CN112624110A - Layered porous carbon material prepared by freeze-drying auxiliary template method and preparation and application thereof - Google Patents
Layered porous carbon material prepared by freeze-drying auxiliary template method and preparation and application thereof Download PDFInfo
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- 239000003575 carbonaceous material Substances 0.000 title claims abstract description 69
- 238000000034 method Methods 0.000 title claims abstract description 58
- 238000004108 freeze drying Methods 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title abstract description 9
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims abstract description 47
- 235000010413 sodium alginate Nutrition 0.000 claims abstract description 47
- 229940005550 sodium alginate Drugs 0.000 claims abstract description 47
- 239000000661 sodium alginate Substances 0.000 claims abstract description 47
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 41
- 238000003756 stirring Methods 0.000 claims abstract description 38
- 238000009656 pre-carbonization Methods 0.000 claims abstract description 27
- 238000010438 heat treatment Methods 0.000 claims abstract description 18
- 150000003751 zinc Chemical class 0.000 claims abstract description 17
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 30
- 229910052799 carbon Inorganic materials 0.000 claims description 26
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 24
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical group [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 22
- 239000004246 zinc acetate Substances 0.000 claims description 22
- 238000003763 carbonization Methods 0.000 claims description 17
- 239000007788 liquid Substances 0.000 claims description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims description 12
- 238000001994 activation Methods 0.000 claims description 9
- 230000008569 process Effects 0.000 claims description 9
- 230000004913 activation Effects 0.000 claims description 5
- 238000007710 freezing Methods 0.000 claims description 5
- 230000008014 freezing Effects 0.000 claims description 5
- 230000003213 activating effect Effects 0.000 abstract description 23
- 238000010000 carbonizing Methods 0.000 abstract description 8
- 239000002028 Biomass Substances 0.000 abstract description 7
- 238000012986 modification Methods 0.000 abstract description 4
- 230000004048 modification Effects 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 3
- 239000003795 chemical substances by application Substances 0.000 description 15
- 239000008367 deionised water Substances 0.000 description 14
- 229910021641 deionized water Inorganic materials 0.000 description 14
- 239000000843 powder Substances 0.000 description 14
- 239000003990 capacitor Substances 0.000 description 7
- 150000002500 ions Chemical class 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 239000007772 electrode material Substances 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 238000003760 magnetic stirring Methods 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 241001474374 Blennius Species 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 229910021607 Silver chloride Inorganic materials 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 239000012190 activator Substances 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229920001940 conductive polymer Polymers 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 1
- 150000003623 transition metal compounds Chemical class 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
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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
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/342—Preparation characterised by non-gaseous activating agents
- C01B32/348—Metallic compounds
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/318—Preparation characterised by the starting materials
Abstract
The invention relates to a layered porous carbon material prepared by a freeze-drying auxiliary template method, and preparation and application thereof, wherein the preparation method comprises the following steps: 1) dissolving sodium alginate in water, stirring and heating to obtain a sodium alginate solution; 2) dripping a zinc salt water solution into a sodium alginate solution, and stirring to obtain a gel; 3) freeze-drying the gel in the step 2), crushing, and performing pre-carbonization treatment to obtain a pre-carbonization product; 4) carbonizing and activating the pre-carbonized product at high temperature to obtain a layered porous carbon material; layered porous carbon materials are used in supercapacitors. Compared with the prior art, the preparation process of the carbon material is simple, the prepared biomass-based carbon material has a layered porous structure, the subsequent modification and other operations are convenient, and the raw material sodium alginate has rich sources, low price and wide application prospect.
Description
Technical Field
The invention belongs to the technical field of carbon materials, and relates to a layered porous carbon material prepared by a freeze-drying auxiliary template method, and preparation and application thereof.
Background
With the increasing exhaustion of fossil energy, global warming and environmental pollution, researchers in all countries around the world are not only dedicated to developing renewable clean energy sources, such as solar energy, wind energy, tidal energy, etc., but also dedicated to developing low-cost, high-performance energy storage devices. The biomass resources are various in types, wide in distribution, extremely rich in reserves and low in price, are very important renewable resources, and can achieve the purpose of sustainable circulation by utilizing and developing the biomass resources. Meanwhile, the biomass is a carrier of naturally existing renewable carbon elements, is converted into a novel functional carbon material for utilization, and has a great development space.
Super capacitors, as a class of high efficiency energy storage devices, can provide high power density and excellent cycling stability, have the potential to evolve to approach the energy density of conventional batteries, and thus have attracted considerable attention. The electrode material is one of the key factors influencing the electrochemical performance of the super capacitor, and the following three types are mainly adopted: carbon materials, transition metal compounds, and conductive polymers. Among them, the porous carbon material, especially activated carbon, is the most widely used electrode material because of its characteristics of good chemical stability, light weight, low cost, high electrical conductivity, and environmental friendliness. The developed micropore or mesoporous pore canal and the ultra-high specific surface area of the activated carbon not only accelerate the dynamic process of ion migration, but also can provide rich surface active potential, which is important for the high specific capacitance and excellent cycle stability of the super capacitor.
However, the existing process for preparing biomass carbon materials has the problems of insufficient precursor materials, poor material morphology, complex preparation process and the like, and limits further application of the biomass carbon materials.
Disclosure of Invention
The invention aims to provide a layered porous carbon material prepared by a freeze-drying auxiliary template method and preparation and application thereof.
The purpose of the invention can be realized by the following technical scheme:
a method for preparing a layered porous carbon material by a freeze-drying auxiliary template method comprises the following steps:
1) dissolving sodium alginate in water, stirring and heating to obtain a sodium alginate solution;
2) dripping a zinc salt water solution into a sodium alginate solution, and stirring to obtain a gel;
3) freeze-drying the gel in the step 2), crushing, and performing pre-carbonization treatment to obtain a pre-carbonization product;
4) and (3) carrying out high-temperature carbonization and activation on the pre-carbonized product to obtain the layered porous carbon material.
Furthermore, in the step 1), the dosage ratio of the sodium alginate to the water is 2g (50-70) ml.
Further, in the step 1), the temperature is 80-100 ℃ during stirring and heating, and the time is 1-2 h. The stirring is preferably magnetic stirring.
Further, in the step 2), the zinc salt is zinc acetate; in the zinc salt water solution, the dosage ratio of zinc acetate to water is (3-3.5) g:20 ml; the mass ratio of the zinc acetate to the sodium alginate is (3-3.5) to 2.
Further, in the step 2), the stirring time is 0.5-1.5 h. The stirring is preferably magnetic stirring.
Further, in step 3), pre-freezing with liquid nitrogen is performed before lyophilization.
Further, in the step 3), the temperature is 450-550 ℃ and the time is 1.5-2.5h in the carbon pretreatment process.
Further, in the step 4), the temperature is 500-800 ℃ in the high-temperature carbonization activation process, the time is 1.5-2.5h, the activating agent is KOH, and the mass ratio of the pre-carbon product to the activating agent is 1 (1-2).
The layered porous carbon material is prepared by the freeze-drying auxiliary template method.
The application of the layered porous carbon material prepared by the freeze-drying auxiliary template method is that the layered porous carbon material is used in a super capacitor.
Sodium alginate is a water-soluble polysaccharide extracted from seaweed, has abundant carboxyl and hydroxyl, and is a natural renewable resource. The invention adopts sodium alginate as the raw material, has rich sources, low price and higher carbon content, and is an environment-friendly material which completely meets the requirement of green chemistry.
In the invention, carboxyl and hydroxyl contained in sodium alginate can be coordinated with metal ions in a zinc salt template, during carbonization, carbon matrix is naturally converted into carbon-containing substances, and the metal ions are converted into corresponding carbonate or oxide. The pore size of the carbon material is controlled by the template generated by in-situ pyrolysis through a high-temperature calcination method, and the derived mesopores provide a channel for accelerating ion transfer in an electrochemical process. KOH as an activator can create numerous micropores while introducing oxygen atoms.
Compared with the prior art, the preparation process of the carbon material is simple, the prepared biomass-based carbon material has a layered porous structure, the subsequent modification and other operations are convenient, and the raw material sodium alginate has rich sources, low price and wide application prospect.
Drawings
FIG. 1 is a TEM image of a layered porous carbon material prepared in example 1;
FIG. 2 shows the concentration of 10 mV. multidot.s of the layered porous carbon material prepared in example 1-1A CV curve of (a);
FIG. 3 shows the results of the measurement of the concentration of 0.5A g in the layered porous carbon material prepared in example 1-1GCD graph of (a).
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments. The present embodiment is implemented on the premise of the technical solution of the present invention, and a detailed implementation manner and a specific operation process are given, but the scope of the present invention is not limited to the following embodiments.
Example 1:
the method for preparing the layered porous carbon material by the freeze-drying auxiliary template method specifically comprises the following steps:
1) slowly dissolving 2g of sodium alginate powder in 60ml of deionized water, continuously stirring and heating to form a solution, wherein the temperature is 80 ℃, and the time is 2 hours;
2) adding 3.14g of zinc acetate into 20ml of deionized water, slowly dropping sodium alginate solution to form gel, and continuously stirring for 1 h;
3) crushing the gel freeze-dried powder in the step 2), and then carrying out pre-carbonization treatment, wherein liquid nitrogen is used for treatment before freeze-drying, the pre-carbonization temperature is 500 ℃, and the time is 2 hours;
4) carbonizing and activating the pre-carbon product in the step 3) at high temperature, wherein the mass ratio of the pre-carbon product to an activating agent KOH is 1:1, the carbonization temperature is 600 ℃, and the time is 2 hours, so as to obtain the layered porous carbon material.
The obtained layered porous carbon material was characterized, and the results are shown in fig. 1. As can be seen from fig. 1, the carbon material is in the form of a sheet and forms a large number of pore structures that facilitate ion transfer.
The electrochemical performance test of the prepared layered porous carbon material is carried out, and the process is as follows:
and (3) carrying out electrochemical performance test on the prepared layered porous carbon material in a three-electrode system by adopting an electrochemical workstation. The working electrode is a layered porous carbon material, the counter electrode is a platinum wire electrode, and the reference electrode is an Ag/AgCl electrode. The CV curve and the GCD curve were measured using 6M KOH solution as the electrolyte, and are shown in FIGS. 2 and 3, respectively. As can be seen from fig. 2, the layered porous carbon material has a closed curve close to a rectangle, and has a large specific gravity capacitance. As can be seen from FIG. 3, the current density was 0.5 A.g-1When the carbon dioxide is used, the GCD curve of the sample shows an approximately symmetrical triangle, which proves that the layered porous carbon material has good electrochemical reversibility and coulombic efficiency.
Example 2:
the method for preparing the layered porous carbon material by the freeze-drying auxiliary template method specifically comprises the following steps:
1) slowly dissolving 2g of sodium alginate powder in 60ml of deionized water, continuously stirring and heating to form a solution, wherein the temperature is 850 ℃, and the time is 2 hours;
2) adding 3.14g of zinc acetate into 20ml of deionized water, slowly dropping sodium alginate solution to form gel, and continuously stirring for 1 h;
3) crushing the gel freeze-dried powder in the step 2), and then carrying out pre-carbonization treatment, wherein liquid nitrogen is used for treatment before freeze-drying, the pre-carbonization temperature is 500 ℃, and the time is 2 hours;
4) carbonizing and activating the pre-carbon product in the step 3) at high temperature, wherein the mass ratio of the pre-carbon product to an activating agent KOH is 1:1, the carbonization temperature is 600 ℃, and the time is 3 hours, so as to obtain the layered porous carbon material.
Example 3:
the method for preparing the layered porous carbon material by the freeze-drying auxiliary template method specifically comprises the following steps:
1) slowly dissolving 2g of sodium alginate powder in 60ml of deionized water, continuously stirring and heating to form a solution, wherein the temperature is 90 ℃, and the time is 1 h;
2) adding 3.14g of zinc acetate into 20ml of deionized water, slowly dropping sodium alginate solution to form gel, and continuously stirring for 1 h;
3) crushing the gel freeze-dried powder in the step 2), and then carrying out pre-carbonization treatment, wherein liquid nitrogen is used for treatment before freeze-drying, the pre-carbonization temperature is 500 ℃, and the time is 2 hours;
4) carbonizing and activating the pre-carbon product in the step 3) at high temperature, wherein the mass ratio of the pre-carbon product to an activating agent KOH is 1:2, the carbonization temperature is 700 ℃, and the time is 2 hours, so as to obtain the layered porous carbon material.
Example 4:
the method for preparing the layered porous carbon material by the freeze-drying auxiliary template method specifically comprises the following steps:
1) slowly dissolving 2g of sodium alginate powder in 60ml of deionized water, continuously stirring and heating to form a solution, wherein the temperature is 90 ℃, and the time is 2 hours;
2) adding 3.14g of zinc acetate into 20ml of deionized water, slowly dropping sodium alginate solution to form gel, and continuously stirring for 1 h;
3) crushing the gel freeze-dried powder in the step 2), and then carrying out pre-carbonization treatment, wherein liquid nitrogen is used for treatment before freeze-drying, the pre-carbonization temperature is 500 ℃, and the time is 2 hours;
4) carbonizing and activating the pre-carbon product in the step 3) at high temperature, wherein the mass ratio of the pre-carbon product to an activating agent KOH is 1:2, the carbonization temperature is 600 ℃, and the time is 2 hours, so as to obtain the layered porous carbon material.
Example 5:
the method for preparing the layered porous carbon material by the freeze-drying auxiliary template method specifically comprises the following steps:
1) slowly dissolving 2g of sodium alginate powder in 60ml of deionized water, continuously stirring and heating to form a solution, wherein the temperature is 90 ℃, and the time is 1 h;
2) adding 3.14g of zinc acetate into 20ml of deionized water, slowly dropping sodium alginate solution to form gel, and continuously stirring for 1 h;
3) crushing the gel freeze-dried powder in the step 2), and then carrying out pre-carbonization treatment, wherein liquid nitrogen is used for treatment before freeze-drying, the pre-carbonization temperature is 500 ℃, and the time is 2 hours;
4) carbonizing and activating the pre-carbon product in the step 3) at high temperature, wherein the mass ratio of the pre-carbon product to an activating agent KOH is 1:1, the carbonization temperature is 800 ℃, and the time is 2 hours, so as to obtain the layered porous carbon material.
Example 6:
the method for preparing the layered porous carbon material by the freeze-drying auxiliary template method specifically comprises the following steps:
1) slowly dissolving 2g of sodium alginate powder in 60ml of deionized water, continuously stirring and heating to form a solution, wherein the temperature is 95 ℃, and the time is 2 hours;
2) adding 3.14g of zinc acetate into 20ml of deionized water, slowly dropping sodium alginate solution to form gel, and continuously stirring for 1 h;
3) crushing the gel freeze-dried powder in the step 2), and then carrying out pre-carbonization treatment, wherein liquid nitrogen is used for treatment before freeze-drying, the pre-carbonization temperature is 500 ℃, and the time is 2 hours;
4) carbonizing and activating the pre-carbon product in the step 3) at high temperature, wherein the mass ratio of the pre-carbon product to an activating agent KOH is 1:1, the carbonization temperature is 800 ℃, and the time is 3 hours, so as to obtain the layered porous carbon material.
Example 7:
the method for preparing the layered porous carbon material by the freeze-drying auxiliary template method specifically comprises the following steps:
1) slowly dissolving 2g of sodium alginate powder in 60ml of deionized water, continuously stirring and heating to form a solution, wherein the temperature is 100 ℃, and the time is 1 h;
2) adding 3.14g of zinc acetate into 20ml of deionized water, slowly dropping sodium alginate solution to form gel, and continuously stirring for 1 h;
3) crushing the gel freeze-dried powder in the step 2), and then carrying out pre-carbonization treatment, wherein liquid nitrogen is used for treatment before freeze-drying, the pre-carbonization temperature is 500 ℃, and the time is 2 hours;
4) carbonizing and activating the pre-carbon product in the step 3) at high temperature, wherein the mass ratio of the pre-carbon product to an activating agent KOH is 1:2, the carbonization temperature is 800 ℃, and the time is 2 hours, so as to obtain the layered porous carbon material.
Example 8:
a method for preparing a layered porous carbon material by a freeze-drying auxiliary template method comprises the following steps:
1) dissolving sodium alginate in water, stirring and heating to obtain a sodium alginate solution;
2) dripping a zinc salt water solution into a sodium alginate solution, and stirring to obtain a gel;
3) freeze-drying the gel in the step 2), crushing, and performing pre-carbonization treatment to obtain a pre-carbonization product;
4) and (4) carrying out high-temperature carbonization and activation on the pre-carbonized product to obtain the layered porous carbon material.
In the step 1), the dosage ratio of sodium alginate to water is 2g to 50 ml. The temperature is 100 ℃ during the stirring and heating process, and the time is 1 h.
In the step 2), the zinc salt is zinc acetate; in the zinc salt water solution, the dosage ratio of zinc acetate to water is 3.5g to 20 ml; the mass ratio of the zinc acetate to the sodium alginate is 3: 2. The stirring time was 1.5 h.
In step 3), pre-freezing with liquid nitrogen before freeze-drying. In the process of the pre-carbon treatment, the temperature is 450 ℃ and the time is 2.5 h.
In the step 4), in the high-temperature carbonization and activation process, the temperature is 500 ℃, the time is 2.5 hours, the activating agent is KOH, and the mass ratio of the pre-carbon product to the activating agent is 1:1.
The prepared layered porous carbon material is used in a super capacitor.
Example 9:
a method for preparing a layered porous carbon material by a freeze-drying auxiliary template method comprises the following steps:
1) dissolving sodium alginate in water, stirring and heating to obtain a sodium alginate solution;
2) dripping a zinc salt water solution into a sodium alginate solution, and stirring to obtain a gel;
3) freeze-drying the gel in the step 2), crushing, and performing pre-carbonization treatment to obtain a pre-carbonization product;
4) and (4) carrying out high-temperature carbonization and activation on the pre-carbonized product to obtain the layered porous carbon material.
In the step 1), the dosage ratio of sodium alginate to water is 2g to 70 ml. The temperature is 80 ℃ during the stirring and heating process, and the time is 2 h.
In the step 2), the zinc salt is zinc acetate; in the zinc salt water solution, the dosage ratio of zinc acetate to water is 3g to 20 ml; the mass ratio of the zinc acetate to the sodium alginate is 3.5: 2. The stirring time was 0.5 h.
In step 3), pre-freezing with liquid nitrogen before freeze-drying. In the process of the pre-carbon treatment, the temperature is 550 ℃ and the time is 1.5 h.
In the step 4), in the high-temperature carbonization and activation process, the temperature is 800 ℃, the time is 1.5h, the activating agent is KOH, and the mass ratio of the pre-carbon product to the activating agent is 1: 2.
The prepared layered porous carbon material is used in a super capacitor.
Example 10:
a method for preparing a layered porous carbon material by a freeze-drying auxiliary template method comprises the following steps:
1) dissolving sodium alginate in water, stirring and heating to obtain a sodium alginate solution;
2) dripping a zinc salt water solution into a sodium alginate solution, and stirring to obtain a gel;
3) freeze-drying the gel in the step 2), crushing, and performing pre-carbonization treatment to obtain a pre-carbonization product;
4) and (4) carrying out high-temperature carbonization and activation on the pre-carbonized product to obtain the layered porous carbon material.
In the step 1), the dosage ratio of sodium alginate to water is 2g to 60 ml. The temperature is 90 ℃ during the stirring and heating process, and the time is 1.5 h.
In the step 2), the zinc salt is zinc acetate; in the zinc salt water solution, the dosage ratio of zinc acetate to water is 3.2g to 20 ml; the mass ratio of the zinc acetate to the sodium alginate is 3.2: 2. The stirring time was 1 h.
In step 3), pre-freezing with liquid nitrogen before freeze-drying. In the process of the pre-carbonization, the temperature is 500 ℃ and the time is 2 h.
In the step 4), in the high-temperature carbonization and activation process, the temperature is 650 ℃, the time is 2 hours, the activating agent is KOH, and the mass ratio of the pre-carbon product to the activating agent is 1: 1.5.
The prepared layered porous carbon material is used in a super capacitor.
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (10)
1. The method for preparing the layered porous carbon material by the freeze-drying auxiliary template method is characterized by comprising the following steps of:
1) dissolving sodium alginate in water, stirring and heating to obtain a sodium alginate solution;
2) dripping a zinc salt water solution into a sodium alginate solution, and stirring to obtain a gel;
3) freeze-drying the gel in the step 2), crushing, and performing pre-carbonization treatment to obtain a pre-carbonization product;
4) and (3) carrying out high-temperature carbonization and activation on the pre-carbonized product to obtain the layered porous carbon material.
2. The method for preparing the layered porous carbon material by the freeze-drying auxiliary template method according to claim 1, wherein in the step 1), the dosage ratio of the sodium alginate to the water is 2g (50-70) ml.
3. The method for preparing the layered porous carbon material by the freeze-drying assisted template method according to claim 1, wherein in the step 1), the temperature is 80-100 ℃ and the time is 1-2h during the stirring and heating process.
4. The method for preparing the layered porous carbon material by the freeze-drying assisted template method according to claim 1, wherein in the step 2), the zinc salt is zinc acetate; in the zinc salt water solution, the dosage ratio of zinc acetate to water is (3-3.5) g:20 ml; the mass ratio of the zinc acetate to the sodium alginate is (3-3.5) to 2.
5. The method for preparing the layered porous carbon material by the freeze-drying assisted template method according to claim 1, wherein in the step 2), the stirring time is 0.5-1.5 h.
6. The method for preparing a layered porous carbon material by freeze-drying assisted template method according to claim 1, wherein in step 3), liquid nitrogen is used for pre-freezing before freeze-drying.
7. The method for preparing a layered porous carbon material by using a freeze-drying auxiliary template method as claimed in claim 1, wherein the temperature is 450-550 ℃ and the time is 1.5-2.5h in the pre-carbon treatment process in the step 3).
8. The method for preparing the layered porous carbon material by the freeze-drying auxiliary template method as claimed in claim 1, wherein in the step 4), the temperature is 500-.
9. A layered porous carbon material prepared by a freeze-drying assisted template method, characterized in that the layered porous carbon material is prepared by the method of any one of claims 1 to 8.
10. The use of the layered porous carbon material prepared by freeze-drying assisted template method according to claim 9, wherein the layered porous carbon material is used in a supercapacitor.
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| CN110556546A (en) * | 2019-09-03 | 2019-12-10 | 武汉工程大学 | Nitrogen and oxygen co-doped hierarchical porous carbon material and preparation method thereof |
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2021
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