the magnesium ion battery is solved. And the preparation method is simple, the process conditions are easy to realize, the energy consumption is low, and the preparation is pollution-free.
Drawings
FIG. 1 is a graph of the cycle life of the magnesium copper hydroxy sulfate nanoflower of example 1.
FIG. 2 is a graph of the cycle life of the magnesium copper hydroxy sulfate nanoflower of example 2.
FIG. 3 is a graph of rate capability of the magnesium copper hydroxy sulfate nano flower-like material of example 3.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
A method for preparing magnesium-copper hydroxy sulfate nano flower-like material comprises the following steps,
the first step is as follows: dissolving magnesium salt, copper salt and sulfonate in ethanol solution, and magnetically stirring until the magnesium salt, the copper salt and the sulfonate are completely dissolved to form blue solution marked as solution A;
the second step is that: adding an alkali metal base solution to the solution, wherein the molar weight ratio of the magnesium salt, the copper salt, the sulfonate and the alkali metal base is as follows: 1: 1: 2: 2, labeled as solution B;
the third step: transferring the solution B into a reaction kettle, reacting for 36-48 h at 160-180 ℃, and naturally cooling to room temperature;
the fourth step: and centrifuging the blue product, and drying the blue product in an oven at the temperature of 60-80 ℃ to obtain the final product, namely the magnesium-copper hydroxy sulfate nano flower-like material.
The first embodiment is as follows:
a method for preparing magnesium-copper hydroxy sulfate nano flower-like material comprises the following steps,
the first step is as follows: dissolving magnesium acetate, copper acetate and sodium sulfonate in an ethanol solution, and magnetically stirring until the magnesium acetate, the copper acetate and the sodium sulfonate are completely dissolved to form a blue solution which is marked as solution A;
the second step is that: adding a potassium hydroxide solution into the solution, wherein the molar weight ratio of magnesium acetate, copper acetate, sodium sulfonate and potassium hydroxide is as follows: 1: 1: 2: 2, labeled as solution B;
the third step: transferring the solution B into a reaction kettle, reacting for 48 hours at 160 ℃, and naturally cooling to room temperature;
the fourth step: and centrifuging the blue product, and drying the blue product in an oven at 60 ℃ to obtain the final product, namely the magnesium-copper hydroxy sulfate nano flower-like material.
FIG. 1 is a graph of cycle life of magnesium copper hydroxy sulfate nanoflower at 0.1C rate. The first discharge specific capacity is 352mAh/g, after 40 times of circulation, the discharge specific capacity is 296mAh/g, and the capacity retention rate is 84.1%.
Example two:
a method for preparing magnesium-copper hydroxy sulfate nano flower-like material comprises the following steps,
the first step is as follows: dissolving magnesium citrate, copper citrate and sodium dodecyl sulfate in ethanol solution, and magnetically stirring until the magnesium citrate, the copper citrate and the sodium dodecyl sulfate are completely dissolved to form blue solution marked as solution A;
the second step is that: adding a potassium hydroxide solution into the solution, wherein the molar weight ratio of the magnesium citrate to the copper citrate to the sodium dodecyl sulfate to the sodium hydroxide is as follows: 1: 1: 2: 2, labeled as solution B;
the third step: transferring the solution B into a reaction kettle, reacting for 36 hours at 180 ℃, and naturally cooling to room temperature;
the fourth step: and centrifuging the blue product, and drying the blue product in an oven at 80 ℃ to obtain the final product, namely the magnesium-copper hydroxy sulfate nano flower-like material.
FIG. 2 is a graph of cycle life of magnesium copper hydroxy sulfate nanoflower at 0.1C rate. The initial discharge specific capacity is 348mAh/g, after 40 times of circulation, the discharge specific capacity is 290mAh/g, and the capacity retention rate is 83.3%.
Example three:
a method for preparing magnesium-copper hydroxy sulfate nano flower-like material comprises the following steps,
the first step is as follows: magnesium citrate, copper citrate and sodium dioctyl sulfosuccinate are dissolved in an ethanol solution, and are magnetically stirred until the magnesium citrate, the copper citrate and the sodium dioctyl sulfosuccinate are completely dissolved to form a blue solution which is marked as solution A;
the second step is that: adding a potassium hydroxide solution into the solution, wherein the molar weight ratio of magnesium citrate to copper citrate to sodium dioctyl sulfosuccinate to sodium hydroxide is as follows: 1: 1: 2: 2, labeled as solution B;
the third step: transferring the solution B into a reaction kettle, reacting for 48 hours at 180 ℃, and naturally cooling to room temperature;
the fourth step: and centrifuging the blue product, and drying the blue product in an oven at 80 ℃ to obtain the final product, namely the magnesium-copper hydroxy sulfate nano flower-like material.
FIG. 3 is a graph of rate capability of magnesium copper hydroxy sulfate nano flower-like material under different rates. The average specific discharge capacity of 0.1C is about 330mAh/g, after 0.1C activation, the average specific discharge capacity of 0.5C is about 350mAh/g, the average specific discharge capacity of 5C is about 252mAh/g, the average specific discharge capacity is returned to 0.1C again, and the average specific discharge capacity is about 330 mAh/g.
The invention utilizes an alkaline induction auxiliary solvothermal method to prepare the magnesium-copper hydroxy sulfate nano flower-like material. The structure has larger specific surface area, and further can improve the electrochemical performance of the material. The problem that the specific capacity is attenuated relatively fast and the electrochemical performance is relatively poor in the circulation process of the magnesium ion battery is solved. And the preparation method is simple, the process conditions are easy to realize, the energy consumption is low, and the preparation is pollution-free.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (5)
1. A method for preparing magnesium-copper hydroxy sulfate nano flower-like material is characterized by comprising the following steps,
the first step is as follows: dissolving magnesium salt, copper salt and sulfonate in ethanol solution, and magnetically stirring until the magnesium salt, the copper salt and the sulfonate are completely dissolved to form blue solution marked as solution A;
the second step is that: adding an alkali metal base solution to the solution, wherein the molar weight ratio of the magnesium salt, the copper salt, the sulfonate and the alkali metal base is as follows: 1: 1: 2: 2, labeled as solution B;
the third step: transferring the solution B into a reaction kettle, reacting for 36-48 h at 160-180 ℃, and naturally cooling to room temperature;
the fourth step: and centrifuging the blue product, and drying the blue product in an oven at the temperature of 60-80 ℃ to obtain the final product, namely the magnesium-copper hydroxy sulfate nano flower-like material.
2. The method for preparing the magnesium-copper hydroxy sulfate nano flower-like material according to claim 1, which is characterized in that: in the first step, the magnesium salt is one or the combination of magnesium acetate, magnesium citrate or magnesium formate.
3. The method for preparing the magnesium-copper hydroxy sulfate nano flower-like material according to claim 1, which is characterized in that: in the first step, the copper salt is one or the combination of copper acetate, copper citrate or copper formate.
4. The method for preparing the magnesium-copper hydroxy sulfate nano flower-like material according to claim 1, which is characterized in that: in the first step, the sulfonate is one or a combination of sodium dodecyl sulfonate, sodium sulfonate or dioctyl sodium sulfosuccinate.
5. The method for preparing the magnesium-copper hydroxy sulfate nano flower-like material according to claim 1, which is characterized in that: in the second step, the alkali metal base is one or a combination of potassium hydroxide or sodium hydroxide.
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