CN112899704A - Electrochemical method for preparing high-purity molybdenum disulfide nanosheet from molybdenite - Google Patents
Electrochemical method for preparing high-purity molybdenum disulfide nanosheet from molybdenite Download PDFInfo
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Abstract
The invention discloses an electrochemical method for preparing a high-purity molybdenum disulfide nanosheet by utilizing molybdenite, wherein the purity of the obtained molybdenum disulfide nanosheet is up to more than 99.0%, and the average thickness of the nanosheet is only 10-30 nm. The method comprises the following preparation steps: (1) placing alkali metal chloride in a nickel reaction vessel, melting at high temperature, and then reducing the temperature of the molten salt to the reaction temperature; (2) adding molybdenite into a nickel container, immersing the nickel container in molten salt, taking the nickel container as a cathode and the molten salt as an electrolyte, and installing an anode for electrolysis; (3) and after the electrolysis is finished, taking out the anode, cooling to room temperature under an inert atmosphere, collecting the deposit on the surface of the anode, and washing and drying to obtain the high-purity molybdenum disulfide powder. The method has the advantages of simple operation, clean process and low preparation cost; the obtained molybdenum disulfide nanosheet is stable in property, and shows good lithium storage performance and electrochemical stability when used as a lithium ion battery cathode material.
Description
Technical Field
The invention belongs to the technical field of metallurgical engineering, and particularly relates to an electrochemical method for preparing high-purity molybdenum disulfide nanosheets from molybdenite serving as a raw material in a short process, and application of a molybdenum disulfide material in the field of lithium batteries.
Background
The molybdenum disulfide nano material shows wide application prospect in the fields of photoelectric device manufacturing, heterogeneous photoelectrocatalysis, solid lubrication materials, electrochemical energy storage and the like due to special chemical and electronic structures and excellent mechanical, optical and electrical characteristics. However, the scale preparation of the high-performance nano molybdenum disulfide still faces a lot of problems. Currently, molybdenite (main component is MoS) is industrially used mostly2The most important molybdenum source for preparing molybdenum-based compounds) as raw materials to prepare molybdenum disulfide, and the preparation method mainly comprises a physical method and a chemical synthesis method. Separating molybdenum disulfide from molybdenum concentrate by physical method through flotation-chemical leaching and other processes, and obtaining MoS by using the method2The size is large, the impurity content is high, and the subsequent application of the product is not facilitated. The chemical synthesis method mainly comprises a series of chemical processes of roasting, ammonia leaching, acid precipitation, vulcanization, high-temperature desulfurization and the like of molybdenite, and the molybdenite (MoS) is subjected to2)→MoO3→(NH4)2MoO4→(NH4)2MoS4→MoS3→MoS2And finally obtaining the molybdenum disulfide product with higher purity through phase evolution. But the method also has the disadvantages of low conversion rate, high requirement on the grade of the ore raw material, complex process, larger pollution, higher cost and the like. In addition, the structure and the appearance of the molybdenum disulfide product are difficult to control effectively by using the two methods, so that the performance of the molybdenum disulfide product cannot be ensured.
In recent years, researchers have proposed a variety of nano-MoS2The preparation methods of (1) include Chemical Vapor Deposition (CVD), hydrothermal method, organic-inorganic hybrid conversion method, etc., which are advantageous but not too short of the large-scale industrial application. With the molybdenum disulfide materialThe continuous expansion of the application field, the development of economic, clean, short-flow and large-scale preparation process is still the research focus of the related field.
Disclosure of Invention
Aiming at the problems, the invention aims to provide a short-process electrochemical method for preparing high-purity molybdenum disulfide nanosheets by directly taking molybdenite as a raw material. The method takes chloride molten salt with low oxygen anion solubility as electrolyte, and releases sulfur element in molybdenite into the molten salt in the form of sulfur anions through an electrolytic reduction mode; oxygen elements in the ore are greatly enriched in the ore area due to low solubility of negative ions, and then are rapidly combined with molybdenum elements remained in the ore to form soluble molybdate ions; the molybdate ions migrate to the anode region under the action of an electric field, and then combine with sulfur negative ions (forming thiomolybdate ions) which also migrate to the anode region, discharge, and finally deposit on the surface of the anode to form a nano-scale thickness molybdenum disulfide flaky material. In the process, MoS2The phase transformation path of (a) is mainly the cathode region: MoS2+e-→Mo+S2-；Mo+[O]→MoO4 2-(ii) a An anode region: MoO4 2-+S2-→MoS4 2-+O2-；MoS4 2--e-→MoS2+ S ↓. The molybdenum disulfide nanosheet prepared by the method disclosed by the invention is high in purity which can reach more than 99.0%, and can be used as a lithium ion battery cathode material.
The technical scheme provided by the invention is as follows:
one of the purposes of the invention is to provide an electrochemical method for preparing high-purity molybdenum disulfide nanosheets by utilizing molybdenite, wherein the whole reaction process is carried out in an inert gas atmosphere, and the electrochemical method comprises the following preparation steps:
(1) putting alkali metal chloride in a nickel container, melting at high temperature, and cooling to reaction temperature;
(2) adding molybdenite into a nickel container, immersing the nickel container in molten salt, taking the nickel container as a cathode and the molten salt as an electrolyte, and installing an anode for electrolysis;
(3) and after the electrolysis is finished, taking out the anode, cooling to room temperature, collecting the deposit on the surface of the anode, and washing and drying to obtain the molybdenum disulfide powder with purity higher than high purity.
In the invention, the anode after the electrolysis is cooled under the protection of inert gas, so that the anode product can not generate other side reactions under the high-temperature condition to cause component change.
The method of the invention uses molten alkali metal chloride as electrolyte, selectively converts the extremely refractory molybdenum disulfide (melting point is about 2375 ℃) component in molybdenite into soluble thiomolybdate ions by an electrolysis means, and then the thiomolybdate ions are discharged on the surface of an anode and are separated out in the form of solid molybdenum disulfide. The method disclosed by the invention is simple to operate, low in energy consumption, low in operation cost and clean in process, and the prepared ultrathin molybdenum disulfide nanosheet can be used as a high-efficiency lithium ion battery cathode material.
The nickel container was used as the cathode because nickel maintained good conductivity and stability in the molten sodium/potassium chloride salt at the reaction temperature defined in the present invention, stably provided electrons for the molybdenum disulfide conversion reaction, had a low dissolution rate, and was responsible for the anode product (MoS)2Nanoplatelets) the effect of purity is small.
Further, in the step (1), the alkali metal chloride is selected from any one or a mixture of two of KCl and NaCl, and the purity is industrial purity or above.
Further, the reaction temperature in the step (1) is 670-.
Further, in the step (2), the molybdenum grade of the molybdenite ore is 10-51 wt%, and the oxygen content in the ore is more than 3 wt%.
Further, the particle size of the molybdenite ore in the step (2) is less than 20 mm.
Further, the anode in the step (2) is selected from any one of a graphite anode, a molybdenum disulfide coating anode, a carbon cloth anode and a charcoal anode, and the electrode form includes a plate shape, an arc shape, a column shape and a cylinder shape.
Further, the electrolysis mode in the step (2) is constant-voltage or constant-current electrolysis.
Further, in the step (2), when constant-voltage electrolysis is adopted, the pressure of the electrolytic cell is 2.1-3.5V; when constant current electrolysis is adopted, the required cathode current density is 0.1-5000mA/1g molybdenite.
Further, the method for washing the anode deposit in the step (3) comprises soaking the anode deposit in deionized water, and then sequentially carrying out ultrasonic cleaning by using ethanol and deionized water/ultrapure water.
The invention also aims to provide application of the molybdenum disulfide nanosheet prepared by the method as a lithium ion battery cathode material in the field of electrochemical energy storage device preparation.
The invention has the beneficial effects that:
1. the short-flow fused salt electrochemical method is provided, the molybdenum disulfide nanosheet with high purity and good electrochemical stability can be directly and effectively extracted from molybdenite ore, and the method has low requirement on the grade of ore raw materials.
2. The preparation method provided by the invention is simple to operate, short in flow, low in energy consumption (clean energy can be used for supplying energy), cleaner in process (no sulfur-containing waste gas is generated and no ammonia-containing waste water is discharged), lower in raw material cost, and recyclable in used molten salt after treatment, so that the preparation method has a certain industrial application potential.
3. The molybdenum disulfide nanosheet prepared by the method has the advantages of high purity (over 99.0%), high crystallization degree, good stability, thin lamella thickness (10-30nm), excellent electrochemical performance and the like, can be used as a high-performance lithium ion battery cathode material, and shows higher capacity and better charge-discharge cycle stability.
Drawings
FIG. 1 is a schematic view of an electrolytic reaction apparatus used in example 1;
FIG. 2 optical photographs of the graphite anode before and after the electrolytic reaction in example 1;
FIG. 3(a) SEM image of molybdenite raw material (scraped from the ore surface for characterization) and molybdenum disulfide nanosheets prepared in example 1; fig. 3(b) is a high magnification SEM image of molybdenum disulfide nanoplates;
figure 4 XRD spectrum of molybdenum disulphide nanosheets obtained in example 1;
fig. 5 is a charge-discharge curve of a negative electrode of a lithium battery made using the molybdenum disulfide nanosheets obtained in example 1;
fig. 6 is a rate performance test of a negative electrode of a lithium battery made by using the molybdenum disulfide nanosheets obtained in example 1;
fig. 7 shows the cycle performance test of the lithium battery negative electrode made of the molybdenum disulfide nanosheet obtained in example 1.
Detailed Description
The following examples are provided to further illustrate the present invention for better understanding, but the present invention is not limited to the following examples.
Example 1
(1) 1000g of NaCl-KCl (50:50 mol%) mixture was filled into a nickel container of an appropriate size, and one end of a molybdenum rod was connected to the nickel container while the other end extended outside the reactor and connected to the cathode of an external power supply. The nickel vessel was slowly heated to 800 c (temperature rise rate not more than 20 c/min) using an electric furnace under the protection of argon atmosphere to melt the chloride salt, and then the temperature of the salt was reduced to 700 c within 30 min.
(2) Mechanically crushing molybdenite ore with the molybdenum content of about 46.33%, and screening to obtain molybdenite particles with the particle size of below 20 mm; a cylindrical graphite anode is selected, screened molybdenite particles (the mass is about 10g) are put into a nickel container, and constant-voltage electrolysis (the pressure of an electrolytic bath is 2.9V) is carried out under the argon atmosphere for 2.5 h.
(3) And after the electrolysis is finished, collecting the anode deposition product, washing the product by using deionized water, and drying to obtain molybdenum disulfide nanosheet powder with the purity of about 99.7% (the mass fraction of Mo is 59.77%).
FIG. 1 is a schematic view of an electrolytic reaction apparatus used in example 1. FIG. 2 is an optical photograph of the graphite anode before and after the electrolysis reaction in example 1, which shows that a black solid product having a metallic luster is formed on the surface of the graphite anode after the electrolysis is completed. The SEM photograph of FIG. 3 shows that the product collected on the anode is an ultra-thin nanosheet structure, with a lamella thickness of about 10-30 nm; compared withThen, the molybdenite used as the raw material is in a sheet-like shape with a large volume. FIG. 4 is an XRD (X-ray diffraction) spectrum of the molybdenum disulfide nanosheet prepared in example 1, and as shown in the diagram, the product has very high diffraction peak intensity and is MoS-like2The standard spectrum peaks are basically consistent, which indicates that the product is mainly MoS2And the crystallization degree is higher; in addition, no diffraction peaks corresponding to other impurities appeared in the spectra, indicating higher purity of the product. As can be seen from the charge and discharge curves in fig. 5, the molybdenum disulfide nanosheet prepared in example 1 has a relatively high capacity when used as a negative electrode material of a lithium battery (when the charge and discharge current density is 200mA/g, the measured electrode capacity is about 480 to 500 mAh/g). Fig. 6 and 7 are a rate performance test and a charge-discharge cycle test of a lithium battery cathode made of the molybdenum disulfide nanosheet obtained in example 1, respectively, and the data show that the cathode has good high-current discharge performance and good cycle stability.
Example 2
(1) 700g of a NaCl-KCl (45:55 mol%) mixture was filled in a nickel container of an appropriate size, and one end of a nickel rod was connected to the nickel container while the other end extended outside the reactor and connected to the cathode of an external power supply. The nickel vessel was slowly heated to 800 ℃ using an electric furnace under the protection of argon atmosphere to melt the chloride salt, and then the temperature of the salt was adjusted to 685 ℃ within 40 min.
(2) Mechanically crushing molybdenite ore with the molybdenum content of about 41.57%, and screening to obtain molybdenite particles with the particle size of 5-20 mm; selecting a tabular stainless steel-based molybdenum disulfide coating anode (the size is 5 multiplied by 5 cm)2) The screened molybdenite particles were put into a nickel container, and constant-pressure electrolysis was performed under an argon atmosphere (cell pressure: 2.6V), the electrolysis time is 5.0 h.
(3) And after the electrolysis is finished, collecting the anode deposition product, washing and drying the product by using deionized water to obtain molybdenum disulfide nanosheet powder with the purity of about 99.6% (the mass fraction of Mo is 59.69%).
Example 3
(1) 800g of NaCl is filled into a nickel container with a proper size, one end of a nickel-chromium alloy rod is connected with the nickel container, and the other end of the nickel-chromium alloy rod extends out of the reactor and is connected with a cathode of an external power supply. The nickel container was slowly heated to 850 ℃ in an electric furnace under the protection of argon gas atmosphere to melt NaCl.
(2) Mechanically crushing molybdenite ore with the molybdenum content of about 35%, and screening to obtain molybdenite particles with the particle size of below 10 mm; selecting a cylindrical graphite anode, putting the screened molybdenite particles into a nickel container, and carrying out constant current electrolysis (the current density is 1500mA/1g molybdenite) under the argon atmosphere.
(3) And after the electrolysis is finished, collecting the anode deposition product, washing and drying the product to obtain molybdenum disulfide nanosheet powder with the purity of about 99.2% (the mass fraction of Mo is 59.48%).
Example 4
(1) 1000g of KCl is filled into a nickel container with proper size, one end of a molybdenum rod is connected with the nickel container, and the other end extends out of the reactor and is connected with a cathode of an external power supply. The nickel container is slowly heated to 800 ℃ by using an electric furnace under the protection of argon atmosphere, so that KCl is melted.
(2) Mechanically crushing molybdenite ore with the molybdenum content of about 20%, and screening to obtain molybdenite particles with the particle size of 2-20 mm; selecting carbon cloth anode (size 7X 4 cm)2) The screened molybdenite particles were put into a nickel container and subjected to constant current electrolysis (current density 2000mA/1g molybdenite) in an argon atmosphere.
(3) And after the electrolysis is finished, collecting the anode deposition product, washing and drying the product, and finally obtaining molybdenum disulfide nanosheet powder with the purity of about 99.2% (the mass fraction of Mo is 59.44%).
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any modification, equivalent replacement, and improvement made by those skilled in the art within the technical scope of the present invention should be included in the scope of the present invention.
Claims (10)
1. An electrochemical method for preparing high-purity molybdenum disulfide nanosheets from molybdenite is characterized in that the reaction is carried out in an inert gas atmosphere in the whole process, and comprises the following preparation steps:
(1) putting alkali metal chloride in a nickel reaction vessel, melting at high temperature, and then cooling to the reaction temperature;
(2) adding molybdenite into a nickel container, immersing the nickel container in molten salt, taking the nickel container as a cathode, and installing an anode for electrolysis;
(3) and after the electrolysis is finished, taking out the anode, cooling to room temperature, collecting the deposit on the surface of the anode, and washing and drying to obtain the high-purity molybdenum disulfide powder.
2. The method of claim 1, wherein: in the step (1), the alkali metal chloride is selected from any one or mixture of two of KCl and NaCl, and the purity is industrial purity or more.
3. The method of claim 1, wherein: the reaction temperature in the step (1) is 670-.
4. The method of claim 1, wherein: in the step (2), the molybdenum grade of the molybdenite ore is 10-51 wt%, and the oxygen content in the ore is more than 3 wt%.
5. The method of claim 1, wherein: in the step (2), the particle size of the molybdenite ore is less than 20 mm.
6. The method of claim 1, wherein: the anode in the step (2) is selected from any one of a graphite anode, a molybdenum disulfide coating anode, a carbon cloth anode and a biochar anode, and the electrode form comprises a plate shape, an arc shape, a column shape and a cylinder shape.
7. The method of claim 1, wherein: the electrolysis mode in the step (2) is constant-voltage or constant-current electrolysis.
8. The method of claim 7, wherein: in the step (2), when constant-voltage electrolysis is adopted, the pressure of the electrolytic cell is 2.1-3.5V; when constant current electrolysis is adopted, the required cathode current density is 0.1-5000mA/1g molybdenite.
9. The method of claim 1, wherein: and (3) soaking the anode sediment in deionized water, and then sequentially carrying out ultrasonic cleaning by using ethanol and deionized water/ultrapure water.
10. The application of the molybdenum disulfide nanosheet prepared by the method of any one of claims 1 to 9 as a lithium ion battery cathode material in the field of electrochemical energy storage device preparation.
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