A two-dimensional porous oxide and a method for preparing the same

Two-dimensional porous oxides were prepared by reacting with lithium initiators using a molten salt method, which solved the problems of complex preparation processes and uneven pore size in existing technologies. This method enables the efficient and low-cost production of porous oxides, which are suitable for catalysis, adsorption and energy storage.

CN116812873BActive Publication Date: 2026-02-24HUAZHONG UNIV OF SCI & TECH
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Patent Information

Application Number
CN202310741186.5
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-06-21
Publication Date
2026-02-24
Estimated Expiration
2043-06-21

AI Technical Summary

Technical Problem

Existing methods for preparing two-dimensional porous oxides suffer from problems such as complex processes, small specific surface area of ​​the products, and uneven pore size distribution.

Method used

Ion-intercalated two-dimensional oxides were prepared by molten salt method and formed a uniform porous structure by reacting with a lithium initiator. The specific steps included mixing metal salt and molten salt, heating, cooling, washing and then mixing with lithium initiator, controlling the reaction conditions and time, and using liquid alkanes as dispersants.

Benefits of technology

Two-dimensional porous oxides with large specific surface area and uniform pore size distribution are prepared. The process is simple, low-cost, and widely adaptable, and can be applied to catalysis, adsorption, energy storage and other fields.

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Abstract

A method for preparing a two-dimensional porous oxide belongs to the technical field of porous oxide preparation. The method includes the following steps: (1) using a metal salt as a precursor, an ion-intercalated two-dimensional oxide is prepared by a molten salt method; (2) the ion-intercalated two-dimensional oxide is mixed with a lithium initiator, reacted for a predetermined time, and then the unreacted lithium initiator is removed, filtered, and washed to obtain the two-dimensional porous oxide. The two-dimensional porous oxide prepared by this method forms uniform pores with a pore size range of 2-10 nm and a specific surface area of ​​200-300 m². 2 / g.
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Description

Technical Field

[0001] This invention belongs to the technical field of preparing porous oxides, and more specifically, relates to a two-dimensional porous oxide and its preparation method. Background Technology

[0002] Two-dimensional materials are atomic sheets that expose more atoms and thus possess unique electronic, optical, and mechanical properties, with enormous potential for technological applications and a wealth of unexplored fundamental science.

[0003] Porous materials possess unique pore structures and large specific surface areas, giving them significant advantages and potential in fields such as adsorption, separation, catalysis, biology, environmental protection, and energy. The pore size can be controlled within a suitable range depending on the composition and processing method. The large specific surface area, good permeability, and resistance to high temperatures and corrosion give porous materials superior properties that are difficult for other materials to replace.

[0004] Different preparation methods can yield porous metal oxides with varying morphologies and pore structures. These oxides, exhibiting excellent chemical and thermal stability, are used in catalysis, adsorption, and energy storage, making the study of their preparation methods of great significance. Common methods for preparing two-dimensional porous oxides include template methods, sol-gel methods, solvothermal methods, freeze-drying methods, chemical vapor deposition, and co-precipitation methods. However, these methods suffer from problems such as complex preparation processes, small specific surface areas of the products, and uneven pore size distribution. Summary of the Invention

[0005] To address the aforementioned deficiencies or improvement needs of existing technologies, the present invention aims to provide a method for preparing two-dimensional porous oxides. This method involves preparing ion-intercalated two-dimensional oxides via a molten salt method, followed by lithiation of the ion-intercalated two-dimensional oxides to create pores, thereby preparing a novel two-dimensional porous oxide. Compared with existing two-dimensional porous oxides, the novel two-dimensional porous oxide prepared by this method has advantages such as a large specific surface area and uniform pore size distribution. Moreover, the preparation method is simple and has low production costs.

[0006] In a first aspect of the present invention, a method for preparing a two-dimensional porous oxide is provided, the method comprising the following steps:

[0007] (1) Using metal salts as precursors, ion-intercalated two-dimensional oxides were prepared by the molten salt method;

[0008] (2) The ion-intercalated two-dimensional oxide is mixed with a lithium initiator, and after a predetermined reaction time, the unreacted lithium initiator is removed, filtered and washed to obtain a two-dimensional porous oxide.

[0009] As a preferred embodiment of the present invention, the lithium initiator includes n-butyllithium, isopropyl lithium, n-pentyllithium, and n-hexyllithium, with n-butyllithium being the most preferred.

[0010] As a preferred embodiment of the present invention, the ratio of the ion-intercalated two-dimensional oxide to the lithium initiator is 10-50 mg / mL, preferably 20-30 mg / mL.

[0011] As a preferred embodiment of the present invention, in step (3), the reaction conditions are an inert atmosphere and the reaction time is 16-24h, preferably 18-20h.

[0012] As a preferred embodiment of the present invention, the method further includes: before mixing the ion-intercalated two-dimensional oxide with the lithium initiator, using liquid alkane as a dispersant to uniformly disperse the ion-intercalated two-dimensional oxide in the dispersant; wherein the ratio of the ion-intercalated two-dimensional oxide to the liquid alkane is 5-25 mg / mL.

[0013] As a preferred embodiment of the present invention, the specific steps of step (1) are as follows: the metal salt precursor is mixed with molten salt and heated, quenched and cooled, and washed to obtain an ion-intercalated two-dimensional oxide; wherein the mass ratio of the molten salt to the metal salt precursor is 10-25:1; and the reaction time is 30-300s.

[0014] As a preferred embodiment of the present invention, in step (1), the molten salt is a salt with a melting point not higher than 400°C, preferably a nitrate, sulfate, chloride, or phosphate.

[0015] As a preferred embodiment of the present invention, the metal salt precursor in step (1) is selected from nitrates, sulfates, chlorides, carbonates, acetates, phosphates, hydrogen phosphates, vanadates, niobates, molybdates, titanates, and tungstates.

[0016] As a preferred embodiment of the present invention, the metal element of the metal salt precursor is selected from Al, Ca, Ti, V, Cr, Mn, Fe, Co, Ni, Nb, Mo, Ru, Rh, In, Sn, Cs, and W.

[0017] In a second aspect of the invention, a two-dimensional porous oxide obtained using the method of the first aspect of the invention has a surface with uniform pores having a pore size range of 2-10 nm and a specific surface area of ​​200-300 m². 2 / g.

[0018] In summary, compared with the prior art, the above-described technical solutions conceived by this invention mainly possess the following technical advantages:

[0019] This invention makes targeted research and improvements on the preparation process and pore-forming mechanism, resulting in a simple and low-cost preparation process. The method prepares ion-intercalated two-dimensional oxides via a molten salt method, then disperses and lithiates the ion-intercalated two-dimensional oxides to prepare novel two-dimensional porous oxides. Due to the reaction between the crystal water between the interlayers of the ion-intercalated two-dimensional oxide and the lithium initiator, a high concentration of lithium hydroxide is generated on the oxide surface, which etches the oxide to form a uniform porous structure.

[0020] In this invention, the lithium initiator selected includes n-butyllithium, isopropyllithium, n-pentyllithium, and n-hexyllithium. Based on the inventors' experimental research, the two-dimensional porous oxide prepared using n-butyllithium exhibits superior performance. Furthermore, by optimizing the ratio of ion-intercalated two-dimensional oxide to lithium initiator to 10-50 mg / mL, preferably 20-30 mg / mL, specifically in Example 1 of this invention, the two-dimensional porous oxide prepared in Comparative Example 7 exhibits advantages such as a larger specific surface area and more uniform pore size distribution.

[0021] In this invention, by optimizing the reaction conditions of ion-intercalated two-dimensional oxides and lithium initiators, such that the reaction conditions are inert atmosphere and the reaction time is 16-24h, preferably 18-20h, the prepared two-dimensional porous oxides have the advantages of large specific surface area and uniform pore size distribution.

[0022] In particular, liquid alkanes are used as a dispersant in this invention, which makes the ion-intercalated two-dimensional oxides more uniformly dispersed, providing a uniformly distributed space for the reaction of the ion-intercalated two-dimensional oxides with lithium, thereby preparing two-dimensional oxides with uniform pores.

[0023] In this invention, an ion-intercalated two-dimensional oxide is prepared using a molten salt method. The salt is in a molten state, and the ions have a higher diffusion coefficient, thereby enhancing reaction kinetics and the uniform mixing of reactants, resulting in an ion-intercalated two-dimensional oxide with interlayer water of crystallization. During the subsequent preparation of the porous structure, the water of crystallization between the interlayers of the ion-intercalated two-dimensional oxide reacts with lithium to generate a high concentration of lithium hydroxide on the oxide surface, etching the oxide to form a uniform porous structure.

[0024] This invention optimizes the mass ratio of molten salt to metal salt precursor, reaction temperature, and time in the molten salt method, and prepares an ion-intercalated two-dimensional oxide with interlayer water of crystallization and ultrathin characteristics, which provides favorable conditions for subsequent lithiation and pore formation.

[0025] The types of two-dimensional porous oxides obtained by this invention are controlled by metal salt precursors. By using different types of metal salt precursors, two-dimensional oxides of different types of metals can be obtained based on the molten salt method, which has a wider adaptability to the preparation of two-dimensional oxides.

[0026] In summary, the preparation method provided by this invention achieves rapid and efficient preparation of ion-intercalated two-dimensional porous oxides, and can conveniently realize the large-scale production of two-dimensional porous oxides. The two-dimensional porous oxides prepared by this method have a pore size range of 2-10 nm and a specific surface area of ​​200-300 m². 2 / g. Attached Figure Description

[0027] Figure 1 This is a schematic diagram of the preparation method of the two-dimensional porous oxide in Example 1 of the present invention;

[0028] Figure 2 These are transmission electron microscope (TEM) images, high-resolution transmission electron microscope (HR-TEM) images, and standard electron diffraction (SAED) patterns of the two-dimensional porous manganese oxide prepared in Example 1 of this invention; wherein... Figure 2 In the image, a and b are transmission electron microscope (TEM) images. Figure 2 In the image, 'c' represents a high-resolution transmission electron microscope (HR-TEM) image. Figure 2 In the diagram, d represents the selected area electron diffraction (SAED) pattern of two-dimensional porous manganese oxide.

[0029] Figure 3 This is a specific surface area (BET) test diagram of the two-dimensional porous manganese oxide prepared in Example 1 of the present invention;

[0030] Figure 4 This is a pore size distribution diagram of the two-dimensional porous manganese oxide prepared in Example 1 of the present invention;

[0031] Figure 5 This is a pore size distribution diagram of the two-dimensional porous manganese oxide prepared in Example 7 of the present invention; Figure 5 The scale bar is 2nm. Detailed Implementation

[0032] To make the objectives, technical solutions, and advantages of this invention clearer, the invention will be further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative and not intended to limit the invention. Furthermore, the technical features involved in the various embodiments of this invention described below can be combined with each other as long as they do not conflict with each other.

[0033] like Figure 1 As shown, the preparation method of the two-dimensional porous oxide involved in the embodiments of the present invention is as follows:

[0034] Preparation of ion-intercalated two-dimensional oxides:

[0035] The preparation steps for ion-intercalated two-dimensional oxides can be found in the patent text of application number 201611186961.1, as follows:

[0036] Step 1: Place the low-melting-point salt in a muffle furnace, and set the furnace temperature between the salt's melting point and its decomposition temperature or boiling point to make the salt molten; the types of molten salt include, but are not limited to: nitrates, chlorides, sulfates, and phosphates.

[0037] Step 2: Add the metal salt precursor to the molten salt for reaction; wherein the metal elements of the metal salt include, but are not limited to: Al, Ca, Ti, V, Cr, Mn, Co, Ni, Nb, Mo, Ru, Rh, In, Sn, Cs, W; and the types of metal salts include, but are not limited to: nitrates, chlorides, sulfates, phosphates, titanates, tungstates, vanadates, niobates, hydrogen phosphates, acetates, and molybdates; heat the reaction for 30-300 seconds.

[0038] Step 3: After removing the reaction product from the muffle furnace, cool it to room temperature, soak it in water to remove the salt, and then wash and filter it with deionized water.

[0039] Step 4: The cleaned sample is dried to obtain ion-intercalated two-dimensional material powder. This ion-intercalated two-dimensional material powder contains water of crystallization between its layers.

[0040] Pretreatment of ion-intercalated two-dimensional materials;

[0041] A predetermined amount of liquid alkane is added to a glass bottle containing the oxide to ensure uniform dispersion of the ion-intercalated two-dimensional oxide in hexane. Since lithium initiators are typically stored in liquid alkane in practical applications, the ion-intercalated two-dimensional material obtained above can be directly mixed with the lithium initiator. Alternatively, the ion-intercalated two-dimensional material can be directly and uniformly mixed with the lithium initiator. During the experiment, it is sufficient to ensure thorough mixing of the ion-intercalated two-dimensional oxide and the lithium initiator.

[0042] It should be noted that pretreatment of the ion-intercalated two-dimensional material can be a preferred option, or physical methods that achieve the same dispersion effect can also be used, as long as the ion-intercalated two-dimensional material and the lithium initiator are fully mixed before preparing the product of this application. In the following embodiments, the two-dimensional porous oxides are preferably prepared by dispersion treatment with liquid alkanes.

[0043] Preparation of two-dimensional porous oxides:

[0044] In a glove box, a predetermined amount of lithium initiator is added to a glass bottle containing ion-intercalated two-dimensional material. After stirring for 16-24 hours, ethanol is added to consume the unreacted lithium initiator. The reaction product is filtered, washed with water to remove the lithium hydroxide produced in the reaction, and dried to obtain a two-dimensional porous oxide.

[0045] The method for preparing two-dimensional porous oxides provided in the examples specifically includes the following steps:

[0046] The following will provide some specific embodiments, and the characteristics of the obtained two-dimensional porous oxides will be described in detail with reference to the accompanying drawings.

[0047] Example 1:

[0048] Preparation of molten salt: Heat the muffle furnace to 380℃, place a crucible containing 5g KNO3 into the muffle furnace, and keep it in air atmosphere for 10min until the KNO3 becomes molten.

[0049] Preparation of ion-intercalated two-dimensional manganese oxide: 0.2g of MnSO4 powder was quickly added to molten KNO3 and reacted for 1 min. The crucible was then quickly removed from the muffle furnace and quenched in air at room temperature. After the crucible cooled to room temperature, deionized water was added to soak it. The mixture was then filtered and washed to remove excess unreacted salt. After drying at 60℃, brown-black ion-intercalated two-dimensional manganese oxide was obtained.

[0050] Preparation of two-dimensional porous manganese oxide:

[0051] Weigh 50 mg of the obtained ion-intercalated manganese oxide and place it in a 15 mL glass sample bottle. Add 10 mL of hexane to disperse the manganese oxide evenly.

[0052] 2 mL of n-butyllithium solution was added to a glass bottle in a glove box. A magnetic stir bar was placed in the glass bottle and the mixture was stirred on a magnetic stirrer for 20 h. After standing, ethanol was added to consume the unreacted n-butyllithium. The reaction product in the glass bottle was filtered, washed with water, and dried at 60 °C to obtain two-dimensional porous manganese oxide.

[0053] TEM image of the two-dimensional porous manganese oxide prepared in Example 1, wherein, Figure 2 In the image, a and b are TEM images. Figure 2 c in the image is an HR-TEM image, which shows that the obtained manganese oxide is a two-dimensional mesoporous nanosheet with a relatively uniform distribution. Figure 2 In the diagram, d is a selected area SAED image of two-dimensional porous manganese oxide, which shows that its crystal structure maintains the original layered structure.

[0054] like Figure 3 The figure shown is a specific surface area test diagram of the two-dimensional porous manganese oxide prepared in Example 1, which shows that it has a high specific surface area.

[0055] like Figure 4 The figure shows the pore size distribution of the two-dimensional porous manganese oxide prepared in Example 1. It can be seen that it has a relatively uniform pore size distribution, and the pore size is mainly concentrated between 2-10 nm.

[0056] Example 2:

[0057] Preparation of molten salt: Heat the muffle furnace to 350℃, place a crucible containing 5g of NaNO3 into the muffle furnace, and keep it heated in air for 10 minutes until the NaNO3 becomes molten.

[0058] Preparation of ion-intercalated two-dimensional iron oxide: 0.2g Fe(NO3)3 powder was quickly added to molten NaNO3 and reacted for 1min. The crucible was then quickly removed from the muffle furnace and quenched in air at room temperature. After the crucible cooled to room temperature, deionized water was added to soak it. The crucible was then filtered and washed to remove excess unreacted salt. After drying at 60℃, brown-black ion-intercalated two-dimensional iron oxide was obtained.

[0059] Preparation of two-dimensional porous iron oxide:

[0060] Weigh 50 mg of the obtained ion-intercalated iron oxide and place it in a 15 mL glass sample bottle. Add 10 mL of hexane to disperse the iron oxide evenly.

[0061] 2 mL of n-butyllithium solution was added to a glass bottle in a glove box. A magnetic stir bar was placed in the glass bottle and the mixture was stirred on a magnetic stirrer for 20 h. After standing, ethanol was added to consume the unreacted n-butyllithium. The reaction product in the glass bottle was filtered, washed with water, and dried at 60 °C to obtain two-dimensional porous iron oxide.

[0062] The pore size and specific surface area of ​​the two-dimensional porous iron oxide prepared by this method are within the protection scope of this invention.

[0063] Example 3:

[0064] Preparation of molten salt: Heat the muffle furnace to 420℃, place a crucible containing 5g of LiNO3 into the muffle furnace, and keep it heated in air for 10 minutes until the LiNO3 becomes molten.

[0065] Preparation of ion-intercalated two-dimensional cobalt oxide: 0.2g of CoCO3 powder was quickly added to molten LiNO3 and reacted for 1 min. The crucible was then quickly removed from the muffle furnace and quenched in air at room temperature. After the crucible cooled to room temperature, deionized water was added to soak it. The mixture was then filtered and washed to remove excess unreacted salt. After drying at 60℃, brownish-black ion-intercalated two-dimensional cobalt oxide was obtained.

[0066] Preparation of two-dimensional porous cobalt oxide:

[0067] Weigh 50 mg of the obtained ion-intercalated cobalt oxide and place it in a 15 mL glass sample bottle. Add 10 mL of hexane to disperse the cobalt oxide evenly.

[0068] 2 mL of n-butyllithium solution was added to a glass bottle in a glove box. A magnetic stir bar was placed in the glass bottle and the mixture was stirred on a magnetic stirrer for 20 h. After standing, ethanol was added to consume the unreacted n-butyllithium. The reaction product in the glass bottle was filtered, washed with water, and dried at 60 °C to obtain two-dimensional porous cobalt oxide.

[0069] The pore size and specific surface area of ​​the two-dimensional porous iron oxide prepared by this method are within the protection scope of this invention.

[0070] Example 4:

[0071] Preparation of molten salt: Heat the muffle furnace to 380℃, place a crucible containing 5g KNO3 into the muffle furnace, and keep it in air atmosphere for 10min until the KNO3 becomes molten.

[0072] Ion-intercalated two-dimensional nickel oxide: 0.2g NiCl2 powder was quickly added to molten KNO3 and reacted for 1 min. The crucible was then quickly removed from the muffle furnace and quenched in air at room temperature. After the crucible cooled to room temperature, deionized water was added to soak it. The crucible was then filtered and washed to remove excess unreacted salt. After drying at 60°C, brown-black ion-intercalated two-dimensional nickel oxide was obtained.

[0073] Preparation of two-dimensional porous nickel oxide:

[0074] Weigh 50 mg of the obtained ion-intercalated nickel oxide and place it in a 15 mL glass sample bottle. Add 10 mL of hexane to disperse the nickel oxide evenly.

[0075] 2 mL of n-butyllithium solution was added to a glass bottle in a glove box. A magnetic stir bar was placed in the glass bottle and the mixture was stirred on a magnetic stirrer for 20 h. After standing, ethanol was added to consume the unreacted n-butyllithium. The reaction product in the glass bottle was filtered, washed with water, and dried at 60 °C to obtain two-dimensional porous nickel oxide.

[0076] The pore size and specific surface area of ​​the two-dimensional porous iron oxide prepared by this method are within the protection scope of this invention.

[0077] Example 5:

[0078] Preparation of molten salt: Heat the muffle furnace to 350℃, place a crucible containing 5g of NaNO3 into the muffle furnace, and keep it heated in air for 10 minutes until the NaNO3 becomes molten.

[0079] Preparation of ion-intercalated two-dimensional alumina: 0.2g of AlCl3 powder was quickly added to molten NaNO3 and reacted for 1 min. The crucible was then quickly removed from the muffle furnace and quenched in air at room temperature. After the crucible cooled to room temperature, deionized water was added to soak it. The mixture was then filtered and washed to remove excess unreacted salt. After drying at 60℃, brownish-black ion-intercalated two-dimensional alumina was obtained.

[0080] Preparation of two-dimensional porous alumina:

[0081] Weigh 50 mg of the obtained ion-intercalated alumina and place it in a 15 mL glass sample bottle. Add 10 mL of hexane to disperse the alumina evenly.

[0082] 2 mL of n-butyllithium solution was added to a glass bottle in a glove box. A magnetic stir bar was placed in the glass bottle and the mixture was stirred on a magnetic stirrer for 20 h. After standing, ethanol was added to consume the unreacted n-butyllithium. The reaction product in the glass bottle was filtered, washed with water, and dried at 60 °C to obtain two-dimensional porous alumina.

[0083] The pore size and specific surface area of ​​the two-dimensional porous iron oxide prepared by this method are within the protection scope of this invention.

[0084] Example 6:

[0085] Preparation of molten salt: Heat the muffle furnace to 420℃, place a crucible containing 5g of LiNO3 into the muffle furnace, and keep it heated in air for 10 minutes until the LiNO3 becomes molten.

[0086] Ion-intercalated two-dimensional tungsten oxide: 0.2g of ammonium tungstate powder was quickly added to molten LiNO3 and reacted for 2 minutes. The crucible was then quickly removed from the muffle furnace and quenched in air at room temperature. After the crucible cooled to room temperature, deionized water was added to soak it. The mixture was then filtered and washed to remove excess unreacted salts. After drying at 60°C, brownish-black ion-intercalated two-dimensional tungsten oxide was obtained.

[0087] Two-dimensional porous tungsten oxide:

[0088] Weigh 50 mg of the obtained ion-intercalated tungsten oxide and place it in a 15 mL glass sample bottle. Add 10 mL of hexane to disperse the tungsten oxide evenly.

[0089] 2 mL of n-butyllithium solution was added to a glass bottle in a glove box. A magnetic stir bar was placed in the glass bottle and the mixture was stirred on a magnetic stirrer for 20 h. After standing, ethanol was added to consume the unreacted n-butyllithium. The reaction product in the glass bottle was filtered, washed with water, and dried at 60 °C to obtain two-dimensional porous tungsten oxide.

[0090] The pore size and specific surface area of ​​the two-dimensional porous iron oxide prepared by this method are within the protection scope of this invention.

[0091] Example 7:

[0092] Preparation of molten salt: Heat the muffle furnace to 380℃, place a crucible containing 5g KNO3 into the muffle furnace, and keep it in air atmosphere for 10min until the KNO3 becomes molten.

[0093] Preparation of ion-intercalated two-dimensional manganese oxide: 0.2g of MnSO4 powder was quickly added to molten KNO3 and reacted for 1 min. The crucible was then quickly removed from the muffle furnace and quenched in air at room temperature. After the crucible cooled to room temperature, deionized water was added to soak it. The mixture was then filtered and washed to remove excess unreacted salt. After drying at 60℃, brown-black ion-intercalated two-dimensional manganese oxide was obtained.

[0094] Preparation of two-dimensional porous manganese oxide:

[0095] Weigh 50 mg of the obtained ion-intercalated manganese oxide and place it in a 15 mL glass sample bottle. Add 10 mL of hexane to disperse the manganese oxide evenly.

[0096] 1 mL of n-butyllithium solution was added to a glass bottle in a glove box. A magnetic stir bar was placed in the glass bottle and the mixture was stirred on a magnetic stirrer for 20 h. After standing, ethanol was added to consume the unreacted n-butyllithium. The reaction product in the glass bottle was filtered, washed with water, and dried at 60 °C to obtain two-dimensional porous manganese oxide.

[0097] The HR-TEM image of the two-dimensional porous manganese oxide prepared in Example 7 has a scale bar of 2 nm. It can be seen that the obtained manganese oxide has a certain pore structure, but the effect on the pore structure is not obvious compared with that when 2 mL of n-butyllithium was added in Example 1.

[0098] Those skilled in the art will readily understand that the above description is merely a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, and improvements made within the spirit and principles of the present invention should be included within the scope of protection of the present invention.

Claims

1. A method for preparing a two-dimensional porous oxide, characterized in that, The method includes the following steps: (1) Using metal salt as a precursor, an ion-intercalated two-dimensional oxide with water of crystallization in the interlayer was prepared by the molten salt method. (2) The ion-intercalated two-dimensional oxide is mixed with a lithium initiator, and after a predetermined reaction time, the unreacted lithium initiator is removed, filtered and washed to obtain a two-dimensional porous oxide; the lithium initiator includes n-butyllithium, isopropyllithium, n-pentyllithium, and n-hexyllithium.

2. The method for preparing a two-dimensional porous oxide according to claim 1, characterized in that, The lithium initiator is n-butyllithium.

3. The method for preparing a two-dimensional porous oxide according to claim 1, characterized in that, The ratio of the ion-intercalated two-dimensional oxide to the lithium initiator is 10-50 mg / mL.

4. The method for preparing a two-dimensional porous oxide according to claim 1, characterized in that, In step (2), the reaction conditions are an inert atmosphere and the reaction time is 16-24 hours.

5. The method for preparing a two-dimensional porous oxide according to claim 1, characterized in that, The method further includes: before mixing the ion-intercalated two-dimensional oxide with the lithium initiator, using liquid alkane as a dispersant to uniformly disperse the ion-intercalated two-dimensional oxide in the dispersant; wherein the ratio of the ion-intercalated two-dimensional oxide to the liquid alkane is 5-25 mg / mL.

6. The method for preparing a two-dimensional porous oxide according to claim 1, characterized in that, The specific steps of step (1) are as follows: the metal salt and molten salt are mixed and heated, quenched and cooled, and washed to obtain an ion-intercalated two-dimensional oxide; The mass ratio of the molten salt to the metal salt is 10-25:1; the reaction time is 30-300s.

7. The method for preparing a two-dimensional porous oxide according to claim 6, characterized in that, In step (1), the molten salt is a salt with a melting point not higher than 400°C.

8. The method for preparing a two-dimensional porous oxide according to claim 1, characterized in that, In step (1), the metal salt is selected from nitrates, sulfates, chlorides, carbonates, acetates, phosphates, hydrogen phosphates, vanadates, niobates, molybdates, titanates, and tungstates.

9. A method for preparing a two-dimensional porous oxide according to claim 1, characterized in that, The metal elements in the metal salt are selected from Ti, V, Cr, Mn, Fe, Co, Ni, Nb, Mo, Ru, Rh, In, Sn, Cs, and W.

10. The two-dimensional porous oxide obtained by the preparation method according to any one of claims 1-9, characterized in that, The two-dimensional porous oxide surface forms uniform pores with a pore size ranging from 2-10 nm and a specific surface area of ​​200-300 m². 2 / g.

Citation Information

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