CN114807999A - High-performance gelatin electrocatalyst prepared by electrostatic spinning method - Google Patents
High-performance gelatin electrocatalyst prepared by electrostatic spinning method Download PDFInfo
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- CN114807999A CN114807999A CN202210394603.9A CN202210394603A CN114807999A CN 114807999 A CN114807999 A CN 114807999A CN 202210394603 A CN202210394603 A CN 202210394603A CN 114807999 A CN114807999 A CN 114807999A
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- 108010010803 Gelatin Proteins 0.000 title claims abstract description 54
- 239000008273 gelatin Substances 0.000 title claims abstract description 54
- 229920000159 gelatin Polymers 0.000 title claims abstract description 54
- 235000019322 gelatine Nutrition 0.000 title claims abstract description 54
- 235000011852 gelatine desserts Nutrition 0.000 title claims abstract description 54
- 239000010411 electrocatalyst Substances 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 title claims abstract description 21
- 238000010041 electrostatic spinning Methods 0.000 title claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000003763 carbonization Methods 0.000 claims abstract description 18
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 14
- 239000000835 fiber Substances 0.000 claims abstract description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000008367 deionised water Substances 0.000 claims abstract description 10
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 10
- 239000004744 fabric Substances 0.000 claims abstract description 9
- 239000012300 argon atmosphere Substances 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 238000002360 preparation method Methods 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 238000005303 weighing Methods 0.000 claims abstract description 8
- 238000004321 preservation Methods 0.000 claims description 3
- 238000011534 incubation Methods 0.000 claims description 2
- 150000001721 carbon Chemical class 0.000 abstract description 2
- 239000003792 electrolyte Substances 0.000 description 8
- 238000002484 cyclic voltammetry Methods 0.000 description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 229910052760 oxygen Inorganic materials 0.000 description 6
- 239000001301 oxygen Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- 238000001523 electrospinning Methods 0.000 description 5
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000000017 hydrogel Substances 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 241000282414 Homo sapiens Species 0.000 description 1
- IMQLKJBTEOYOSI-GPIVLXJGSA-N Inositol-hexakisphosphate Chemical compound OP(O)(=O)O[C@H]1[C@H](OP(O)(O)=O)[C@@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@@H]1OP(O)(O)=O IMQLKJBTEOYOSI-GPIVLXJGSA-N 0.000 description 1
- IMQLKJBTEOYOSI-UHFFFAOYSA-N Phytic acid Natural products OP(O)(=O)OC1C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C1OP(O)(O)=O IMQLKJBTEOYOSI-UHFFFAOYSA-N 0.000 description 1
- 239000004642 Polyimide Substances 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 238000004523 catalytic cracking Methods 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002052 molecular layer Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229940068041 phytic acid Drugs 0.000 description 1
- 235000002949 phytic acid Nutrition 0.000 description 1
- 239000000467 phytic acid Substances 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920000128 polypyrrole Polymers 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
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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
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
- C25B11/042—Electrodes formed of a single material
- C25B11/043—Carbon, e.g. diamond or graphene
-
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Fibers (AREA)
Abstract
The invention relates to a method for preparing a high-performance gelatin electrocatalyst by an electrostatic spinning method. The preparation method comprises the following steps: weighing 1.5 g of gelatin, putting the gelatin into a small beaker filled with 8.5 mL of deionized water, and stirring the gelatin in a constant-temperature water bath kettle at 50 ℃ for 0.5 h until the gelatin is completely dissolved; starting electrostatic spinning equipment, and setting the temperature to be 40 ℃; the applied voltage was 18 kV; the flow rate is 0.7 mm/min and the distance from the tip to the collector electrode is 12 cm, and a sample sprayed by the electrostatic spinning equipment is directly sprayed on the treated carbon cloth; placing the obtained product in a crucible, and carrying out carbonization treatment by adopting a tube furnace under the conditions that: and (3) keeping the temperature for 3 h under the argon atmosphere and at the carbonization temperature of 300 ℃, wherein the heating rate is 5 ℃/min. The preparation method has the advantages of simple preparation process, easy operation and short time consumption, and the obtained gelatin fiber has excellent electrochemical performance and stable structure and has the current density of 10 mA cm ‑2 The overpotential is only 376.5 mV, which is superior to the reported carbon-based metal-free electrocatalyst.
Description
Technical Field
The invention belongs to the technical field of new energy electronic materials, and relates to a high-performance gelatin electrocatalyst prepared by an electrostatic spinning method.
Background
The rapid development of the world economy and the increasing demand of human beings have prompted people to seek more environment-friendly and reusable clean energy. Particularly, the national advocates carbon peak reaching and carbon neutralization, and a great number of scientific researchers continuously strive to research and develop in order to actively respond to the national call. At present, electrolysis of water is the most potential way to produce clean renewable energy at present, and the electrolysis process consists of two half-reactions: the Hydrogen Evolution Reaction (HER) of the cathode and the Oxygen Evolution Reaction (OER) of the anode are key processes of water electrocatalytic cracking due to the water oxidation, and the inherent slow dynamic characteristics of the water oxidation enable the water oxidation to become a key process of water catalytic cracking, so that efficient catalysts are further developed to reduce the energy barrier of catalytic reaction, and finally the purposes of improving energy conversion efficiency and reducing hydrogen production cost are achieved. At present, the most effective oxygen evolution reaction is a noble metal catalyst, and in addition, the oxide/hydroxide of the transition metal which is a substitute product of the noble metal catalyst also shows higher electrocatalytic activity, but in order to further reduce the cost and realize large-scale production preparation, a carbon-based metal-free material is considered to be used in the electrocatalytic oxygen evolution process. Lin and the like utilize a novel in-situ polymerization method to design the PPPI material into a nano-scale film on carbon cloth, so that the catalytic activity of the PPPI material is improved, and the prepared PPPI electrode has the current density of 32.8 mA cm -2 The overpotential is 510 mV, and has high durability. However, the electrocatalytic performance of the Electrode material prepared by the method has larger promotion space (Lin Y-X, Feng W-J, Zhang J-J, et al A Polyimide Nanolayer as a Metal-Free and Dual Organic Electrode heated high efficiency Oxygen Evolution [ J Y-X)]Angewandte Chemie International Edition, 2018, 57(38): 12563-. Hu and other phytic acid doped polypyrrole form a porous and conductive hydrogel, show good activity on OER and are 10 mA cm -2 The overpotential is 340 mV, the Tafel slope is 54.9 mV dec -1 And is combined withAnd has long-term stability of up to 20 hours, exceeding that of most metal-free electrocatalysts. However, the material prepared by the experiment has higher overpotential under higher current density, and can be further improved (Hu Q, Li G, Liu X, et al. Superhydrophic polymeric-Acid-Doped Conductive Hydrogels as Metal-Free and Binder-Free electrolytes for Efficient Water Oxidation [ J Q, G, Li, X, J, C]Angewandte Chemie International Edition, 2019, 58(13): 4318-. Hu and the like prepare a two-dimensional N and S co-doped graphite sheet which has a unique hierarchical structure consisting of three-dimensional holes, and the sheet is proved to be an efficient three-function ORR/OER/HER catalyst based on the unique structure, the large surface area, the rich active sites and the good electron/electrolyte transport performance, and has excellent electrocatalytic activity and stability. However, the experimental preparation process is complicated and needs to be improved (Hu C, Dai L. Multifunctional Carbon-Based Metal-Free electrolytes for Simultaneous Oxygen Reduction, Oxygen Evolution, and Hydrogen Evolution [ J]. Advanced Materials, 2017, 29(9): 1604942.）。
Disclosure of Invention
Aiming at the defects of the prior art, the invention adopts an electrostatic spinning method to prepare the high-performance gelatin electrocatalyst.
According to the invention, the method for preparing the high-performance gelatin electrocatalyst by the electrostatic spinning method comprises the following steps:
(1) weighing 1-3 g of gelatin, putting the gelatin into a small beaker filled with 7-9 mL of deionized water, and stirring for 0.5 h in a constant-temperature water bath kettle at 50 ℃ until the gelatin is completely dissolved;
(2) starting electrostatic spinning equipment, and setting the temperature to be 30-40 ℃; the applied voltage is 17-20 kV; the flow velocity is 0.5-1 mm/min and the distance from the tip to the collector is 12 cm, and a sample sprayed by the electrostatic spinning equipment is directly sprayed and coated on the treated carbon cloth;
(3) putting the product obtained in the step (2) into a crucible, and carrying out carbonization treatment by adopting a tube furnace under the conditions that: and (3) carrying out heat preservation for 1-3 h under the argon atmosphere and at the carbonization temperature of 250-500 ℃, wherein the heating rate is 5 ℃/min.
According to the present invention, it is preferable that the gelatin mass in the step (1) is 1.5 g.
According to the present invention, it is preferred that the amount of deionized water used in step (1) is 8.5 mL.
According to the present invention, it is preferred that the temperature of the apparatus in the step (2) is 40 ℃.
According to the present invention, it is preferable that the applied voltage in the step (2) is 18 kV.
According to the present invention, it is preferred that the flow rate in step (2) is 0.7 mm/min.
According to the present invention, it is preferable that the carbonization temperature in the step (3) is 300 ℃.
According to the present invention, it is preferable that the incubation time in the step (3) is 3 hours.
The technical advantages of the invention are as follows:
(1) the preparation method is simple in preparation process, easy to operate and short in time consumption.
(2) The gelatin fiber prepared by the invention has excellent electrochemical performance and stable structure, and has the current density of 10 mA cm -2 The overpotential is only 376.5 mV, which is superior to the reported carbon-based metal-free electrocatalyst.
Drawings
FIG. 1 is a scanning electron microscope image of a gelatin fiber electrocatalyst prepared in example 1 of the present invention.
FIG. 2 is a linear cyclic voltammogram of the gelatin fiber electrocatalyst prepared in example 1 of the present invention.
Detailed Description
The present invention will be further described with reference to the following embodiments and drawings, but is not limited thereto.
Meanwhile, the experimental methods described in the following examples are all conventional methods unless otherwise specified; the reagents and materials are commercially available, unless otherwise specified.
Example 1:
weighing 1.5 g of gelatin, putting the gelatin into a small beaker filled with 8.5 mL of deionized water, and stirring the gelatin in a constant-temperature water bath kettle at 50 ℃ for 0.5 h until the gelatin is completely dissolved; starting electrostatic spinning equipment, and setting the temperature to be 40 ℃; the applied voltage was 18 kV; the flow rate was 0.7 mm/min and the tip-to-collector distance was 12 cm, and the sample sprayed from the electrospinning device was directly sprayed on the carbon cloth which had been treated. Placing the obtained product in a crucible, and carrying out carbonization treatment by adopting a tube furnace under the conditions that: and (3) keeping the temperature for 3 h under the argon atmosphere and at the carbonization temperature of 300 ℃, wherein the heating rate is 5 ℃/min.
Adopting a three-electrode system, in 1 mol/L KOH electrolyte, the sweep rate is 2 mV s -1 Linear cyclic voltammetry tests were performed under conditions.
The scanning electron microscope image of the gelatin fiber electrocatalyst prepared in this example is shown in fig. 1, and it can be seen from fig. 1 that the gelatin fiber after the test is relatively uniform.
The linear cyclic voltammogram of the gelatin fiber electrocatalyst prepared in this example is shown in FIG. 2, and it can be seen from FIG. 2 that the current density is 10 mA cm -2 The overpotential is only 376.5 mV, which shows that the catalyst performance in this example is excellent.
Example 2:
weighing 1 g of gelatin, placing the gelatin in a small beaker filled with 9 mL of deionized water, and stirring the gelatin in a constant-temperature water bath kettle at 50 ℃ for 0.5 h until the gelatin is completely dissolved; starting electrostatic spinning equipment, and setting the temperature to be 40 ℃; the applied voltage was 18 kV; the flow rate was 0.7 mm/min and the tip-to-collector distance was 12 cm, and the sample sprayed from the electrospinning device was directly sprayed on the carbon cloth which had been treated. Placing the obtained product in a crucible, and carrying out carbonization treatment by adopting a tube furnace under the conditions that: and (3) keeping the temperature for 3 h under the argon atmosphere and at the carbonization temperature of 300 ℃, wherein the heating rate is 5 ℃/min.
Adopting a three-electrode system, in 1 mol/L KOH electrolyte, the sweep rate is 2 mV s -1 Linear cyclic voltammetry tests were performed under conditions.
Example 3:
weighing 1.5 g of gelatin, putting the gelatin into a small beaker filled with 8.5 mL of deionized water, and stirring the gelatin in a constant-temperature water bath kettle at 50 ℃ for 0.5 h until the gelatin is completely dissolved; starting electrostatic spinning equipment, and setting the temperature to be 35 ℃; the applied voltage was 19 kV; the flow rate was 1 mm/min and the tip-to-collector distance was 12 cm, and the sample sprayed from the electrospinning apparatus was directly sprayed onto the treated carbon cloth. Placing the obtained product in a crucible, and carrying out carbonization treatment by adopting a tube furnace under the conditions that: in argon atmosphere, the carbonization temperature is 400 ℃, the temperature is kept for 1 h, and the heating rate is 5 ℃/min.
Adopting a three-electrode system, in 1 mol/L KOH electrolyte, the sweep rate is 2 mV s -1 Linear cyclic voltammetry tests were performed under conditions.
Example 4:
weighing 1.5 g of gelatin, putting the gelatin into a small beaker filled with 8.5 mL of deionized water, and stirring the gelatin in a constant-temperature water bath kettle at 50 ℃ for 0.5 h until the gelatin is completely dissolved; starting electrostatic spinning equipment, and setting the temperature to be 30 ℃; the applied voltage was 19 kV; the flow rate was 0.5 mm/min and the tip-to-collector distance was 12 cm, and the sample sprayed from the electrospinning device was directly sprayed on the treated carbon cloth. Placing the obtained product in a crucible, and carrying out carbonization treatment by adopting a tube furnace under the conditions that: and (3) keeping the temperature for 3 h under the argon atmosphere and at the carbonization temperature of 250 ℃, wherein the heating rate is 5 ℃/min.
Adopting a three-electrode system, in 1 mol/L KOH electrolyte, the sweep rate is 2 mV s -1 Linear cyclic voltammetry tests were performed under conditions.
Example 5:
weighing 1.5 g of gelatin, putting the gelatin into a small beaker filled with 8.5 mL of deionized water, and stirring the gelatin in a constant-temperature water bath kettle at 50 ℃ for 0.5 h until the gelatin is completely dissolved; starting electrostatic spinning equipment, and setting the temperature to be 40 ℃; the applied voltage was 18 kV; the flow rate was 0.7 mm/min and the tip-to-collector distance was 12 cm, and the sample sprayed from the electrospinning device was directly sprayed on the carbon cloth which had been treated. Placing the obtained product in a crucible, and carrying out carbonization treatment by adopting a tube furnace under the conditions that: in the argon atmosphere, the carbonization temperature is 400 ℃, the heat preservation is carried out for 2.5 h, and the heating rate is 5 ℃/min.
Adopting a three-electrode system, in 1 mol/L KOH electrolyte, the sweep rate is 2 mV s -1 Linear cyclic voltammetry tests were performed under conditions.
Claims (9)
1. According to the invention, the method for preparing the high-performance gelatin electrocatalyst by the electrostatic spinning method, which comprises the following steps:
(1) weighing 1-3 g of gelatin, putting the gelatin into a small beaker filled with 7-9 mL of deionized water, and stirring for 0.5 h in a constant-temperature water bath kettle at 50 ℃ until the gelatin is completely dissolved;
(2) starting electrostatic spinning equipment, and setting the temperature to be 30-40 ℃; the applied voltage is 17-20 kV; the flow rate is 0.5-1 mm/min, the distance from the tip to the collector is 12 cm, and a sample sprayed by electrostatic spinning equipment is directly sprayed on the treated carbon cloth;
(3) putting the product obtained in the step (2) into a crucible, and carrying out carbonization treatment by adopting a tube furnace under the conditions that: and (3) carrying out heat preservation for 1-3 h under the argon atmosphere and at the carbonization temperature of 250-500 ℃, wherein the heating rate is 5 ℃/min.
2. The manufactured gelatin fiber electrocatalyst according to claim 1, wherein the mass of gelatin in step (1) is 1.5 g.
3. The method for preparing gelatin fiber electrocatalyst according to claim 1, wherein the amount of deionized water used in step (1) is 8.5 mL.
4. The gelatin fiber-producing electrocatalyst according to claim 1, wherein the apparatus temperature in step (2) is 40 ℃.
5. The method for preparing gelatin fiber electrocatalyst according to claim 1, wherein the applied voltage in step (2) is 18 kV.
6. The method for preparing gelatin fiber electrocatalyst according to claim 1, wherein the flow rate in step (2) is 0.7 mm/min.
7. The gelatin fiber electrocatalyst for preparation according to claim 1, wherein the carbonization temperature in step (3) is 300 ℃.
8. The method for preparing gelatin fiber electrocatalyst according to claim 1, wherein the incubation time in step (3) is 3 h.
9. An electrostatic spinning method for preparing high-performance gelatin electrocatalyst.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111593761 | 2021-12-24 | ||
| CN2021115937619 | 2021-12-24 |
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| CN114807999A true CN114807999A (en) | 2022-07-29 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004330181A (en) * | 2003-04-17 | 2004-11-25 | Sony Corp | Catalyst, its production method and electrochemical device |
| US20060263674A1 (en) * | 2003-04-17 | 2006-11-23 | Mamoru Hosoya | Catalyst and process for producing the same, catalytic electrode and process for producing the same, membrane/electrode union, and electrochemical device |
| CN112301464A (en) * | 2020-09-30 | 2021-02-02 | 北京化工大学 | Gelatin-based carbon nanofiber and preparation method thereof |
| CN112695341A (en) * | 2020-12-24 | 2021-04-23 | 齐鲁工业大学 | Preparation and application of gelatin-based transition metal oxide material |
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2022
- 2022-04-15 CN CN202210394603.9A patent/CN114807999A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004330181A (en) * | 2003-04-17 | 2004-11-25 | Sony Corp | Catalyst, its production method and electrochemical device |
| US20060263674A1 (en) * | 2003-04-17 | 2006-11-23 | Mamoru Hosoya | Catalyst and process for producing the same, catalytic electrode and process for producing the same, membrane/electrode union, and electrochemical device |
| CN112301464A (en) * | 2020-09-30 | 2021-02-02 | 北京化工大学 | Gelatin-based carbon nanofiber and preparation method thereof |
| CN112695341A (en) * | 2020-12-24 | 2021-04-23 | 齐鲁工业大学 | Preparation and application of gelatin-based transition metal oxide material |
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Application publication date: 20220729 |