CN111204755A - Preparation method and application of biomass porous carbon material - Google Patents
Preparation method and application of biomass porous carbon material Download PDFInfo
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- CN111204755A CN111204755A CN202010106182.6A CN202010106182A CN111204755A CN 111204755 A CN111204755 A CN 111204755A CN 202010106182 A CN202010106182 A CN 202010106182A CN 111204755 A CN111204755 A CN 111204755A
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/469—Treatment of water, waste water, or sewage by electrochemical methods by electrochemical separation, e.g. by electro-osmosis, electrodialysis, electrophoresis
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/08—Seawater, e.g. for desalination
Abstract
The invention relates to a biomass porous carbon and a preparation method thereof, wherein the preparation method comprises the following steps: s1, carrying out dry grinding on the biomass, the zinc chloride, the ammonium bicarbonate, the ammonium chloride and the potassium ferrate, and uniformly mixing; s2, carbonizing the mixture obtained in the step S1 for 2 hours at 850 ℃ in a protective gas atmosphere, and cooling to room temperature to obtain a carbon material; s3, acid washing, deionized water cleaning and drying are carried out on the obtained carbon material, the method is cheap and environment-friendly, the prepared porous carbon material has good pore structure and electrochemical performance, and experiments in desalination show that the material has great application value in the field of seawater desalination.
Description
Technical Field
The invention relates to a biomass porous carbon and a preparation method thereof, belonging to the technical field of carbon materials.
Background
At present, carbon materials are widely used in the fields of adsorbents, catalysts, electrode materials for fuel cells and secondary batteries, supercapacitors, composite materials, gas sensors, solar cells, various electronic devices, and the like due to their excellent porous properties.
The carbon material is a material taking carbon as a main element as the name implies, mainly comprises graphite, carbon black, activated carbon, carbon fiber, carbon nano tube and the like, the structure, the composition and the properties of the carbon material directly determine the overall performance, the application and the price of the carbon material, and the development and the utilization of the non-renewable resources with limited resources are limited. In recent years, more and more people have focused on research and development of a carbon material with sufficient source and excellent performance, renewable biomass resources become an ideal carbon source, and the obtained carbon material is mainly determined by an activation treatment process.
At present, commonly used activating agents are potassium hydroxide, potassium carbonate, sulfuric acid or zinc chloride, the obtained carbon material has poor conductivity, and in order to overcome the defects, CN107265436A discloses a preparation method of a biomass graphitized porous carbon material, wherein biomass is used as a raw material, potassium ferrate is used as a pore-forming agent and a catalyst, the biomass graphitized porous carbon material is obtained, and the specific surface area is 1000-2000 m2A higher degree of graphitization, but a lower surface area, limits its application.
In view of the above, a method for improving the performance of a carbon material is needed to meet the requirements of the high-demand field.
Disclosure of Invention
The invention aims to overcome the defects in the prior art, provides a preparation method of biomass porous carbon with large specific surface area, high adsorption performance and high conductivity, and simultaneously provides application of the biomass porous carbon.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
subject of the technology 1
A biomass porous carbon and a preparation method thereof comprise the following steps:
s1: carrying out dry grinding on the biomass, zinc chloride, ammonium bicarbonate, ammonium chloride and potassium ferrate, and uniformly mixing;
s2: carbonizing the mixture obtained in the step S1 at 750-950 ℃ for 1-3 h in a protective gas atmosphere, and cooling to room temperature to obtain a carbon material;
s3: and (3) carrying out acid washing and deionized water cleaning on the obtained carbon material, and drying to obtain the carbon material.
In some embodiments of the invention, the biomass, zinc chloride, ammonium bicarbonate, ammonium chloride, and potassium ferrate are selected from the group consisting ofMeasurement ofThe ratio is 1: 0.5-1.5: 0.5-2: 1-3: 1-2.5.
In some embodiments of the invention, the mass ratio of the biomass, zinc chloride, ammonium bicarbonate, ammonium chloride and potassium ferrate is 1:1:1:1: 1.
In some embodiments of the invention, the biomass is selected from one or a combination of any two or more of chitin, lignin or cellulose.
In some embodiments of the invention, the biomass is selected from chitin.
In some embodiments of the invention, the dry milling is dry ball milling, the mass ratio of the milling balls to the total mass of the biomass, the zinc chloride, the ammonium bicarbonate, the ammonium chloride and the potassium ferrate is 1: 4-6, the diameter of the milling balls is 0.5 mm-10 mm, the rotating speed is 250-600 r/min, and the milling time is 1-5 h.
In some embodiments of the invention, the ratio of the mass of the milling balls to the total mass of the biomass, zinc chloride, ammonium bicarbonate, ammonium chloride and potassium ferrate is 1:5, the milling balls have a diameter of 3mm, a rotation speed of 450 r/min and a milling time of 3 h.
In some embodiments of the present invention, the step S2 specifically includes: continuously introducing protective gas at the speed of 15-40 mL/min, heating to 280-320 ℃ from room temperature at the speed of 1.2-1.8 ℃/min, then heating to 750-950 ℃ at the speed of 2-2.2 ℃/min, keeping for 1-3 hours, and then slowly cooling to room temperature to obtain the black carbon material.
In some embodiments of the invention the shielding gas is selected from nitrogen, helium or carbon dioxide.
In some embodiments of the invention, the hydrochloric acid has a concentration of 5 wt%.
Subject matter two
The application of the biomass porous carbon material obtained by the preparation method provided by the technical subject I in the field of seawater desalination.
In some embodiments of the invention, the application is the preparation of a desalination electrode.
Adopt the produced beneficial effect of above-mentioned technical scheme to lie in:
according to the method provided by the invention, zinc chloride, ammonium bicarbonate, ammonium chloride and potassium ferrate are used at the same time, so that pore-forming can be cooperated and graphitization of the material can be improved, the ammonium chloride and the ammonium bicarbonate can be decomposed at high temperature to generate hydrogen chloride and ammonia gas, and then the hydrogen chloride and the ammonia gas react at high temperature to form ammonium chloride for recycling.
The material obtained by the method provided by the invention has the specific surface area of more than 2000 m by verification2The maximum of the water content can reach 2980m2The specific capacitance can reach more than 200F/g, and can reach more than 320F/g at most. The porous carbon material prepared by the method is used for preparing the desalting electrode, and seawater desalting experiments are carried out, so that the highest sodium chloride adsorption capacity can reach 45 mg/g.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is an electron micrograph of a carbon material according to example 1 of the present invention;
FIG. 2 is a cyclic voltammogram of the carbon material of the electrode in example 1 of the present invention;
FIG. 3 is a graph showing the cyclic charge and discharge at a current density of 6A/g of the carbon material electrode of example 1 of the present invention;
FIG. 4 is a Raman spectrum of the carbon material of example 1 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in detail and fully with reference to the following embodiments.
Example 1
A biomass porous carbon and a preparation method thereof comprise the following steps:
s1: 3g of chitin, 3g of zinc chloride, 3g of ammonium bicarbonate, 3g of ammonium chloride and 3g of potassium ferrate are subjected to ball milling and mixing, the diameter of a milling ball is 3mm, the mass ratio of the milling ball to the total mass ratio of the biomass, the zinc chloride, the ammonium bicarbonate, the ammonium chloride and the potassium ferrate is 1:5, the rotating speed is 400 r/min, the milling is carried out for 3 hours, and the mixing is uniform;
s2: placing the mixture obtained in the step S1 into a high-temperature carbonization furnace, continuously introducing inert protective gas nitrogen at the speed of 25 mL/min, heating to 300 ℃ from room temperature at the speed of 1.5 ℃/min, heating to 850 ℃ at the speed of 2 ℃/min, keeping for 2 hours, and slowly cooling to room temperature to obtain a black carbon material;
s3: and washing the porous carbon material with 5wt% hydrochloric acid solution for three times, washing the porous carbon material with deionized water for three times, and drying to obtain the porous carbon material.
The parameters of the prepared carbon material are as follows: specific surface area 2980m2The specific capacitance is up to 320F/g, and the graphitization degree (I)G) Is 0.98.
The prepared carbon material is observed by a Scanning Electron Microscope (SEM), and the morphology of the carbon material is shown in figure 1, and the carbon material is an obvious three-dimensional porous structure. Cyclic voltammograms and cyclic charge-discharge plots of the prepared carbon materials are shown in fig. 2 and 3, respectively. The prepared carbon material is observed by Raman spectrum, and the graphitization degree of the carbon material is reflected.
Example 2
A biomass porous carbon and a preparation method thereof comprise the following steps:
s1: 3g of lignin, 3g of zinc chloride, 3g of ammonium bicarbonate, 3g of ammonium chloride and 3g of potassium ferrate are subjected to ball milling and mixing, the diameter of a grinding ball is 5mm, the mass ratio of the grinding ball to the total mass of the biomass, the zinc chloride, the ammonium bicarbonate, the ammonium chloride and the potassium ferrate is 1:5.3g, the rotating speed is 400 r/min, the grinding time is 3 hours, and the lignin, the zinc chloride, the ammonium bicarbonate, the ammonium chloride and the potassium ferrate are uniformly mixed;
s2: placing the mixture obtained in the step S1 into a high-temperature carbonization furnace, continuously introducing inert protective gas nitrogen at the speed of 25 mL/min, heating to 300 ℃ from room temperature at the speed of 1.5 ℃/min, heating to 850 ℃ at the speed of 2 ℃/min, keeping for 2 hours, and slowly cooling to room temperature to obtain a black carbon material;
s3: and washing the porous carbon material with 5wt% hydrochloric acid solution for three times, washing the porous carbon material with deionized water for three times, and drying to obtain the porous carbon material.
The parameters of the prepared carbon material are as follows: specific surface area 2100m2The specific capacitance is up to above 260F/g, and the graphitization degree (I)G) Was 1.13.
Example 3
A biomass porous carbon and a preparation method thereof comprise the following steps:
s1: 3g of cellulose, 3g of zinc chloride, 3g of ammonium bicarbonate, 3g of ammonium chloride and 3g of potassium ferrate are subjected to ball milling and mixing, the diameter of a grinding ball is 5mm, the mass ratio of the grinding ball to the total mass of the biomass, the zinc chloride, the ammonium bicarbonate, the ammonium chloride and the potassium ferrate is 1:4.8, the rotating speed is 400 r/min, the grinding time is 3 hours, and the mixture is uniformly mixed;
s2: placing the mixture obtained in the step S1 into a high-temperature carbonization furnace, continuously introducing protective gas nitrogen at the speed of 25 mL/min, heating to 300 ℃ from room temperature at the speed of 1.5 ℃/min, heating to 850 ℃ at the speed of 2 ℃/min, keeping for 2 hours, and slowly cooling to room temperature to obtain a black carbon material;
s3: and washing the porous carbon material with 5wt% hydrochloric acid solution for three times, washing the porous carbon material with deionized water for three times, and drying to obtain the porous carbon material.
The parameters of the prepared carbon material are as follows: specific surface area 2680m2/g，The specific capacitance is up to over 240F/g, and the graphitization degree (I)G) Is 1.35.
Example 4
S1: performing ball milling and mixing on 3g of chitin, 1.5g of zinc chloride, 1.5g of ammonium bicarbonate, 4.5g of ammonium chloride and 4.5g of potassium ferrate, wherein the diameter of a milling ball is 3mm, the mass ratio of the milling ball to the total mass of the biomass, the zinc chloride, the ammonium bicarbonate, the ammonium chloride and the potassium ferrate is 1:6, the rotating speed is 600 r/min, the milling is performed for 2 hours, and the mixing is uniform;
s2: placing the mixture obtained in the step S1 into a high-temperature carbonization furnace, continuously introducing inert protective gas nitrogen at the speed of 25 mL/min, heating to 300 ℃ from room temperature at the speed of 1.5 ℃/min, heating to 850 ℃ at the speed of 2 ℃/min, keeping for 2 hours, and slowly cooling to room temperature to obtain a black carbon material;
s3: and washing the porous carbon material with 5wt% hydrochloric acid solution for three times, washing the porous carbon material with deionized water for three times, and drying to obtain the porous carbon material.
The parameters of the prepared carbon material are as follows: specific surface area 2218m2The specific capacitance is higher than 231F/g, and the graphitization degree (I)G) Was 1.08.
Example 5
S1: performing ball milling and mixing on 3g of chitin, 4.5g of zinc chloride, 3g of ammonium bicarbonate, 6g of ammonium chloride and 4.5g of potassium ferrate, wherein the diameter of a milling ball is 3mm, the mass ratio of the milling ball to the total mass of the biomass, the zinc chloride, the ammonium bicarbonate, the ammonium chloride and the potassium ferrate is 1:4, the rotating speed is 300 r/min, the milling is performed for 4 hours, and the mixing is uniform;
s2: placing the mixture obtained in the step S1 into a high-temperature carbonization furnace, continuously introducing inert protective gas nitrogen at the speed of 25 mL/min, heating to 300 ℃ from room temperature at the speed of 1.5 ℃/min, heating to 850 ℃ at the speed of 2 ℃/min, keeping for 2 hours, and slowly cooling to room temperature to obtain a black carbon material;
s3: and washing the porous carbon material with 5wt% hydrochloric acid solution for three times, washing the porous carbon material with deionized water for three times, and drying to obtain the porous carbon material.
The parameters of the prepared carbon material are as follows: specific surface area 2116m2A specific capacitance of more than 225F/g, graphiteDegree of conversion (I)G) Is 1.11.
Example 6
S1: performing ball milling and mixing on 3g of chitin, 3g of zinc chloride, 6g of ammonium bicarbonate, 9g of ammonium chloride and 6g of potassium ferrate, wherein the diameter of a milling ball is 3mm, the mass ratio of the milling ball to the total mass of the biomass, the zinc chloride, the ammonium bicarbonate, the ammonium chloride and the potassium ferrate is 1:4, the rotating speed is 300 r/min, the milling is performed for 4 hours, and the mixing is uniform;
s2: placing the mixture obtained in the step S1 into a high-temperature carbonization furnace, continuously introducing inert protective gas nitrogen at the speed of 25 mL/min, heating to 300 ℃ from room temperature at the speed of 1.5 ℃/min, heating to 850 ℃ at the speed of 2 ℃/min, keeping for 2 hours, and slowly cooling to room temperature to obtain a black carbon material;
s3: and washing the porous carbon material with 5wt% hydrochloric acid solution for three times, washing the porous carbon material with deionized water for three times, and drying to obtain the porous carbon material.
The parameters of the prepared carbon material are as follows: specific surface area 2680m2The specific capacitance is up to more than 210F/g, and the graphitization degree (I)G) Is 1.02.
Effect example 1
Desalted electrode samples 1 to 4 were prepared from the carbon materials prepared in examples 1 to 6 by the following method:
(1) respectively crushing the carbon materials prepared in the embodiments 1-6 into powder which is sieved by a 200-mesh sieve, mixing the powder with polytetrafluoroethylene, wherein the mass ratio of the carbon materials to the polytetrafluoroethylene is 95:5, adding deionized water into the obtained mixture to enable the mass fraction of the carbon materials to be 8%, stirring for 4 hours, and drying for 12 hours at 105 ℃ to obtain a sticky solid;
(2) and uniformly coating the obtained sticky solid on foamed nickel, coating the material with double-layer foamed nickel, pressing and rolling the material into a sheet material, and then sticking the foamed nickel on a porous reticular inert polytetrafluoroethylene plate to obtain the corresponding desalting electrode plate.
The obtained desalination electrode was subjected to a seawater desalination experiment, and the results were as follows:
the sodium chloride adsorption capacity of the sample 1 reaches 45 mg/g; the sodium chloride adsorption capacity of the sample 2 reaches 37 mg/g; the absorption amount of the sodium chloride of the sample 3 reaches 40 mg/g; the absorption amount of the sodium chloride of the sample 4 reaches 38 mg/g; the absorption amount of the sodium chloride of the sample 5 reaches 32 mg/g; the absorption amount of the sodium chloride of the sample 6 reaches 37 mg/g;
comparative example 1
The difference from example 1 is that ammonium bicarbonate and ammonium chloride are not added in step S1.
The parameters of the prepared carbon material are as follows: specific surface area 760m2The specific capacitance is up to 112F/g, and the graphitization degree (I)G) The adsorption amount of sodium chloride was 1.53, and 21mg/g was obtained.
Comparative example 2
The difference from example 2 is that ammonium bicarbonate is not added in step S1.
The parameters of the prepared carbon material are as follows: specific surface area 2730m2The specific capacitance is more than 217F/g, and the graphitization degree (I)G) The adsorption amount of sodium chloride is 1.61, and the adsorption amount of sodium chloride reaches 38 mg/g.
Comparative example 3
The difference from example 3 is that ammonium chloride was not added in step S1.
The parameters of the prepared carbon material are as follows: specific surface area 923m2The specific capacitance is higher than 151F/g, and the graphitization degree (I)G) The adsorption amount of sodium chloride was 1.56, and the adsorption amount of sodium chloride reached 27 mg/g.
Comparative example 4
The difference from example 1 is that zinc chloride is not added in step S1.
The parameters of the prepared carbon material are as follows: specific surface area 580m2The specific capacitance is more than 119F/g, and the graphitization degree (I)G) The adsorption quantity of sodium chloride is 1.60, and the adsorption quantity of sodium chloride reaches 18 mg/g.
Comparative example 5
The difference from example 1 is that potassium ferrate is not raised in step S1.
The parameters of the prepared carbon material are as follows: specific surface area 2638m2The specific capacitance is over 202F/g, and the graphitization degree (I)G) Is 1.89, and the absorption amount of sodium chloride reaches 42 mg/g.
Comparative example 6
The difference from example 1 is that potassium chloride is used instead of zinc chloride in step S1.
The parameters of the prepared carbon material are as follows: specific surface area 1074m2A specific capacitance of more than 129F/g, a graphitization degree (I)G) The adsorption amount of sodium chloride was 1.69, and the adsorption amount of sodium chloride reached 27 mg/g.
Comparative example 7
The difference from example 1 is that potassium ferrate is replaced with potassium permanganate in step S1.
The parameters of the prepared carbon material are as follows: specific surface area 2731m2The specific capacitance is more than 255F/g, and the graphitization degree (I)G) The adsorption quantity of sodium chloride is 1.11, and the adsorption quantity of sodium chloride reaches 40 mg/g.
Comparative example 8
The difference from example 1 is that wet mixing is performed, and water is used as a solvent, and ball milling wet mixing is performed.
The parameters of the prepared carbon material are as follows: specific surface area 1700m2The specific capacitance is up to 158F/g, and the graphitization degree (I)G) The adsorption quantity of sodium chloride is 1.51, and the adsorption quantity of sodium chloride reaches 26 mg/g.
Comparative example 9
The difference from the embodiment 1 is that only potassium ferrate and chitin are added for mixing, ball milling and high-temperature carbonization.
The parameters of the prepared carbon material are as follows: specific surface area 1690m2The specific capacitance is over 238F/g, and the graphitization degree (I)G) Is 1.01, and the absorption amount of sodium chloride reaches 30 mg/g.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. The biomass porous carbon and the preparation method thereof are characterized by comprising the following steps:
s1: carrying out dry grinding on the biomass, zinc chloride, ammonium bicarbonate, ammonium chloride and potassium ferrate, and uniformly mixing;
s2: carbonizing the mixture obtained in the step S1 at 750-950 ℃ for 1-3 h in a protective gas atmosphere, and cooling to room temperature to obtain a carbon material;
s3: and (3) carrying out acid washing and deionized water cleaning on the obtained carbon material, and drying to obtain the carbon material.
2. The biomass porous carbon and the preparation method thereof according to claim 1, wherein the mass ratio of the biomass to the zinc chloride to the ammonium bicarbonate to the ammonium chloride to the potassium ferrate is 1: 0.5-1.5: 0.5-2: 1-3: 1-2.5.
3. The biomass porous carbon and the preparation method thereof according to claim 1, wherein the mass ratio of the biomass to the zinc chloride to the ammonium bicarbonate to the ammonium chloride to the potassium ferrate is 1:1:1: 1.
4. The biomass porous carbon and the preparation method thereof according to claim 1, wherein the biomass is selected from one or a combination of any two or more of chitin, lignin or cellulose.
5. The biomass porous carbon and the preparation method thereof according to claim 1, wherein the biomass is selected from chitin.
6. The biomass porous carbon and the preparation method thereof according to claim 1, characterized in that the dry grinding is dry ball milling, the mass ratio of grinding balls to the total mass of the biomass, the zinc chloride, the ammonium bicarbonate, the ammonium chloride and the potassium ferrate is 1: 4-6, the diameter of the grinding balls is 0.5-10 mm, the rotating speed is 250-600 r/min, and the grinding time is 1-5 h.
7. The biomass porous carbon and the preparation method thereof according to claim 1, wherein the step S2 specifically comprises: continuously introducing protective gas at the speed of 15-40 mL/min, heating to 280-320 ℃ from room temperature at the speed of 1.2-1.8 ℃/min, then heating to 750-950 ℃ at the speed of 2-2.2 ℃/min, keeping for 1-3 hours, and then slowly cooling to room temperature to obtain the black carbon material.
8. The biomass porous carbon and the preparation method thereof according to claim 1, wherein the hydrochloric acid concentration is 5 wt%.
9. Application of the biomass porous carbon material obtained by the preparation method according to any one of claims 1 to 8 in the field of seawater desalination.
10. Use according to claim 9 for the preparation of desalination electrodes.
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| CN110318066A (en) * | 2019-06-20 | 2019-10-11 | 青岛鼎海电化学科技有限公司 | A kind of preparation method of tetra-alkyl ammonium hydroxide |
| CN111634907A (en) * | 2020-06-08 | 2020-09-08 | 惠州市贝特瑞新材料科技有限公司 | Nitrogen-iron co-doped graphite carbon and preparation method and application thereof |
| CN116199223A (en) * | 2023-03-24 | 2023-06-02 | 河北省科学院能源研究所 | Preparation method of hard porous carbon for sodium ion battery |
| CN116726877A (en) * | 2023-07-03 | 2023-09-12 | 河北省科学院能源研究所 | Preparation of biomass porous carbon and carbon dioxide adsorption application thereof |
| CN116747833A (en) * | 2023-04-10 | 2023-09-15 | 南京信息工程大学 | Activated carbon wood fiber foam and preparation method thereof |
| CN116986584A (en) * | 2023-09-28 | 2023-11-03 | 河北省科学院能源研究所 | Preparation method of nitrogen, phosphorus and iron doped carbon material and application of nitrogen, phosphorus and iron doped carbon material in rubber |
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| CN116986584B (en) * | 2023-09-28 | 2024-01-02 | 河北省科学院能源研究所 | Preparation method of nitrogen, phosphorus and iron doped carbon material and application of nitrogen, phosphorus and iron doped carbon material in rubber |
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