CN114520341A - Electro-catalytic composite material based on bacterial cellulose and preparation method and application thereof - Google Patents
Electro-catalytic composite material based on bacterial cellulose and preparation method and application thereof Download PDFInfo
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- CN114520341A CN114520341A CN202210032493.1A CN202210032493A CN114520341A CN 114520341 A CN114520341 A CN 114520341A CN 202210032493 A CN202210032493 A CN 202210032493A CN 114520341 A CN114520341 A CN 114520341A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/9041—Metals or alloys
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/88—Processes of manufacture
- H01M4/8825—Methods for deposition of the catalytic active composition
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/9075—Catalytic material supported on carriers, e.g. powder carriers
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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
- Y02E60/50—Fuel cells
Abstract
The invention provides an electro-catalytic composite material based on bacterial cellulose and a preparation method and application thereof, wherein the electro-catalytic composite material comprises the following steps: (a) putting the bacterial cellulose into boiling water and boiling for 15-40 min; (b) under the condition of room temperature, uniformly mixing a ferric iron ethanol solution, water, ethanol and dimethyl ammonium acetate mixed solution in a container to obtain a hydrothermal solution; (c) placing the bacterial cellulose in a hydrothermal solution for hydrothermal treatment at the temperature of 100-120 ℃ for 20-23 h; (d) and after the reaction is finished, taking out the bacterial cellulose, washing, drying, and calcining in an argon saturation state at the calcining temperature of 600-800 ℃ for 1-3 h. The iron MOF prepared by the invention can be uniformly loaded on bacterial cellulose, and has good dispersibility and good electrocatalysis effect. The invention is environment-friendly, the raw materials are easy to find, and the cost is low.
Description
Technical Field
The invention relates to the technical field of preparation of electrocatalytic materials, in particular to an electrocatalytic composite material based on bacterial cellulose and a preparation method and application thereof.
Background
With the rapid development of economy, resources are gradually reduced and tensed, and pollution to the environment caused by the vigorous development process of people is not a little. Therefore, scientists are keenly looking for and studying clean energy and new energy. The catalyst can maximize the utilization of energy, and naturally becomes a major research hotspot of scientists.
The Metal Organic Framework (MOF) is a novel nano porous crystal form material, and has the advantages of good chemical stability, large specific surface area, high porosity, strong changeability and the like. The bacterial cellulose is a porous reticular nano-scale biopolymer synthesized by microbial fermentation, has high crystallinity and polymerization degree, and has a high-precision reticular structure, good elasticity and strong tensile strength. Bacterial cellulose has wide application in various fields and has become one of the hot spots of international research.
However, MOFs generally have limited stability, pore size, and most importantly limited conductivity. Therefore, the MOF is loaded on the bacterial cellulose framework, so that the improvement of the overall stability and the physicochemical property of the formed composite material has important research significance.
Disclosure of Invention
The invention aims to provide an electro-catalytic composite material based on bacterial cellulose and a preparation method and application thereof, and aims to solve the problems of poor stability and non-ideal catalytic effect of the conventional material.
The technical scheme of the invention is as follows: an electro-catalytic composite material based on bacterial cellulose, which is prepared by the following method:
(a) putting the bacterial cellulose into boiling water, boiling for 15-40 min, taking out, and cooling to room temperature;
(b) under the condition of room temperature, uniformly mixing a ferric iron ethanol solution, water, ethanol and dimethyl ammonium acetate mixed solution in a container to obtain a hydrothermal solution;
(c) placing the bacterial cellulose treated in the step (a) in a hydrothermal solution for hydrothermal treatment at the temperature of 100-120 ℃ for 20-23 h;
(d) after the reaction is finished, taking out the bacterial cellulose loaded with the iron metal-organic framework material, washing, drying, and calcining in an argon saturation state at the calcining temperature of 600-800 ℃ for 1-3 h;
(e) and after the calcination is finished, naturally cooling to obtain the electrocatalytic composite material.
In the step (a), the bacterial cellulose is a bacterial cellulose sheet with an area of 3-5 square centimeters.
In the step (c), the dosage ratio of the bacterial cellulose to the hydrothermal solution is 3-5: 50 mL.
In the step (b), the ferric iron ethanol solution is ferric nitrate nonahydrate ethanol solution, and the concentration is 0.1-0.2 mol/L; the mixed solution of dimethylammonium acetate is a mixed solution of dimethylammonium acetate and polyacrylonitrile, and the concentration of the dimethylammonium acetate is 0.2-0.4 mol/L.
In the step (b), the volume ratio of the water to the ethanol to the ferric iron ethanol solution to the mixed solution of dimethyl ammonium acetate is 1-2: 1: 1: 35-40.
And (d) washing with methanol, wherein the drying is freeze drying, and the freeze drying time is 12-20 h.
A preparation method of an electro-catalytic composite material based on bacterial cellulose comprises the following steps:
(a) putting the bacterial cellulose into boiling water, boiling for 15-40 min, taking out, and cooling to room temperature;
(b) under the condition of room temperature, uniformly mixing a ferric iron ethanol solution, water, ethanol and dimethyl ammonium acetate mixed solution in a container to obtain a hydrothermal solution;
(c) placing the bacterial cellulose treated in the step (a) in a hydrothermal solution for hydrothermal treatment at the temperature of 100-120 ℃ for 20-23 h;
(d) after the reaction is finished, taking out the bacterial cellulose loaded with the iron metal-organic framework material, washing, drying, and calcining in an argon saturation state at the calcining temperature of 600-800 ℃ for 1-3 h;
(e) and after the calcination is finished, naturally cooling to obtain the electrocatalytic composite material.
In the step (a), the bacterial cellulose is a bacterial cellulose sheet with the area of 3-5 square centimeters; in the step (c), the dosage ratio of the bacterial cellulose to the hydrothermal solution is 3-5: 50 mL.
In the step (b), the ferric iron ethanol solution is ferric nitrate nonahydrate ethanol solution, and the concentration is 0.1-0.2 mol/L; the dimethyl ammonium acetate mixed solution is a mixed solution of dimethyl ammonium acetate and polyacrylonitrile, and the concentration of the dimethyl ammonium acetate is 0.2-0.4 mol/L; the volume ratio of the water to the ethanol to the mixed solution of the ferric iron ethanol solution and the dimethyl ammonium acetate is 1-2: 1: 1: 35-40.
The application of the electrocatalytic composite material in battery preparation.
Compared with the prior art, the method has the following technical effects:
(1) according to the invention, the iron MOF and the bacterial cellulose are combined in a hydrothermal mode, the steps are simple and convenient, and the catalytic effect is good.
(2) According to the composite material of the iron MOF-loaded bacterial cellulose, the iron MOF can be uniformly loaded on the bacterial cellulose, the dispersibility is good, the agglomeration and aggregation phenomena are avoided, and a better catalytic effect can be generated during use. And the specific surface area is large, the structure is stable, and the application prospect is good.
(3) The composite material of the iron MOF-loaded bacterial cellulose takes the bacterial cellulose as a three-dimensional mechanism frame, has little influence on the environment, is easy to find raw materials and has low cost.
Drawings
FIG. 1 is a scanning electron microscope image of the composite material prepared by the present invention.
FIG. 2 is a graph of oxygen reduction performance of the composite material prepared by the present invention in an alkaline environment.
Detailed Description
The present invention is further illustrated by the following examples in which the procedures and methods not described in detail are conventional and well known in the art, and the starting materials or reagents used in the examples are commercially available, unless otherwise specified, and are commercially available. The bacterial cellulose is a conventional bacterial cellulose membrane, and is commercially available.
Example 1:
(1) the bacterial cellulose membrane was cut into 4 square centimeter square pieces, which were then placed in a beaker and boiled for 20 min. Cooling to room temperature for later use.
(2) Preparing 50mL of hydrothermal solution, wherein the volume ratio of the water to the ethanol to the ferric iron ethanol solution to the dimethyl ammonium acetate mixed solution is 1.5: 1: 1: 35. the ferric iron ethanol solution is ferric nitrate nonahydrate ethanol solution, the concentration is 0.15mol/L, the dimethyl ammonium acetate mixed solution is dimethyl ammonium acetate and polyacrylonitrile mixed solution, and the concentration of the dimethyl ammonium acetate is 0.3 mol/L.
(3) Putting 4 bacterial cellulose square sheets into 50mL of hydrothermal solution, then putting the solution into an autoclave, and carrying out hydrothermal treatment at 110 ℃ for 22 h. And after the hydrothermal reaction is finished, naturally cooling the high-pressure kettle to room temperature, taking out the bacterial cellulose loaded with the iron MOF, and washing with methanol.
(4) And (3) freeze-drying the bacterial cellulose loaded with the iron MOF for 18h, then putting the bacterial cellulose into a porcelain boat, and calcining the bacterial cellulose for 2h at 700 ℃ under the argon condition to obtain the composite material of the bacterial cellulose loaded with the iron MOF. The scanning electron micrograph is shown in FIG. 1. And (3) detecting the oxygen reduction performance of the composite material in an alkaline environment to obtain a graph 2.
From FIG. 1, it can be seen that the three-dimensional framework of the bacterial cellulose and the iron MOF are loaded on the fiber, and the specific surface area is large. As can be seen from figure 2, the material has good ORR performance, the half-wave potential is about 0.8, and the electrocatalytic performance is good.
Example 2:
(1) the bacterial cellulose membrane was cut into 4 square centimeter square pieces, which were then placed in a beaker and boiled for 20 min. Cooling to room temperature for later use.
(2) Preparing 50mL of hydrothermal solution, wherein the volume ratio of water to ethanol to the mixed solution of ferric iron ethanol and dimethyl ammonium acetate is 1: 1: 1: 35. the ferric iron ethanol solution is ferric nitrate nonahydrate ethanol solution with the concentration of 0.2mol/L, the dimethyl ammonium acetate mixed solution is dimethyl ammonium acetate and polyacrylonitrile mixed solution, and the dimethyl ammonium acetate concentration is 0.4 mol/L.
(3) Putting 4 bacterial cellulose square sheets into 50mL of hydrothermal solution, then putting the solution into an autoclave, and carrying out hydrothermal treatment at 120 ℃ for 20 h. And after the hydrothermal reaction is finished, naturally cooling the high-pressure kettle to room temperature, taking out the bacterial cellulose loaded with the iron MOF, and washing with methanol.
(4) And (3) freeze-drying the bacterial cellulose loaded with the iron MOF for 18h, then putting the bacterial cellulose into a porcelain boat, and calcining the bacterial cellulose for 1h at 800 ℃ under the argon condition to obtain the composite material of the bacterial cellulose loaded with the iron MOF. The resulting material was characterized and had properties similar to those of the material of example 1.
Example 3:
(1) the bacterial cellulose membrane was cut into 4 square centimeter square pieces, which were then placed in a beaker and boiled for 20 min. Cooling to room temperature for later use.
(2) Preparing 50mL of hydrothermal solution, wherein the volume ratio of water to ethanol to the mixed solution of ferric iron ethanol and dimethyl ammonium acetate is 2: 1: 1: 40. the ferric iron ethanol solution is ferric nitrate nonahydrate ethanol solution with the concentration of 0.1mol/L, the dimethyl ammonium acetate mixed solution is dimethyl ammonium acetate and polyacrylonitrile mixed solution, and the dimethyl ammonium acetate concentration is 0.2 mol/L.
(3) Putting 4 bacterial cellulose square sheets into 50mL of hydrothermal solution, then placing the solution into an autoclave, and carrying out hydrothermal treatment at 100 ℃ for 23 h. And after the hydrothermal reaction is finished, naturally cooling the high-pressure kettle to room temperature, taking out the bacterial cellulose loaded with the iron MOF, and washing with methanol.
(4) And (3) freeze-drying the bacterial cellulose loaded with the iron MOF for 18h, then putting the bacterial cellulose into a porcelain boat, and calcining the bacterial cellulose for 3h at 600 ℃ under the argon condition to obtain the composite material of the bacterial cellulose loaded with the iron MOF. The resulting material was characterized and had properties similar to those of the material of example 1.
The composite material of the iron MOF-loaded bacterial cellulose prepared by the invention has a stable nano three-dimensional structure, the pore diameter is in a nano level, the specific surface area is increased, and the oxygen reduction performance is improved. Although the material is fragile, the catalytic performance is not affected along with the fragmentation of the material, and the electrocatalytic performance is stable.
Claims (10)
1. An electro-catalytic composite material based on bacterial cellulose, characterized in that the material is prepared by the following method:
(a) putting the bacterial cellulose into boiling water, boiling for 15-40 min, taking out, and cooling to room temperature;
(b) under the condition of room temperature, uniformly mixing a ferric iron ethanol solution, water, ethanol and dimethyl ammonium acetate mixed solution in a container to obtain a hydrothermal solution;
(c) placing the bacterial cellulose treated in the step (a) in a hydrothermal solution for hydrothermal treatment at the temperature of 100-120 ℃ for 20-23 h;
(d) after the reaction is finished, taking out the bacterial cellulose loaded with the iron metal-organic framework material, washing, drying, and calcining in an argon saturation state at the calcining temperature of 600-800 ℃ for 1-3 h;
(e) and after the calcination is finished, naturally cooling to obtain the electrocatalytic composite material.
2. The electrocatalytic composite material as set forth in claim 1, wherein in step (a), the bacterial cellulose is a bacterial cellulose sheet having an area of 3-5 cm.
3. The electrocatalytic composite material as set forth in claim 2, wherein in the step (c), the ratio of the bacterial cellulose to the hydrothermal solution is 3-5 pieces: 50 mL.
4. The electrocatalytic composite material as set forth in claim 1, wherein in the step (b), the ferric ethanol solution is ferric nitrate nonahydrate ethanol solution, and the concentration is 0.1-0.2 mol/L; the mixed solution of dimethylammonium acetate is a mixed solution of dimethylammonium acetate and polyacrylonitrile, and the concentration of the dimethylammonium acetate is 0.2-0.4 mol/L.
5. The electrocatalytic composite material as set forth in claim 4, wherein in the step (b), the volume ratio of the water, the ethanol, the ferric iron ethanol solution and the dimethyl ammonium acetate mixed solution is 1-2: 1: 1: 35-40.
6. The electrocatalytic composite material as set forth in claim 1, wherein in the step (d), the washing is performed with methanol, and the drying is freeze-drying, wherein the freeze-drying time is 12-20 hours.
7. A preparation method of an electro-catalytic composite material based on bacterial cellulose is characterized by comprising the following steps:
(a) putting the bacterial cellulose into boiling water, boiling for 15-40 min, taking out, and cooling to room temperature;
(b) under the condition of room temperature, uniformly mixing a ferric iron ethanol solution, water, ethanol and dimethyl ammonium acetate mixed solution in a container to obtain a hydrothermal solution;
(c) placing the bacterial cellulose treated in the step (a) in a hydrothermal solution for hydrothermal treatment at the temperature of 100-120 ℃ for 20-23 h;
(d) after the reaction is finished, taking out the bacterial cellulose loaded with the iron metal-organic framework material, washing, drying, and calcining in an argon saturation state at the calcining temperature of 600-800 ℃ for 1-3 h;
(e) and after the calcination is finished, naturally cooling to obtain the electrocatalytic composite material.
8. The preparation method according to claim 7, wherein in the step (a), the bacterial cellulose is a bacterial cellulose sheet with an area of 3-5 square centimeters; in the step (c), the dosage ratio of the bacterial cellulose to the hydrothermal solution is 3-5: 50 mL.
9. The preparation method according to claim 7, wherein in the step (b), the ferric ethanol solution is a ferric nitrate nonahydrate ethanol solution with a concentration of 0.1-0.2 mol/L; the dimethyl ammonium acetate mixed solution is a mixed solution of dimethyl ammonium acetate and polyacrylonitrile, and the concentration of the dimethyl ammonium acetate is 0.2-0.4 mol/L; the volume ratio of the water to the ethanol to the ferric iron ethanol solution to the dimethyl ammonium acetate mixed solution is (1-2): 1: 1: 35-40.
10. Use of an electrocatalytic composite material as claimed in any one of claims 1 to 6 in the preparation of a battery.
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CN115591583A (en) * | 2022-09-28 | 2023-01-13 | 北京理工大学(Cn) | Preparation method and application of cellulose-MOF core-shell structure |
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