Transition metal sulfide intercalated graphite and its preparation method and application

Abstract

This invention discloses a transition metal sulfide intercalated graphite, its preparation method, and its applications, belonging to the field of materials science and technology. Utilizing the characteristics of a two-chamber system, a synthesis strategy based on temperature and time differences is adopted. Pretreated transition metal chlorides are uniformly mixed with flake graphite and then subjected to heat treatment. By introducing low-melting-point nitrates, the mechanical energy from ball milling is converted into internal energy, allowing the reaction system to reach the eutectic temperature and initially activating the flake graphite, significantly shortening the reaction time. Simultaneously, sublimed sulfur is used as a sulfur source for sulfidation treatment, synthesizing transition metal sulfide intercalated graphite in one step. Unlike traditional methods that first synthesize transition metal chloride intercalated graphite and then perform secondary processing to obtain transition metal sulfide intercalated graphite, the transition metal sulfide intercalated graphite obtained by this invention has advantages such as low cost, simple process, convenient preparation, high reproducibility, no impurity phases in the product, and high sulfidation rate, making it directly applicable to the field of electromagnetic wave absorption.

Description

Technical Field

[0001] This invention belongs to the field of materials science and technology, specifically relating to a transition metal sulfide intercalated graphite, its preparation method, and its application. Background Technology

[0002] Transition metals and sulfides often coexist in the materials science field, combining to form transition metal sulfides. Transition metal sulfides are low-cost materials with easily tunable structures, making them promising for applications in electrocatalysis and electromagnetic pollution control. However, their susceptibility to surface oxidation in the environment significantly diminishes their practical value. Flake graphite, on the other hand, possesses a unique two-dimensional layered structure. Carbon atoms in the same plane along the a-axis are connected by covalent bonds, giving flake graphite high-temperature resistance and corrosion resistance. The presence of π-π conjugated bonds also contributes to its excellent electrical conductivity. Furthermore, the carbon atom layers along the c-axis are connected by weak van der Waals forces. Since van der Waals forces are far less stable and robust than covalent bonds, this facilitates the insertion of atoms, ions, and ionic groups between the graphite layers. Inserting transition metal sulfides into the interlayer of graphite to form intercalated graphite not only improves the surface oxidation of transition metal sulfides in the environment, but also results in products with better physicochemical properties due to the introduction of transition metal sulfides.

[0003] Currently, most methods for synthesizing transition metal sulfide intercalated graphite are based on first synthesizing transition metal chlorides, and then using hydrothermal reaction or high-temperature secondary treatment for sulfidation to synthesize transition metal sulfide intercalated graphite. The cumbersome process and increased cost undoubtedly restrict the production and application of transition metal sulfide intercalated graphite.

[0004] To address the technical problems of cumbersome processes and high costs in existing methods for synthesizing transition metal sulfide intercalated graphite, there is an urgent need to find an efficient, low-cost, and simple method for synthesizing transition metal sulfide intercalated graphite. Summary of the Invention

[0005] In order to overcome the shortcomings of the prior art, the present invention aims to provide a transition metal sulfide intercalated graphite, its preparation method and application, so as to solve the technical problems of complex process, high cost and long reaction time in the prior art.

[0006] To achieve the above objectives, the present invention employs the following technical solution:

[0007] This invention discloses a method for preparing transition metal sulfide intercalated graphite, comprising the following steps:

[0008] 1) After mixing and grinding transition metal chlorides with flake graphite, the mixture is dissolved in anhydrous ethanol, ball-milled, vacuum dried, and then a mixture of nitrates is added. After dry milling, a mixed powder is obtained.

[0009] 2) Under an inert atmosphere, the mixed powder obtained in step 1) is placed at the outlet of the dual-chamber device, heated rapidly and then kept at that temperature; the sublimed sulfur powder is placed at the inlet of the dual-chamber device, heated slowly and then kept at that temperature; after the reaction is completed, a mixture is obtained at the outlet of the dual-chamber device, and the mixture is washed with water, alcohol, filtered and dried to obtain transition metal sulfide intercalated graphite.

[0010] Preferably, in step 1), the molar ratio of transition metal chloride to flake graphite is (1-10):1, the flake graphite is high-purity flake graphite with a purity greater than 99.00%, and the transition metal chloride is copper chloride, ferric chloride, molybdenum chloride, or cobalt chloride.

[0011] Preferably, in step 1), the nitrate mixture is obtained by mixing two or three of sodium nitrate, potassium nitrate and copper nitrate; the molar ratio of sodium nitrate to potassium nitrate is 4:6; the molar ratio of sodium nitrate to copper nitrate is 4:1; the molar ratio of potassium nitrate to copper nitrate is 6:1; and the molar ratio of sodium nitrate to potassium nitrate to copper nitrate is 4:6:1.

[0012] Preferably, in step 1), the mass ratio of nitrate mixture to flake graphite is (1-3):1; and the dry grinding time is 3.5-8.5 h.

[0013] Preferably, the molar ratio of transition metal chloride to sublimed sulfur is (1-3):1.

[0014] Preferably, in step 2), the rapid heating rate is 9–21 °C / min; the holding temperature is 14–146 °C higher than the melting point of transition metal chlorides; and the holding time is 12.5–70.5 h.

[0015] Preferably, in step 2), the slow heating rate is 0.5–1 °C / min; the holding temperature is 171–210 °C; and the holding time is 2–6 h.

[0016] Preferably, the equipment used for ball milling and dry milling is a planetary ball mill; the number of water washing and alcohol washing cycles is 3-6.

[0017] The present invention also discloses the transition metal sulfide intercalated graphite prepared by the above preparation method.

[0018] The present invention also discloses the application of the above-mentioned transition metal sulfide intercalated graphite in the preparation of electromagnetic wave absorbing materials.

[0019] Compared with the prior art, the present invention has the following beneficial effects:

[0020] This invention discloses a method for preparing transition metal sulfide intercalated graphite. The method involves mixing and grinding transition metal chlorides with flake graphite, dissolving the mixture in anhydrous ethanol, ball milling, and vacuum drying to allow the transition metal chlorides to dissolve and precipitate, resulting in uniform particle size and increased contact with the flake graphite. A nitrate mixture is then added, and the mixture is dry-milled to obtain a mixed powder. By introducing the low-melting-point nitrate mixture, the mechanical energy from ball milling and the friction between particles generate heat, raising the material's temperature to the eutectic temperature during the ball milling process. This activates the flake graphite in the molten salt, further facilitating the subsequent intercalation of the transition metal sulfide. The low melting point of the nitrate mixture ensures the reactants are molten during ball milling, activating the flake graphite and weakening the van der Waals forces between the graphite layers, effectively shortening the time required for subsequent reactions. This invention employs a dual-room temperature difference method, utilizing temperature and time differences to synthesize transition metal sulfide intercalated graphite in a single step. Unlike other methods that first synthesize transition metal chloride intercalated graphite followed by secondary reactions / treatments, this invention features a simpler process, achieving one-step synthesis using a dual-chamber apparatus. By introducing low-melting-point nitrates and converting the mechanical energy from ball milling into internal energy, the reaction system reaches the eutectic temperature, initially activating the flake graphite and significantly shortening subsequent reaction time. Compared to traditional synthesis processes, this method eliminates relatively complex secondary treatments, greatly improves the synthesis success rate, and achieves extremely high sulfidation rates. Furthermore, it avoids the use of environmentally harmful solvents such as acids and alkalis during the reaction.

[0021] The present invention also discloses the transition metal sulfide intercalated graphite prepared by the above preparation method; the prepared transition metal sulfide intercalated graphite has the advantages of high purity, controllable and adjustable transition metal sulfide intercalation amount; and has excellent electromagnetic wave absorption performance.

[0022] This invention also discloses the application of the above-mentioned transition metal sulfide intercalated graphite in the preparation of electromagnetic wave absorbing materials. In actual production, the requirements for manual operation are relatively low, which improves production safety. At the same time, this process has low energy consumption, low production cost, and relatively low environmental protection investment cost. The process is simple, the preparation process is convenient and highly repeatable, and the product is free of impurities, which can significantly improve economic benefits. Attached Figure Description

[0023] Figure 1 This is a SEM image of the transition metal sulfide intercalated graphite obtained in Example 2 of the present invention. Detailed Implementation

[0024] To enable those skilled in the art to better understand the present invention, the technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings of the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort should fall within the scope of protection of the present invention.

[0025] It should be noted that the terms "first," "second," etc., in the specification, claims, and accompanying drawings of this invention are used to distinguish similar objects and are not necessarily used to describe a specific order or sequence. It should be understood that such data can be interchanged where appropriate so that the embodiments of the invention described herein can be implemented in orders other than those illustrated or described herein. Furthermore, the terms "comprising" and "having," and any variations thereof, are intended to cover a non-exclusive inclusion; for example, a process, method, system, product, or apparatus that comprises a series of steps or units is not necessarily limited to those steps or units explicitly listed, but may include other steps or units not explicitly listed or inherent to such processes, methods, products, or apparatus.

[0026] The present invention will now be described in further detail with reference to the accompanying drawings:

[0027] This invention provides a method for preparing transition metal sulfide intercalated graphite, employing a dual room temperature difference method to synthesize transition metal sulfide intercalated graphite in a one-step process utilizing temperature and time differences. By introducing low-melting-point nitrates, the mechanical energy from a planetary ball mill is converted into internal energy, allowing the reaction system to reach the eutectic temperature and initially activating the flake graphite, significantly shortening the subsequent reaction time. It is important to note that the ratio of the mixed nitrates and the ratio of the mixed nitrates to the flake graphite must strictly adhere to the patent requirements. The resulting transition metal sulfide intercalated graphite has advantages such as low cost, simple process, convenient and highly reproducible preparation, and the absence of impurity phases in the product.

[0028] This invention discloses a method for preparing transition metal sulfide intercalated graphite, comprising the following steps:

[0029] 1) Dry the transition metal chloride powder under vacuum at 80°C until it is ready for use;

[0030] 2) The dried transition metal chloride and high-purity flake graphite were mixed and ground into powder 1 at a molar ratio of 1:(1-10); using anhydrous ethanol as a solvent, powder 1 was placed in anhydrous ethanol to obtain mixed solution 1. After thorough mixing, the mixture was ball-milled for 2.5 hours using a planetary ball mill; after ball milling, mixed solution 1 was vacuum-dried for 1.5 hours to obtain powder 2; the purity of the high-purity flake graphite was above 99.00%; the transition metal chloride was copper chloride, ferric chloride, molybdenum chloride, or cobalt chloride.

[0031] 3) Add the nitrate mixture to powder 2 and dry grind it using a planetary ball mill for 3.5 to 8.5 hours. After dry grinding, powder 3 is obtained. The nitrate mixture is obtained by mixing two or three of sodium nitrate, potassium nitrate, and copper nitrate. The molar ratio between each nitrate follows the order described above: 4:6:1. That is, the molar ratio of sodium nitrate to potassium nitrate is 4:6; the molar ratio of sodium nitrate to copper nitrate is 4:1; the molar ratio of potassium nitrate to copper nitrate is 6:1; the molar ratio of sodium nitrate to potassium nitrate to copper nitrate is 4:6:1; and the mass ratio of nitrate mixture to flake graphite is (1 to 3):1.

[0032] 4) Weigh a certain proportion of sublimed sulfur with transition metal chloride and grind it to obtain powder 4. Place powder 4 in a non-sealed alumina ceramic boat for later use; the molar ratio of transition metal chloride to sublimed sulfur is (1~3):1.

[0033] 5) Place powder 3 at one end of the double-chamber device near the outlet, rapidly heat to a certain temperature, and then hold at that temperature; place powder 4 at one end of the double-chamber device near the inlet, slowly heat to a certain temperature, and then hold at that temperature; the reaction is carried out under an inert atmosphere; the rapid heating rate is 9–21 °C / min; the holding temperature is 14–146 °C higher than the melting point of transition metal chlorides; the holding time is 12.5–70.5 h; the slow heating rate is 0.5–1 °C / min; the holding temperature is 171–210 °C; the holding time is 2–6 h.

[0034] 6) After the reaction is complete, take out the powder 3 to obtain mixture 1. After washing the mixture 1 with water and alcohol several times, filtering and drying, the transition metal sulfide intercalated graphite is obtained; the number of water washing and alcohol washing is 3 to 6 times.

[0035] During the process, attention must be paid to the timing of heating the inlet chamber containing sublimed sulfur, and the gas flow rate of the inert gas must be controlled. The gas flow rate should be significantly reduced when the inlet chamber containing sublimed sulfur enters the heat preservation stage. The ratio of various nitrates must be strictly implemented according to the requirements of this invention. The alumina ceramic boat containing sublimed sulfur must be in a non-sealed state. Furthermore, for transition metal sulfide intercalated graphite with different precursor transition metal chlorides, the order of water washing and alcohol washing must be carefully considered. The prepared transition metal sulfide intercalated graphite can be applied to electromagnetic wave absorbing materials.

[0036] This invention discloses a method for preparing transition metal sulfide intercalated graphite, applicable to the synthesis of most transition metal sulfide intercalated graphites. Compared with traditional synthesis processes, the method disclosed in this invention eliminates relatively complex secondary processing, significantly improves the synthesis success rate, and achieves extremely high sulfidation rates. Furthermore, it avoids the use of environmentally harmful solvents such as acids and alkalis during the reaction process. In actual production, the requirements for manual operation are relatively low, improving production safety. Simultaneously, this process has low energy consumption, low production costs, and relatively low environmental protection investment costs, significantly improving economic benefits.

[0037] Example 1

[0038] A method for preparing transition metal sulfide intercalated graphite includes the following steps:

[0039] 1) Dry anhydrous ferric chloride in a vacuum drying oven at 80℃ until it is ready for use;

[0040] 2) Grind and mix 1.892g of high-purity flake graphite with 6.48g of dried anhydrous ferric chloride to form powder 1. Measure 50mL of anhydrous ethanol and mix it with powder 1 to form mixed solution 1. Ball mill mixed solution 1 for 2.5h and vacuum dry it at 80℃ for 1.5h to obtain powder 2. The purity of high-purity flake graphite is 99.90%.

[0041] 3) Take 0.680g of sodium nitrate and 1.212g of potassium nitrate and mix them evenly with powder 2. After ball milling for 8 hours, powder 3 is obtained.

[0042] 4) Weigh 6.4g of sublimed sulfur, put it into an unsealed alumina ceramic boat, and place it in the air inlet chamber for later use;

[0043] 5) Take out powder 3 and place it in the gas outlet chamber. Rapidly heat it to 350°C at 21°C / min, which is 44°C higher than the melting point of ferric chloride. After holding it at this temperature for 12.5 hours, start heating the gas inlet chamber to 200°C at 1°C / min. Hold it at this temperature for 3 hours and then stop the reaction together with the gas outlet chamber.

[0044] 6) Take out the powder 3 after the reaction is completed to obtain mixture 1. Wash mixture 1 with deionized water 3 times and ethanol 3 times. After filtration and drying, iron sulfide intercalated graphite is obtained.

[0045] Example 2

[0046] A method for preparing transition metal sulfide intercalated graphite includes the following steps:

[0047] 1) Dry anhydrous copper chloride in a vacuum drying oven at 80℃ until it is ready for use;

[0048] 2) Grind and mix 6.804g of high-purity flake graphite with 7.623g of dried anhydrous copper chloride to form powder 1. Measure 50mL of anhydrous ethanol and mix it with powder 1 to form mixed solution 1. Ball mill mixed solution 1 for 2.5h and vacuum dry it at 80℃ for 1.5h to obtain powder 2. The purity of high-purity flake graphite is 99.90%.

[0049] 3) Take 0.680g sodium nitrate, 1.212g potassium nitrate, and 0.376g copper nitrate and mix them evenly with powder 2. After ball milling for 8.5h, powder 3 is obtained.

[0050] 4) Weigh 0.609g of sublimed sulfur, put it into an unsealed alumina ceramic boat, and place it in the air inlet chamber for later use;

[0051] 5) Take out powder 3 and place it in the gas outlet chamber. Rapidly heat it to 634°C at 9°C / min, which is 14°C higher than the melting point of anhydrous copper chloride. After holding it at this temperature for 70.5 hours, start heating the gas inlet chamber to 210°C at 0.5°C / min. Hold it at this temperature for 2 hours and then stop the reaction together with the gas outlet chamber.

[0052] 6) Take out the powder 3 after the reaction is completed to obtain mixture 1. Wash mixture 1 with ethanol 6 times and deionized water 3 times. After filtration and drying, copper sulfide intercalated graphite is obtained.

[0053] See Figure 1 This is a SEM image of the transition metal sulfide intercalated graphite obtained in Example 2 of the present invention; as can be seen from the image, the interlayer size of the flake graphite increased, proving the successful insertion of copper sulfide.

[0054] Example 3

[0055] A method for preparing transition metal sulfide intercalated graphite includes the following steps:

[0056] 1) Dry anhydrous molybdenum chloride in a vacuum drying oven at 80℃ until it is ready for use;

[0057] 2) Grind and mix 4.8g of high-purity flake graphite with 10.93g of dried anhydrous molybdenum chloride to form powder 1. Measure 100mL of anhydrous ethanol and mix it with powder 1 to form mixed solution 1. Ball mill mixed solution 1 for 2.5h and vacuum dry it at 80℃ for 1.5h to obtain powder 2. The purity of the high-purity flake graphite is 99.90%.

[0058] 3) Take 1.360g of sodium nitrate and 2.424g of potassium nitrate and mix them evenly with powder 2. After ball milling for 3.5h, powder 3 is obtained.

[0059] 4) Weigh 6.4g of sublimed sulfur, put it into an unsealed alumina ceramic boat, and place it in the air inlet chamber for later use;

[0060] 5) Take out powder 3 and place it in the gas outlet chamber. Rapidly heat it to 340°C at 10°C / min, which is higher than the melting point of anhydrous molybdenum chloride 146°C. After holding it at this temperature for 12.5 hours, start heating the gas inlet chamber to 171°C at 1°C / min. Hold it at this temperature for 3 hours and then stop the reaction together with the gas outlet chamber.

[0061] 6) After the reaction is complete, take out the powder 3 to obtain mixture 1. Wash mixture 1 with deionized water 3 times and ethanol 3 times. After filtration and drying, molybdenum sulfide intercalated graphite is obtained.

[0062] Example 4

[0063] A method for preparing transition metal sulfide intercalated graphite includes the following steps:

[0064] 1) Dry anhydrous molybdenum chloride in a vacuum drying oven at 80℃ until it is ready for use;

[0065] 2) Grind and mix 4.8g of high-purity flake graphite with 10.93g of dried anhydrous molybdenum chloride to form powder 1. Measure 100mL of anhydrous ethanol and mix it with powder 1 to form mixed solution 1. Ball mill mixed solution 1 for 2.5h and vacuum dry it at 80℃ for 1.5h to obtain powder 2. The purity of the high-purity flake graphite is 99.90%.

[0066] 3) Take 1.360g of sodium nitrate and 2.424g of potassium nitrate and mix them evenly with powder 2. After ball milling for 8.5h, powder 3 is obtained.

[0067] 4) Weigh 6.4g of sublimed sulfur, put it into an unsealed alumina ceramic boat, and place it in the air inlet chamber for later use;

[0068] 5) Take out powder 3 and place it in the gas outlet chamber. Rapidly heat it to 280°C at 10°C / min, which is higher than the melting point of anhydrous molybdenum chloride 86°C. After holding it at this temperature for 12 hours, start heating the gas inlet chamber to 171°C at 0.8°C / min. Hold it at this temperature for 6 hours and then stop the reaction together with the gas outlet chamber.

[0069] 6) After the reaction is complete, take out the powder 3 to obtain mixture 1. Wash mixture 1 with deionized water 5 times and ethanol 5 times. After filtration and drying, molybdenum sulfide intercalated graphite is obtained.

[0070] Example 5

[0071] A method for preparing transition metal sulfide intercalated graphite includes the following steps:

[0072] 1) Dry anhydrous molybdenum chloride in a vacuum drying oven at 80℃ until it is ready for use;

[0073] 2) Grind and mix 4.8g of high-purity flake graphite with 10.93g of dried anhydrous molybdenum chloride to form powder 1. Measure 100mL of anhydrous ethanol and mix it with powder 1 to form mixed solution 1. Ball mill mixed solution 1 for 2.5h and vacuum dry it at 80℃ for 1.5h to obtain powder 2. The purity of the high-purity flake graphite is 99.90%.

[0074] 3) Take 1.360g of sodium nitrate and 2.424g of potassium nitrate, mix them evenly with powder 2, and ball mill for 8 hours to obtain powder 3:

[0075] 4) Weigh 6.4g of sublimed sulfur, put it into an unsealed alumina ceramic boat, and place it in the air inlet chamber for later use;

[0076] 5) Take out powder 3 and place it in the gas outlet chamber. Rapidly heat it to 280°C at 10°C / min, which is higher than the melting point of anhydrous molybdenum chloride, 86°C. After holding it at this temperature for 12 hours, start heating the gas inlet chamber to 171°C at 1°C / min. Hold it at this temperature for 3 hours and then stop the reaction together with the gas outlet chamber.

[0077] 6) After the reaction is complete, take out the powder 3 to obtain mixture 1. Wash mixture 1 with deionized water 3 times and ethanol 3 times. After filtration and drying, molybdenum sulfide intercalated graphite is obtained.

[0078] Example 6

[0079] A method for preparing transition metal sulfide intercalated graphite includes the following steps:

[0080] 1) Dry anhydrous cobalt chloride in a vacuum drying oven at 80℃ until it is ready for use;

[0081] 2) Grind and mix 2.4g of high-purity flake graphite with 2.598g of dried anhydrous cobalt chloride to form powder 1. Measure 50mL of anhydrous ethanol and mix it with powder 1 to form mixed solution 1. Ball mill mixed solution 1 for 2.5h and vacuum dry it at 80℃ for 1.5h to obtain powder 2. The purity of high-purity flake graphite is 99.90%.

[0082] 3) Take 0.68g of sodium nitrate and 1.212g of potassium nitrate and mix them evenly with powder 2. After ball milling for 8.5h, powder 3 is obtained.

[0083] 4) Weigh 6.4g of sublimed sulfur, put it into an unsealed alumina ceramic boat, and place it in the air inlet chamber for later use;

[0084] 5) Take out powder 3 and place it in the gas outlet chamber. Rapidly heat it to 738°C at 21°C / min, which is 14°C higher than the melting point of anhydrous ferric chloride. After holding it at this temperature for 12.5 hours, start heating the gas inlet chamber to 210°C at 1°C / min. Hold it at this temperature for 3 hours and then stop the reaction together with the gas outlet chamber.

[0085] 6) Take out the powder 3 after the reaction is completed to obtain mixture 1. Wash mixture 1 with deionized water 4 times and ethanol 4 times. After filtration and drying, iron sulfide intercalated graphite is obtained.

[0086] This invention utilizes principles such as energy conversion and dual-temperature temperature difference to transform the mechanical energy provided by friction generated during planetary ball milling into heat energy. Simultaneously, by controlling the composition of the nitrate eutectic salt and utilizing low-melting-point nitrates, the eutectic temperature is lowered, achieving a molten state during ball milling. The frictional movement of reactants within the molten salt significantly shortens the reaction time of subsequent reactions. This provides a highly efficient, low-cost, and simple method for preparing transition metal sulfide intercalated graphite, applicable to the synthesis of most transition metal sulfide intercalated graphites. In particular, the method utilizes transition metal chlorides such as copper chloride, ferric chloride, molybdenum chloride, and cobalt chloride with flake graphite as precursors to prepare transition metal sulfide intercalated graphite, resulting in products applicable to the field of electromagnetic wave absorption.

[0087] The above content is only for illustrating the technical concept of the present invention and should not be construed as limiting the scope of protection of the present invention. Any modifications made to the technical solution based on the technical concept proposed in this invention shall fall within the scope of protection of the claims of this invention.

Claims

1. A method for preparing transition metal sulfide intercalated graphite, characterized in that, Includes the following steps: 1) A mixture of transition metal chloride and flake graphite is ground and dissolved in anhydrous ethanol. After ball milling and vacuum drying, a nitrate mixture is added and dry-milled to obtain a mixed powder. The nitrate mixture is obtained by mixing two or three of sodium nitrate, potassium nitrate, and copper nitrate. The mass ratio of the nitrate mixture to flake graphite is (1~3):

1. The dry-milling time is 3.5~8.5h. 2) Under an inert atmosphere, the mixed powder obtained in step 1) is placed at the outlet of the dual-chamber device, rapidly heated, and then held at that temperature. After the holding period, the sublimated sulfur powder is placed at the inlet of the dual-chamber device, slowly heated, and then held at that temperature. After the reaction is complete, a mixture is obtained at the outlet of the dual-chamber device. The mixture is washed with water, alcohol, filtered, and dried to obtain transition metal sulfide intercalated graphite. The rapid heating rate is 9~21℃ / min; the holding temperature is 14~146℃ higher than the melting point of the transition metal chloride; the holding time is 12.5~70.5h; the slow heating rate is 0.5~1℃ / min; the holding temperature is 171~210℃; and the holding time is 2-6h.

2. The method for preparing transition metal sulfide intercalated graphite according to claim 1, characterized in that, In step 1), the molar ratio of transition metal chloride to flake graphite is (1~10):1, the flake graphite is high-purity flake graphite with a purity greater than 99.00%, and the transition metal chloride is copper chloride, ferric chloride, molybdenum chloride or cobalt chloride.

3. The method for preparing transition metal sulfide intercalated graphite according to claim 1, characterized in that, In step 1), when the nitrate mixture is obtained by mixing sodium nitrate and potassium nitrate, the molar ratio of sodium nitrate to potassium nitrate is 4:6; when the nitrate mixture is obtained by mixing sodium nitrate and copper nitrate, the molar ratio of sodium nitrate to copper nitrate is 4:1; when the nitrate mixture is obtained by mixing potassium nitrate and copper nitrate, the molar ratio of potassium nitrate to copper nitrate is 6:1; and when the nitrate mixture is obtained by mixing sodium nitrate, potassium nitrate, and copper nitrate, the molar ratio of sodium nitrate to potassium nitrate to copper nitrate is 4:6:

1.

4. The method for preparing transition metal sulfide intercalated graphite according to claim 1, characterized in that, The molar ratio of the transition metal chloride to sublimed sulfur is (1~3):

1.

5. The method for preparing transition metal sulfide intercalated graphite according to claim 1, characterized in that, The ball milling and dry milling are performed using a planetary ball mill; the water washing and alcohol washing are performed 3-6 times.

6. The transition metal sulfide intercalated graphite prepared by the preparation method according to any one of claims 1 to 5.

7. The application of the transition metal sulfide intercalated graphite according to claim 6 in the preparation of electromagnetic wave absorbing materials.

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