CN115215299A - Method for preparing porous material - Google Patents
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- CN115215299A CN115215299A CN202110424480.4A CN202110424480A CN115215299A CN 115215299 A CN115215299 A CN 115215299A CN 202110424480 A CN202110424480 A CN 202110424480A CN 115215299 A CN115215299 A CN 115215299A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B13/00—Oxygen; Ozone; Oxides or hydroxides in general
- C01B13/14—Methods for preparing oxides or hydroxides in general
- C01B13/145—After-treatment of oxides or hydroxides, e.g. pulverising, drying, decreasing the acidity
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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
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/20—Methods for preparing sulfides or polysulfides, in general
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/08—Drying; Calcining ; After treatment of titanium oxide
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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
- C01P2006/16—Pore diameter
Abstract
The invention discloses a method for preparing a porous material, which comprises the following steps: reacting a reducing agent with the continuous medium nonporous material containing the metal to reduce high-potential ions in the continuous medium nonporous material containing the metal to obtain the porous material with controllable pore size. The method is a solution method, has wide application objects, simple operation, easily obtained raw materials and low cost, can accurately control the pore size of the prepared porous material, has no functional group introduced in the reaction process, easily removes byproducts, and can realize large-scale preparation; after a proper solvent is selected, the material has good dispersibility and stability and the concentration of the dispersion liquid is adjustable; the porous material with adjustable pore size has important application prospects in the aspects of energy storage, catalysis, super capacitance, adsorbent, seawater desalination, separation, noise reduction, ion exchange, electromagnetic shielding, bone-implanted biological materials and the like.
Description
Technical Field
The invention belongs to the field of nano material preparation, and particularly relates to a method for preparing a porous material.
Background
The preparation of porous materials is the focus of current research. Compared with continuous medium non-porous materials, the porous material generally has the characteristics of low relative density, high specific strength, large specific surface area, sound absorption, heat insulation, good permeability, high specific surface area, more active sites, selective permeation and the like, shows new physical and chemical properties different from those of the non-porous material, and thus has wide application in the aspects of adsorption, separation, carriers, supports, noise reduction, heat preservation, catalysis, ion exchange and the like.
The current methods for preparing porous materials mainly comprise a template method and a direct synthesis method. (1) The template method is generally classified into a hard template method and a soft template method. The hard template method is to use the inner surface or the outer surface of the material as a template, to fill the monomer of the template to perform chemical or electrochemical reaction, and to remove the template by controlling the reaction time to obtain various porous materials. However, in the preparation process, the template is selected, the template removal is complex, the large-scale production is not easy, and the impurities are easy to remain. (2) Direct synthesis is an effective method for synthesizing microporous materials, but it requires a high reaction system and can only be used for synthesizing certain specific reaction types. Some conventional raw materials are difficult to use as raw materials for preparing the microporous structure, which also results in a narrow selection range of microporous materials.
The traditional porous materials, such as zeolite, have the pore diameter generally below 1nm, and the pore diameter is uncontrollable, so that the application range of the traditional porous materials is limited. However, in the metal oxide porous material reported at present, for example, biological small molecular glycine is used as a template reagent and a copper nitrate solution is used as a copper source, macroporous CuO formed by self-assembly of nanoparticles is synthesized through a thermal decomposition route, the pore size is between 50nm and several micrometers, the pore size is large, the filtering effect on small molecules is not obvious, and the synthesis process is complex. The mesoporous MgO synthesized by the gel method has long sol-gel process time which is several weeks; when the gel is dried, it is liable to shrink, causing structural failure.
In view of the above, it is necessary to develop a new method for preparing porous materials.
Disclosure of Invention
In order to solve the problems raised in the background art described above, it is an object of the present invention to provide a method for producing a porous material. The research of directly reducing the material by the reducing agent to directly obtain the porous material is the initiative of the applicant. Compared with a template method, the method does not need to additionally design a template with specific aperture and morphology, and can directly control the aperture size of the material by controlling the concentration of the reducing agent, the reaction time and the reaction temperature; the method is a solution method, has wide application objects, simple operation, easily obtained raw materials and low cost, can accurately control the pore size of the prepared porous material, has no functional group introduced in the reaction process, easily removes byproducts, and can realize large-scale preparation; after a proper solvent is selected, the material has good dispersibility and stability, and the concentration of the dispersion liquid is adjustable; the porous material with adjustable pore size has important application prospects in the aspects of energy storage, catalysis, super capacitance, adsorbent, seawater desalination, separation, noise reduction, ion exchange, electromagnetic shielding, bone-implanted biological materials and the like.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: in one aspect, the present invention provides a method of making a porous material comprising the steps of: and reacting the reducing agent with the continuous medium nonporous material containing the metal to reduce high-potential ions in the continuous medium nonporous material containing the metal, thereby obtaining the porous material with controllable pore size.
Further, the method comprises the following steps: and dropping the reducing agent into the continuous medium nonporous material dispersion liquid containing the metal at a certain speed to ensure that the reducing agent and high-potential ions in the continuous medium nonporous material containing the metal generate oxidation-reduction reaction, reducing the high-potential ions and removing the high-potential ions from the framework to obtain the porous material.
Further, after the reaction is finished, the sediment is precipitated by adopting a centrifugation mode, wherein the centrifugation speed is 10-12000 rpm, and the centrifugation time is 5-30 minutes. For separating the porous material from the by-products, a centrifugation rate of 8000rpm is preferred, with a centrifugation time of 15 minutes being preferred.
Further, the reducing agent comprises at least one of hydrogen halide and ascorbic acid;
preferably, the hydrogen halide is hydrogen fluoride, hydrogen chloride, hydrogen bromide, hydrogen iodide.
Further, the concentration of the reducing agent is 0.01mol/L to 5mol/L, preferably 1.2mol/L.
Further, the metal-containing continuous media non-porous material comprises a monometallic oxide, a bimetallic oxide, a trimetallic oxide, a monometallic sulfide, a bimetallic sulfide, a trimetallic sulfide;
preferably, the single metal oxide includes titanium oxide, zinc oxide, tin oxide, manganese oxide, cobalt oxide, nickel oxide, iron oxide;
preferably, the bimetallic oxide comprises ferrotitanium oxide, manganese cobalt oxide, ferronickel oxide;
preferably, the trimetallic oxide comprises cobalt nickel iron oxide;
preferably, the single metal sulfide includes titanium sulfide, zinc sulfide, tin sulfide, manganese sulfide, cobalt sulfide, nickel sulfide, iron sulfide;
preferably, the bimetallic sulfide comprises ferrotitanium sulfide, cobalt manganese sulfide, ferronickel sulfide;
preferably, the trimetallic sulfide comprises iron cobalt nickel sulfide.
Further, the reaction temperature is 0-120 ℃, and the reaction time is 1 minute-two hours; the reaction temperature is preferably 25 ℃ and the reaction time is preferably 15 minutes.
Further, the dropping rate of the reducing agent is 0.1mL/min to 100mL/min, preferably 10mL/min.
Further, the pore diameter of the porous material is 0.1 nm-10 nm.
On the other hand, the invention provides a porous material dispersion liquid, the prepared porous material is washed by a solvent, and then the solvent is added to obtain the porous material dispersion liquid with adjustable concentration;
preferably, the solvent comprises deionized water, an organic solvent, a surfactant aqueous solution and a polymer aqueous solution;
more preferably, the organic solvent comprises methanol, ethanol, isopropanol, acetone, diethyl ether, N-methylpyrrolidone, N-dimethylformamide, benzene;
more preferably, the aqueous surfactant solution comprises an aqueous sodium dodecylbenzene sulfonate solution, an aqueous tetrabutylammonium hydroxide solution, an aqueous cetyltrimethylammonium bromide solution;
more preferably, the aqueous polymer solution comprises an aqueous solution of sodium polystyrene sulfonate.
The porous material is washed by the solvent and then added into the proper solvent, so that the porous material dispersion liquid with good dispersibility and stability can be obtained, and the operability of the application of the nano material is greatly improved.
Further, the porous material dispersion liquid is dried to obtain solid-phase porous nano powder, and the solid-phase porous nano powder is dispersed in the solvent again to obtain a secondary dispersion liquid containing the porous material.
The invention has the beneficial effects that: the reducing agent needed in the method is low in price, easy to obtain and simple to operate. Reacting reducing agent with high potential ions to obtain a porous material; on the other hand, the pore size of the porous material can be controlled by controlling the reaction concentration, the reaction temperature and the reaction time of the reducing agent. Compared with the template method which needs to prepare a specific precursor template, the method can obtain the needed porous material only by controlling the concentration of the reducing agent, the reaction time and the reaction temperature. Meanwhile, because the reaction rate of the oxidation-reduction reaction is extremely high, compared with a template method, the preparation time required by the method is greatly shortened. Secondly, compared with the direct synthesis method, the method has wider adaptability and does not need harsh reaction conditions. The method requires materials to have high ionic potential ions, the materials selected in the invention, such as single metal oxides (titanium oxide, zinc oxide, tin oxide, manganese oxide, cobalt oxide, nickel oxide, iron oxide and the like), double metal/trimetal oxides (titanium oxide, cobalt manganese oxide, nickel iron oxide, iron cobalt nickel oxide and the like), single metal sulfides (titanium sulfide, zinc sulfide, tin sulfide, manganese sulfide, cobalt sulfide, nickel sulfide, iron sulfide and the like), double metal/trimetal sulfides (titanium sulfide, cobalt manganese sulfide, nickel iron sulfide, iron cobalt nickel sulfide and the like), and the like, all have high ionic potential ions, and the steps for preparing the porous materials by using a direct synthesis method and a template method are complicated, the energy consumption is large and the efficiency is low in the current large-scale preparation process, and the method effectively solves the problem. In addition, compared with a template method, the method has the advantages that the reducing agent and the by-product are easy to remove, and the purity of the obtained porous material is high. The precipitate after reaction with the reducing agent may be further processed, washed with a suitable solvent and then added with a suitable solvent to obtain a porous material dispersion. Meanwhile, the porous material dispersion liquid with uniform dispersion and adjustable concentration can be prepared by changing the volume of the solvent, and can be directly applied to the fields of energy storage, catalysis, super capacitors, adsorbents, seawater desalination, separation, noise reduction, ion exchange, electromagnetic shielding, bone-implanted biomaterials and the like.
Drawings
FIG. 1 is a TEM image of raw titanium oxide in example 1 of the present invention.
FIG. 2 is a TEM image of porous titanium oxide prepared in example 1 of the present invention.
FIG. 3 is a TEM image of porous titanium oxide prepared at different reaction concentrations; TEM pictures of porous titanium oxide prepared at room temperature and with stirring time of 15 minutes and different hydrogen iodide concentrations, wherein the A. Hydrogen iodide concentration is 0.2mol/L, the B. Hydrogen iodide concentration is 0.1mol/L, the C. Hydrogen iodide concentration is 0.05mol/L and the D. Hydrogen iodide concentration is 0.03mol/L.
Detailed Description
In order that the invention may be more clearly understood by those skilled in the art, the present invention will now be described in detail with reference to the specific embodiments and the accompanying drawings.
The invention adds the reducing agent into the continuous medium non-porous material solution, and the porous material is obtained through the reaction between the reducing agent and the high-potential ions in the non-porous material. In the reaction process, a reducing agent is gradually dripped to reduce high-potential ions, and the pore diameter of the porous material is accurately regulated and controlled by controlling the concentration of the reducing agent, the reaction temperature and the reaction time. The concentration of the reducing agent is 0.01-5 mol/L, the reaction temperature is 0-120 ℃, and the reaction time is 1 minute-two hours. Among these, the reducing agent concentration mainly plays a role in reducing high potential ions. The reducing agent used in the invention is ascorbic acid and hydrogen halide, which is different from the characteristic that a precursor template needs to be prepared by a template method, the method directly prepares the porous material by using the redox reaction of the reducing agent and the nonporous material, and the method has simple operation. Secondly, the concentration of the reducing agent is adjusted, high-potential ions in the non-porous material are directly reduced under the driving of potential, and the pore size of the obtained porous material is controllable. Because different concentrations of reducing agent are used, the material pore size obtained by increasing the concentration of the reducing agent is larger in the same reaction time. Meanwhile, under the same concentration, the reaction time is prolonged, and the pore diameter can also be increased to a certain extent. And (3) cleaning the centrifugal precipitate after the reaction with the reducing agent by using a solvent, adding a proper solvent, and dispersing to obtain the porous material dispersion liquid with adjustable concentration. According to the solubility difference of the porous material in different solvents, the solvents involved in the invention comprise deionized water, organic solvents, surfactant aqueous solutions and polymer aqueous solutions, wherein the organic solvents are preferably methanol, absolute ethyl alcohol, isopropanol, acetone, diethyl ether, N-methylpyrrolidone (NMP), N-dimethylformamide and benzene, the surfactant aqueous solutions are preferably sodium dodecyl benzene sulfonate aqueous solution and hexadecyl trimethyl ammonium bromide aqueous solution, and the polymer aqueous solutions are preferably sodium polystyrene sulfonate aqueous solution.
Example 1
At room temperature, 10mL of 3mol/L hydrogen iodide is dropped into 10mL of 2mg/mL of titanium oxide dispersion liquid at the speed of 2mL/min, then stirring is carried out for 15 minutes, then centrifugation is carried out for 15 minutes at 8000rpm, and precipitates are washed by absolute ethyl alcohol, so that porous solid-phase material powder is obtained. And adding the obtained precipitate into 0.04mol/L TBAOH solution to obtain porous material dispersion liquid with the average pore size of 10nm.
Example 2
At room temperature, 10mL of 1.2mol/L hydrogen iodide was dropped into 10mL of 2mg/mL of titanium oxide dispersion at a rate of 2mL/min, followed by stirring for 15 minutes, centrifugation at 8000rpm for 15 minutes, and the precipitate was washed with absolute ethanol to obtain a porous solid-phase material powder. And adding the obtained precipitate into 0.04mol/L TBAOH solution to obtain porous material dispersion liquid with the average pore size of 5 nm.
Example 3
At room temperature, 10mL of 0.6mol/L hydrogen iodide is dripped into 10mL of 2mg/mL titanium oxide dispersion liquid at the speed of 2mL/min, then the mixture is stirred for 15 minutes, and then the mixture is centrifuged at 8000rpm for 15 minutes, and precipitates are washed by absolute ethyl alcohol to obtain porous solid-phase material powder. And adding the obtained precipitate into 0.04mol/L TBAOH solution to obtain porous material dispersion liquid with the average pore size of 3 nm.
Example 4
At room temperature, 10mL of 0.3mol/L hydrogen iodide is dropped into 10mL of 2mg/mL of titanium oxide dispersion liquid at the speed of 2mL/min, then stirring is carried out for 15 minutes, then centrifugation is carried out at 8000rpm for 15 minutes, and precipitates are washed by absolute ethyl alcohol, so that porous solid-phase material powder is obtained. And adding the obtained precipitate into 0.04mol/L TBAOH solution to obtain porous material dispersion liquid with the average pore size of 1 nm.
Example 5
At room temperature, 10mL of 0.2mol/L hydrogen iodide was dropped into 10mL of 2mg/mL of titanium oxide dispersion at a rate of 2mL/min, followed by stirring for 15 minutes, centrifugation at 8000rpm for 15 minutes, and the precipitate was washed with absolute ethanol to obtain a porous solid-phase material powder. And adding the obtained precipitate into 0.04mol/L TBAOH solution to obtain porous material dispersion liquid with the average pore size of 0.5 nm.
Example 6
At room temperature, 10mL of 0.1mol/L hydrogen iodide was dropped into 10mL of 2mg/mL of titanium oxide dispersion at a rate of 2mL/min, followed by stirring for 15 minutes, centrifugation at 8000rpm for 15 minutes, and the precipitate was washed with absolute ethanol to obtain a porous solid-phase material powder. And adding the obtained precipitate into 0.04mol/L TBAOH solution to obtain porous material dispersion liquid with the average pore size of 0.3 nm.
Example 7
At room temperature, 10mL of 0.05mol/L hydrogen iodide is dropped into 10mL of 2mg/mL of titanium oxide dispersion liquid at the speed of 2mL/min, then stirring is carried out for 15 minutes, then centrifugation is carried out at 8000rpm for 15 minutes, and precipitates are washed by absolute ethyl alcohol, so that porous solid-phase material powder is obtained. And adding the obtained precipitate into 0.04mol/L TBAOH solution to obtain porous material dispersion liquid with the average pore size of 0.2 nm.
Example 8
At room temperature, 10mL of 0.03mol/L hydrogen iodide was dropped into 10mL of 2mg/mL of titanium oxide dispersion at a speed of 2mL/min, and then the mixture was stirred for 15 minutes, and then centrifuged at 8000rpm for 15 minutes, and the precipitate was washed with absolute ethanol, so that porous solid-phase material powder was obtained. And adding the obtained precipitate into 0.04mol/L TBAOH solution to obtain porous material dispersion liquid with the average pore size of 0.1 nm.
Example 9
At room temperature, 10mL of 1.2mol/L hydrogen iodide was dropped into 10mL of 2mg/mL of titanium oxide dispersion at a rate of 2mL/min, and then the mixture was stirred for 30 minutes, then centrifuged at 8000rpm for 15 minutes, and the precipitate was washed with absolute ethanol to obtain a porous solid-phase material powder. And adding the obtained precipitate into 0.04mol/L TBAOH solution to obtain porous material dispersion liquid with the average pore size of 7 nm.
Example 10
At room temperature, 10mL of 1.2mol/L hydrogen iodide was dropped into 10mL of 2mg/mL of titanium oxide dispersion at a rate of 2mL/min, and then the mixture was stirred for 45 minutes, then centrifuged at 8000rpm for 15 minutes, and the precipitate was washed with absolute ethanol to obtain a porous solid-phase material powder. And adding the obtained precipitate into 0.04mol/L TBAOH solution to obtain porous material dispersion liquid with the average pore size of 9 nm.
Example 11
At room temperature, 10mL of 0.2mol/L hydrogen iodide was dropped into 10mL of 2mg/mL of titanium oxide dispersion at a rate of 2mL/min, and then the mixture was stirred for 30 minutes, then centrifuged at 8000rpm for 15 minutes, and the precipitate was washed with absolute ethanol to obtain a porous solid-phase material powder. And adding the obtained precipitate into 0.04mol/L TBAOH solution to obtain porous material dispersion liquid with the average pore size of 0.6 nm.
Example 12
At room temperature, 10mL of 0.2mol/L hydrogen iodide was dropped into 10mL of 2mg/mL of titanium oxide dispersion at a rate of 2mL/min, and then the mixture was stirred for 45 minutes, then centrifuged at 8000rpm for 15 minutes, and the precipitate was washed with absolute ethanol to obtain a porous solid-phase material powder. And adding the obtained precipitate into 0.04mol/L TBAOH solution to obtain porous material dispersion liquid with the average pore size of 0.7 nm.
Example 13
10mL of 0.2mol/L hydrogen iodide is dropped into 10mL of 2mg/mL titanium oxide dispersion liquid at the speed of 2mL/min at the temperature of 40 ℃, then stirring is carried out for 45 minutes, then centrifugation is carried out for 15 minutes at 8000rpm, and precipitates are washed by absolute ethyl alcohol, so that porous solid-phase material powder is obtained. Adding the obtained precipitate into 0.04mol/L TBAOH solution to obtain porous material dispersion liquid with the average pore size of 0.8 nm.
Example 14
At 60 ℃, 10mL of 0.2mol/L hydrogen iodide is dropped into 10mL of 2mg/mL of titanium oxide dispersion liquid at the speed of 2mL/min, then stirring is carried out for 45 minutes, then centrifugation is carried out for 15 minutes at 8000rpm, and precipitates are washed by absolute ethyl alcohol, so that porous solid-phase material powder is obtained. Adding the obtained precipitate into ethanol solution to obtain porous material dispersion liquid with average pore size of 0.9 nm.
Comparative example 1
And stirring the titanium oxide dispersion liquid for 30 minutes at room temperature, centrifuging at 8000rpm for 15 minutes, and cleaning the precipitate by using absolute ethyl alcohol to obtain porous solid-phase material powder. And adding the obtained precipitate into an ethanol solution to obtain the non-porous titanium oxide dispersion liquid of the continuous medium.
Analysis of results
FIG. 1 is a TEM image of the original titanium oxide of example 1. The titanium oxide is shown as a continuous medium non-porous material.
FIG. 2 is a TEM image of porous titanium oxide obtained in example 1. In the figure, the porous titanium oxide is uniformly distributed in the field of the transmission electron microscope, and the existence of most graphite nanosheets in the form can be known through ruler measurement and analysis, and the average pore size is 10nm.
FIG. 3 is a TEM image of porous iron oxides prepared at room temperature with stirring time of 15 minutes and varying reducing agent reaction concentrations. In the figure, the average pore diameter of the porous titanium oxide prepared by different reducing agent concentrations is in positive correlation with the reducing agent concentration, namely, the higher the hydrogen iodide concentration is, the larger the average pore diameter of the porous titanium oxide is at the same temperature.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.
Claims (10)
1. A method of making a porous material comprising the steps of: and reacting the reducing agent with the continuous medium nonporous material containing the metal to reduce ions with high potential in the continuous medium nonporous material containing the metal to obtain the porous material.
2. The method for preparing a porous material according to claim 1, comprising the steps of: dropping the reducing agent into the continuous medium nonporous material dispersion liquid containing the metal at a certain speed to ensure that the reducing agent and high-potential ions in the continuous medium nonporous material containing the metal generate oxidation reduction reaction, reducing the high-potential ions and removing the high-potential ions from the framework to obtain the porous material.
3. The method for producing a porous material according to claim 1 or 2, wherein the reducing agent includes at least one of hydrogen halide, ascorbic acid;
preferably, the hydrogen halide is hydrogen fluoride, hydrogen chloride, hydrogen bromide, hydrogen iodide.
4. The method for preparing a porous material according to claim 3, wherein the concentration of the reducing agent is 0.01 to 5mol/L.
5. The method of producing a porous material according to claim 1 or 2, wherein the metal-containing continuous-medium non-porous material comprises a monometallic oxide, a bimetallic oxide, a trimetallic oxide, a monometallic sulfide, a bimetallic sulfide, a trimetallic sulfide;
preferably, the single metal oxide includes titanium oxide, zinc oxide, tin oxide, manganese oxide, cobalt oxide, nickel oxide, iron oxide;
preferably, the bimetallic oxide comprises ferrotitanium oxide, manganese cobalt oxide, ferronickel oxide;
preferably, the trimetallic oxide comprises cobalt nickel iron oxide;
preferably, the single metal sulfide includes titanium sulfide, zinc sulfide, tin sulfide, manganese sulfide, cobalt sulfide, nickel sulfide, iron sulfide;
preferably, the bimetallic sulfide comprises ferrotitanium sulfide, cobalt manganese sulfide, ferronickel sulfide;
preferably, the trimetallic sulfide comprises iron cobalt nickel sulfide.
6. The method for preparing a porous material according to claim 1 or 2, wherein the reaction temperature is 0 ℃ to 120 ℃ and the reaction time is 1 minute to two hours.
7. The method for preparing a porous material according to claim 2, wherein the dropping speed of the reducing agent is 0.1 to 100mL/min.
8. The method for preparing a porous material according to claim 1 or 2, wherein the pore size of the porous material is 0.1nm to 10nm.
9. A porous material dispersion, characterized in that the porous material prepared according to claim 1 or 2 is washed with a solvent, and then the solvent is added to obtain a porous material dispersion with adjustable concentration;
preferably, the solvent comprises deionized water, an organic solvent, a surfactant aqueous solution and a polymer aqueous solution;
more preferably, the organic solvent comprises methanol, ethanol, isopropanol, acetone, diethyl ether, N-methylpyrrolidone, N-dimethylformamide, benzene;
more preferably, the aqueous surfactant solution comprises an aqueous sodium dodecylbenzene sulfonate solution, an aqueous tetrabutylammonium hydroxide solution, an aqueous cetyltrimethylammonium bromide solution;
more preferably, the aqueous polymer solution comprises an aqueous solution of sodium polystyrene sulfonate.
10. The porous material dispersion liquid according to claim 9, wherein the porous material dispersion liquid is dried to obtain a solid phase porous nano powder, and the solid phase porous nano powder is dispersed in the solvent again to obtain a secondary dispersion liquid containing the porous material.
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| CN110907428A (en) * | 2019-12-19 | 2020-03-24 | 哈尔滨工业大学 | Method for preparing reusable porous SERS metal substrate by reduction induction method and application thereof |
| CN111348676A (en) * | 2018-12-21 | 2020-06-30 | 厦门稀土材料研究所 | Porous metal oxide nanosheet and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111348676A (en) * | 2018-12-21 | 2020-06-30 | 厦门稀土材料研究所 | Porous metal oxide nanosheet and preparation method and application thereof |
| CN110907428A (en) * | 2019-12-19 | 2020-03-24 | 哈尔滨工业大学 | Method for preparing reusable porous SERS metal substrate by reduction induction method and application thereof |
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| GAINI ZHANG等: ""Rational design and controllable preparation of holey MnO2 nanosheets"" * |
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