CN115142089A - Preparation method of organic-inorganic composite membrane for hydrogen production by alkaline electrolysis of water - Google Patents
Preparation method of organic-inorganic composite membrane for hydrogen production by alkaline electrolysis of water Download PDFInfo
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- CN115142089A CN115142089A CN202210690207.0A CN202210690207A CN115142089A CN 115142089 A CN115142089 A CN 115142089A CN 202210690207 A CN202210690207 A CN 202210690207A CN 115142089 A CN115142089 A CN 115142089A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B13/00—Diaphragms; Spacing elements
- C25B13/04—Diaphragms; Spacing elements characterised by the material
- C25B13/05—Diaphragms; Spacing elements characterised by the material based on inorganic materials
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/02—Hydrogen or oxygen
- C25B1/04—Hydrogen or oxygen by electrolysis of water
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
- Y02P20/133—Renewable energy sources, e.g. sunlight
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Abstract
The invention discloses a preparation method of an organic-inorganic composite membrane for hydrogen production by alkaline electrolysis of water. The method comprises the steps of firstly growing layered double hydroxides on the surfaces of inorganic particles in situ by a chemical method to obtain the composite filler, then introducing the composite filler into a polymer matrix, and preparing the organic-inorganic composite membrane by adopting a solution immersion phase conversion method. The existence of the inorganic particles can improve the hydrophilic performance of the diaphragm, promote the conduction of the electrolyte in the anode and the cathode, and reduce the resistance of the diaphragm; after the LDH is introduced, on one hand, the hydrophilic performance of the membrane can be further improved, and on the other hand, the LDH has better intrinsic OH － And the conductivity is favorable for further reducing the resistance of the diaphragm. The preparation method provided by the invention can obtain the organic-inorganic composite membrane with smaller resistance, and has important significance for reducing the system energy consumption of the alkaline water electrolyzer.
Description
Technical Field
The invention relates to the technical field of hydrogen production by water electrolysis, in particular to a preparation method of an organic-inorganic composite membrane for hydrogen production by alkaline water electrolysis.
Background
In recent years, hydrogen energy has received much attention worldwide with the transition of national energy strategy. Compared with the traditional energy, the hydrogen has the advantages of high heat value, wide source, reproducibility, cleanness, low carbon and the like. Most hydrogen in industrial application is mainly obtained by the traditional fossil energy hydrogen production method, such as coal hydrogen production method and natural gas hydrogen production method, but the production processes generate a large amount of greenhouse gases, only "ash hydrogen" or "blue hydrogen" can be obtained, and the aim of "double carbon" is difficult to achieve, so that the application of the hydrogen is increasingly limited.
The method for producing hydrogen by electrolyzing water by utilizing clean energy sources such as photovoltaic energy, wind energy and the like to generate electricity can prepare green hydrogen, is a great trend of energy transformation, and is also one of important paths for realizing the aim of double carbon. The water electrolysis hydrogen production mainly comprises alkaline water electrolysis hydrogen production, proton exchange membrane water electrolysis hydrogen production, solid oxide water electrolysis hydrogen production and anion membrane water electrolysis hydrogen production. Wherein, the alkaline water electrolysis hydrogen production cost is lower, the technology is mature, and the technology is the water electrolysis hydrogen production technology with the highest commercialization degree at present. However, the hydrogen production cost of the current alkaline water electrolysis hydrogen production electrolytic cell is obviously higher than that of hydrogen production by fossil energy, and the higher cost is one of the important problems which restrict the further popularization and application of the electrolytic cell and need to be solved urgently. The cost of hydrogen production from water electrolysis generally includes: equipment costs, energy costs, raw material costs, and other operating costs. Wherein the energy cost accounts for the largest proportion, and is generally 40 to 60 percent. Therefore, reducing the energy consumption of the system is one of the important ways to reduce the cost of the electrolyzer. Most of diaphragms used in industrial application are polyphenylene sulfide braided fabrics, and the polyphenylene sulfide braided fabrics are poor in hydrophilic performance and large in resistance, so that the system consumes large energy. Therefore, the development of a low resistance diaphragm is important for reducing the system power consumption of an alkaline water electrolyzer.
Disclosure of Invention
The present invention is directed to solving, at least to some extent, one of the technical problems in the related art.
Therefore, the invention aims to provide a preparation method of an organic-inorganic composite membrane for hydrogen production by alkaline electrolysis of water.
The invention provides a preparation method of an organic-inorganic composite membrane for hydrogen production by alkaline electrolysis of water, which comprises the following steps:
(1) Growing layered double hydroxides on the surface of inorganic particles in situ by a chemical method to obtain the composite filler with the mass fraction of the layered double hydroxides being 1% -50%, preferably, the mass fraction of the layered double hydroxides is 1%, 3%, 5%, 10%, 15%, 20%, 25%, 30%, 35%, 40%, 45%, 50%;
(2) Adding the composite filler into a polymer solution formed by dissolving a polymer in an organic solvent, and uniformly mixing to obtain a membrane casting solution;
(3) Scraping the film on a glass substrate by using the film casting solution to obtain a liquid film, and pre-evaporating the liquid film in air for 5-60s, preferably for 5s, 10s, 15s, 20s, 25s, 30s, 35s, 40s, 45s, 60s;
(4) Immersing the liquid film into deionized water at the temperature of 5-90 ℃ to induce solidification, and separating the liquid film from the glass substrate after 2-10min, wherein the induced solidification time is preferably 2min, 5min, 8min and 10min;
(5) Soaking in deionized water for several times, and drying to obtain 100-800 μm thick organic-inorganic composite film.
In some embodiments, the inorganic particles in the composite filler have a particle size in the range of 10 to 200nm.
In some embodiments, the inorganic particles are one or more of zirconium dioxide, cerium dioxide, titanium dioxide, and barium sulfate.
In some embodiments, the layered double hydroxide comprises divalent metal ions and trivalent metal ions, the divalent metal ions being Mg 2+ 、Zn 2+ 、Ni 2+ 、Ca 2+ One or more of the trivalent metal ions are Al 3+ 、Fe 3 + 、Mn 3+ 、Cr 3+ One or more of them.
In some embodiments, the chemical process is one of a hydrothermal synthesis process, a coprecipitation process, a microwave process, a sol-gel process, or an ion exchange process.
In some embodiments, the polymer is one or more of polysulfone, polyethersulfone, polyphenylene sulfide, polytetrafluoroethylene, polyphenylsulfone, polypropylene, polyethylene.
In some embodiments, the organic solvent is one or more of N-methyl pyrrolidone, dimethyl sulfoxide, dimethylformamide, and dimethylacetamide.
In some embodiments, the mass fraction of the polymer in the organic-inorganic composite film is 10% to 60%, preferably, the mass fraction of the polymer is 10%, 20%, 30%, 35%, 40%, 60%.
In some embodiments, the number of times of soaking in deionized water in step (5) is 2 to 5, wherein the first soaking time is 2 to 10min, and the rest times except for the first soaking time are 10 to 120min.
In some embodiments, the drying in step (5) is at 25 ℃ to 80 ℃ for 0.5 to 24 hours.
Compared with the prior art, the invention has the beneficial effects that:
the method comprises the steps of firstly growing layered double hydroxides on the surfaces of inorganic particles in situ by a chemical method to obtain the composite filler, then introducing the composite filler into a polymer matrix, and preparing the organic-inorganic composite membrane by adopting a solution immersion phase conversion method.The existence of the inorganic particles can improve the hydrophilic performance of the diaphragm, promote the conduction of the electrolyte in the anode and the cathode, and reduce the resistance of the diaphragm; after the LDH is introduced, on one hand, the hydrophilic performance of the membrane can be further improved, and on the other hand, the LDH has better intrinsic OH － And the conductivity is favorable for further reducing the resistance of the diaphragm. The preparation method provided by the invention can obtain the organic-inorganic composite membrane with smaller resistance, and has important significance for reducing the system energy consumption of the alkaline water electrolyzer.
Drawings
The foregoing and/or additional aspects and advantages of the present invention will become apparent and readily appreciated from the following description of the embodiments, taken in conjunction with the accompanying drawings of which:
FIG. 1 is a schematic view of a process for preparing an organic-inorganic composite film according to the present invention;
FIG. 2 is a schematic diagram of a process for preparing an organic-inorganic composite film according to the present invention.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like reference numerals refer to the same or similar elements or elements having the same or similar functions throughout. The embodiments described below with reference to the accompanying drawings are illustrative and intended to explain the present invention and should not be construed as limiting the present invention.
The following describes a method for preparing an organic-inorganic composite membrane for hydrogen production by alkaline electrolysis of water according to an embodiment of the present invention with reference to the accompanying drawings.
As shown in fig. 1-2, the method for preparing the organic-inorganic composite membrane for hydrogen production by alkaline electrolysis of water according to the present invention comprises the following steps:
(1) Growing layered double hydroxides on the surfaces of the inorganic particles in situ by a chemical method to obtain the composite filler with the mass fraction of the layered double hydroxides being 1-50%;
(2) Adding the composite filler into a polymer solution formed by dissolving a polymer in an organic solvent, and uniformly mixing to obtain a membrane casting solution;
(3) Scraping the film on a glass substrate by using the film casting solution to obtain a liquid film, and pre-evaporating the liquid film in the air for 5-60s;
(4) Immersing the liquid film into deionized water at the temperature of 5-90 ℃ to induce solidification, and separating from the glass substrate after 2-10 min;
(5) Soaking in deionized water for several times, and drying to obtain 100-800 μm thick organic-inorganic composite film.
In the step (1), the layered double hydroxide is grown in situ on the surface of the inorganic particles by a chemical method to obtain the composite filler (inorganic particles @ LDH), that is, the LDH (layered double hydroxide) is firstly used for modifying the inorganic particles to form the composite filler, that is, the inorganic particles @ LDH are formed, and then the composite filler is added into the polymer solution. Wherein the chemical method is one of hydrothermal synthesis, coprecipitation, microwave, sol-gel or ion exchange; the inorganic particles are one or more of zirconium dioxide, cerium dioxide, titanium dioxide and barium sulfate, and the particle size range of the inorganic particles is 10-200nm; the mass fraction of layered double hydroxide in the inorganic particles @ LDH is 1% -50%, the layered double hydroxide contains divalent metal ions and trivalent metal ions, and the divalent metal ions are Mg 2+ 、Zn 2+ 、Ni 2+ 、Ca 2+ One or more of the trivalent metal ions are Al 3 + 、Fe 3+ 、Mn 3+ 、Cr 3+ One or more of them.
In the step (2), the polymer is one or more of polysulfone, polyethersulfone, polyphenylene sulfide, polytetrafluoroethylene, polyphenylsulfone, polypropylene and polyethylene, and the organic solvent is one or more of N-methylpyrrolidone, dimethyl sulfoxide, dimethylformamide and dimethylacetamide. It is understood that the mass fraction of the polymer in the polymer solution is set according to the actual situation.
In the step (5), soaking with deionized water for 2-5 times, wherein the first soaking time is 2-10min, and the soaking times except for the first soaking time are 10-120min, specifically, taking deionized water soaking times as an example, the first soaking time is 2-10min, the second soaking time is 10-120min, and the third soaking time is 10-120min; the drying temperature is 25-80 ℃, and the drying time is 0.5-24h; the mass fraction of the polymer in the prepared organic-inorganic membrane is 10-60%.
The organic-inorganic membrane prepared by the method can be applied to the hydrogen production process by alkaline electrolyzed water.
Example 1:
s1, growing MgAl-LDH with the mass fraction of 3% on the surface of zirconia with the particle size range of 10-200nm in situ by a coprecipitation method to obtain zirconia @ MgAl-LDH filler;
s2, dissolving polysulfone in N-methylpyrrolidone to obtain a polysulfone solution, adding the zirconia @ MgAl-LDH obtained in the step S1 as an inorganic filler into the polysulfone solution, and uniformly mixing to obtain a membrane casting solution;
s3, scraping the film on the glass substrate by using the film casting solution to obtain a liquid film, and pre-evaporating the liquid film in the air for 15S;
s4, immersing the liquid film into deionized water at 15 ℃ to induce solidification, and separating from the glass substrate after 5 minutes;
and S5, soaking and cleaning the organic-inorganic composite membrane for 3 times by using deionized water, drying the organic-inorganic composite membrane for 4 hours at 50 ℃ to obtain the organic-inorganic composite membrane, wherein the mass fraction of polysulfone in the organic-inorganic composite membrane is 20%, the first soaking time is 5min, the second soaking time is 30min, and the third soaking time is 50min, and the residual organic solvent is diffused into water by soaking the organic-inorganic composite membrane in the deionized water to achieve the purpose of cleaning.
Example 2:
s1, carrying out in-situ growth of ZnAl-LDH with the mass fraction of 5% on the surface of cerium oxide with the particle size range of 10-200nm by a hydrothermal method to obtain zirconia @ ZnAl-LDH filler;
s2, dissolving polysulfone in N-methylpyrrolidone to obtain a polysulfone solution, adding the cerium oxide @ ZnAl-LDH obtained in the step S1 as an inorganic filler into the polysulfone solution, and uniformly mixing to obtain a membrane casting solution;
s3, scraping the film on the glass substrate by using the film casting solution to obtain a liquid film, and pre-evaporating the liquid film in the air for 15S;
s4, immersing the liquid film into deionized water at 15 ℃ to induce solidification, and separating from the glass substrate after 5 minutes;
and S5, soaking the organic-inorganic composite membrane for 3 times by using deionized water, drying the organic-inorganic composite membrane for 4 hours at 50 ℃ to obtain the organic-inorganic composite membrane, wherein the mass fraction of polysulfone in the organic-inorganic composite membrane is 30%, the first soaking time is 5min, the second soaking time is 40min, the third soaking time is 60min, and the residual organic solvent is diffused into water by soaking the organic-inorganic composite membrane in the deionized water to achieve the aim of cleaning.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, schematic representations of the above terms may be directed to different embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature. In the description of the present invention, "a plurality" means at least two, e.g., two, three, etc., unless explicitly specified otherwise.
While embodiments of the invention have been shown and described, it will be understood by those of ordinary skill in the art that: various changes, modifications, substitutions and alterations can be made to the embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the claims and their equivalents.
Claims (10)
1. A preparation method of an organic-inorganic composite membrane for hydrogen production by alkaline electrolysis of water is characterized by comprising the following steps:
(1) Growing layered double hydroxides on the surfaces of inorganic particles in situ by a chemical method to obtain a composite filler with the mass fraction of the layered double hydroxides being 1% -50%;
(2) Adding the composite filler into a polymer solution formed by dissolving a polymer in an organic solvent, and uniformly mixing to obtain a membrane casting solution;
(3) Scraping the film on a glass substrate by using the film casting solution to obtain a liquid film, and pre-evaporating the liquid film in air for 5-60s;
(4) Immersing the liquid film into deionized water at the temperature of 5-90 ℃ to induce solidification, and separating from the glass substrate after 2-10 min;
(5) Soaking in deionized water for several times, and drying to obtain 100-800 μm thick organic-inorganic composite film.
2. The method of claim 1, wherein the inorganic particles in the composite filler have a particle size in the range of 10 nm to 200nm.
3. The method of claim 1, wherein the inorganic particles are one or more of zirconium dioxide, cerium dioxide, titanium dioxide, and barium sulfate.
4. The method of claim 1, wherein said layered double hydroxide comprises divalent metal ions and trivalent metal ions, and wherein said divalent metal ions are Mg 2+ 、Zn 2+ 、Ni 2+ 、Ca 2+ One or more of (1), the trivalent metal ion is Al 3+ 、Fe 3+ 、Mn 3+ 、Cr 3+ One or more of them.
5. The method of claim 1, wherein the chemical process is one of a hydrothermal synthesis process, a co-precipitation process, a microwave process, a sol-gel process, or an ion exchange process.
6. The method of claim 1, wherein the polymer is one or more of polysulfone, polyethersulfone, polyphenylene sulfide, polytetrafluoroethylene, polyphenylsulfone, polypropylene, and polyethylene.
7. The method of claim 1, wherein the organic solvent is one or more of N-methylpyrrolidone, dimethyl sulfoxide, dimethylformamide, and dimethylacetamide.
8. The method according to claim 1, wherein the mass fraction of the polymer in the organic-inorganic composite film is 10% to 60%.
9. The method of claim 1, wherein the number of times of soaking in deionized water in step (5) is 2-5, wherein the first soaking time is 2-10min, and the number of times of soaking other than the first soaking time is 10-120min.
10. The method of claim 1, wherein the drying in step (5) is at 25 ℃ to 80 ℃ for 0.5 to 24 hours.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115928145A (en) * | 2022-12-28 | 2023-04-07 | 嘉庚创新实验室 | Organic-inorganic composite diaphragm for hydrogen production by alkaline electrolysis of water and preparation method thereof |
| CN117604571A (en) * | 2024-01-18 | 2024-02-27 | 山东东岳高分子材料有限公司 | Porous composite membrane for hydrogen production by alkaline water electrolysis and preparation method thereof |
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| JP2020007574A (en) * | 2018-07-02 | 2020-01-16 | 株式会社日本触媒 | Inorganic-organic composite membrane, and diaphram for electrochemical element |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115928145A (en) * | 2022-12-28 | 2023-04-07 | 嘉庚创新实验室 | Organic-inorganic composite diaphragm for hydrogen production by alkaline electrolysis of water and preparation method thereof |
| CN115928145B (en) * | 2022-12-28 | 2023-10-13 | 嘉庚创新实验室 | Organic-inorganic composite diaphragm for hydrogen production by alkaline water electrolysis and preparation method thereof |
| CN117604571A (en) * | 2024-01-18 | 2024-02-27 | 山东东岳高分子材料有限公司 | Porous composite membrane for hydrogen production by alkaline water electrolysis and preparation method thereof |
| CN117604571B (en) * | 2024-01-18 | 2024-05-14 | 山东东岳高分子材料有限公司 | Porous composite membrane for hydrogen production by alkaline water electrolysis and preparation method thereof |
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