CN111072027A - Cubic carbon material from hemicellulose and preparation method thereof - Google Patents

Cubic carbon material from hemicellulose and preparation method thereof Download PDF

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Publication number
CN111072027A
CN111072027A CN202010066547.7A CN202010066547A CN111072027A CN 111072027 A CN111072027 A CN 111072027A CN 202010066547 A CN202010066547 A CN 202010066547A CN 111072027 A CN111072027 A CN 111072027A
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hemicellulose
carbon material
supernatant
shaddock peel
derived
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Inventor
蔺华林
李梦琰
王叶函
刘为民
李晓斌
韩生
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Shanghai Institute of Technology
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Shanghai Institute of Technology
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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
    • C01B32/318—Preparation characterised by the starting materials
    • C01B32/324—Preparation characterised by the starting materials from waste materials, e.g. tyres or spent sulfite pulp liquor
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22—Electrodes
    • H01G11/30—Electrodes characterised by their material
    • H01G11/32—Carbon-based
    • H01G11/34—Carbon-based characterised by carbonisation or activation of carbon
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22—Electrodes
    • H01G11/30—Electrodes characterised by their material
    • H01G11/32—Carbon-based
    • H01G11/44—Raw materials therefor, e.g. resins or coal
    • 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
    • Y02E60/13—Energy storage using capacitors

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Power Engineering (AREA)
  • Organic Chemistry (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Inorganic Chemistry (AREA)
  • Environmental & Geological Engineering (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

The invention relates to a cuboidal carbon material from hemicellulose and a preparation method thereof, wherein the preparation method comprises the following steps: 1) cutting the shaddock peel into blocks, washing, drying, and grinding into powder to obtain shaddock peel powder; 2) adding the shaddock peel powder into an alkali solution, uniformly stirring, filtering, and taking a supernatant; 3) adjusting the supernatant to be neutral, mixing the supernatant with ethanol, performing centrifugal washing, and drying to obtain a hemicellulose precursor; 4) and mixing the hemicellulose precursor with an activating agent, and then calcining at a high temperature to obtain the cubic carbon material. Compared with the prior art, the preparation process is simple, the carbon material is directly synthesized by a one-step method, the energy is saved, the prepared biomass-based carbon electrode material has a regular cubic structure, the subsequent modification and other operations are facilitated, the raw material is extracted from the biomass waste shaddock peel, the cost is low, and the application prospect is wide.

Description

Cubic carbon material from hemicellulose and preparation method thereof
Technical Field
The invention belongs to the technical field of carbon materials, and relates to a cubic carbon material from hemicellulose and a preparation method thereof.
Background
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.
Cellulose is a biopolymer material with light weight, good biocompatibility and strong flexibility in nature, and is widely applied to the fields of flexible supercapacitors, biosensors, electromagnetic shielding and the like. In the field of flexible supercapacitors, the polyhydroxy structure of cellulose-based materials is a good medium for electrolyte ion conduction, which is beneficial to improving the capacitance characteristic and cycle characteristic of electrode materials, and is easy to construct a conductive framework with conductive active materials (such as graphene, carbon nanotubes and conductive polymers) by methods of coating, blending, layer-by-layer self-assembly, in-situ polymerization and the like so as to prepare flexible electrode materials. In recent years, the preparation of carbon materials using biomass as a carbon source has become a research focus. At present, the preparation method of the biomass-based carbon material mainly comprises a template method, a carbonization method and a hydrothermal method. The template method can be divided into a hard template method and a soft template method according to the difference in the synthesis route and the action principle of the carbon material.
However, the process for preparing the biomass carbon material by adopting the method has the problems of insufficient precursor material, poor material morphology, complex preparation process and the like, and limits further application of the biomass carbon material.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a cubic carbon material from hemicellulose and a preparation method thereof, and the prepared biomass-based carbon electrode material has a regular cubic structure and a wide application prospect.
The purpose of the invention can be realized by the following technical scheme:
a method of producing a cuboidal carbon material from hemicellulose, the method comprising the steps of:
1) cutting the shaddock peel into blocks, washing, drying, and grinding into powder to obtain shaddock peel powder;
2) adding the shaddock peel powder into an alkali solution, uniformly stirring, filtering, and taking a supernatant;
3) adjusting the supernatant to be neutral, mixing the supernatant with ethanol, performing centrifugal washing, and drying to obtain a hemicellulose precursor;
4) and mixing the hemicellulose precursor with an activating agent, and then calcining at a high temperature to obtain the cubic carbon material.
Further, in step 2), the alkali solution is a KOH solution. The concentration of the KOH solution is 5 to 7mol/L, preferably 6 mol/L.
Further, in the step 2), the mass ratio of the shaddock peel powder to the alkali solution is 1 (1-4). The shaddock peel powder is dissolved in alkali liquor mainly for obtaining hemicellulose.
Further, in the step 2), the stirring is magnetic stirring, the stirring temperature is 45-55 ℃, and the stirring time is 10-15 h.
Further, in the step 3), the volume ratio of the ethanol to the supernatant is (1.5-2.5): 1.
Further, in the step 3), the drying process is carried out in a vacuum drying oven, wherein the temperature is 60-110 ℃ and the time is 6-12h in the drying process.
Further, in the step 4), the activating agent is H3PO4. The activating agent can form the surface physical and chemical properties and abundant pore structures of the carbon material, and the activating agent can crystallize and melt on the surface of the fiber to etch the carbon body to form micropores, so that the activating effect is achieved.
Further, in the step 4), the mass ratio of the hemicellulose precursor to the activating agent is 1 (1-2).
Further, in the step 4), the temperature is 500-900 ℃ and the time is 2-6h in the high-temperature calcination process.
A cuboidal carbon material from hemicellulose, which is produced using the method.
The invention adopts the shaddock peel as the raw material, and the hemicellulose extracted from the shaddock peel is a natural renewable resource, has rich source, low price and higher carbon content, and is an environment-friendly material completely meeting the green chemical requirements.
Compared with the prior art, the preparation process is simple, the carbon material is directly synthesized by a one-step method, the energy is saved, the prepared biomass-based carbon electrode material has a regular cubic structure, the subsequent modification and other operations are facilitated, the raw material is extracted from the biomass waste shaddock peel, the cost is low, and the application prospect is wide.
Drawings
FIG. 1 is an SEM image of a hemicellulose-derived cubic carbon material prepared in example 1;
fig. 2 is an SEM image of the hemicellulose-derived cubic carbon material prepared in example 2.
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:
a preparation method of a cubic carbon material from hemicellulose specifically comprises the following steps:
1) the shaddock peel is cut into small pieces, washed, dried and ground into powder.
2) Dissolving 6g of shaddock peel powder and KOH solution according to the mass ratio of 1:4, stirring and filtering to obtain supernatant, adjusting the supernatant to be neutral, mixing ethanol and the obtained supernatant, and centrifuging and washing to obtain a mixture.
3) And (3) placing the mixture in a vacuum drying oven for vacuum drying, and performing vacuum drying at 80 ℃ for 6h to obtain a hemicellulose precursor.
4) Mixing hemicellulose precursor with activating agent H3PO4After mixing, the mixture is calcined at the high temperature of 600 ℃ for 2 hours to obtain the semi-fiber cubic carbon material. As can be seen from the SEM image of FIG. 1, the prepared carbon material has a more regular morphology and a generally cubic structure. The method is simple to operate and low in cost, and is expected to become a promising material in the fields of super capacitors, lithium ion batteries, electrocatalysis and the like.
Example 2:
a preparation method of a cubic carbon material from hemicellulose specifically comprises the following steps:
1) the shaddock peel is cut into small pieces, washed, dried and ground into powder.
2) Dissolving 8g of shaddock peel powder and KOH solution according to the mass ratio of 1:4, stirring and filtering to obtain supernatant, adjusting the supernatant to be neutral, mixing ethanol and the obtained supernatant, and centrifuging and washing to obtain a mixture.
3) And (3) placing the mixture in a vacuum drying oven for vacuum drying, and performing vacuum drying at 70 ℃ for 8h to obtain a hemicellulose precursor.
4) Mixing hemicellulose precursor with activating agent H3PO4After mixing, the mixture is calcined at a high temperature of 800 ℃ for 3 hours to obtain the semi-fibrous cubic carbon material. As can be seen from the SEM image of FIG. 2, the prepared carbon material has a more regular morphology and a generally cubic structure. However, due to the higher calcination temperature, the structural surface of part of the carbon material collapses, which indicates that a material with good morphology can be obtained by using a proper calcination temperature.
Example 3:
a preparation method of a cubic carbon material from hemicellulose specifically comprises the following steps:
1) the shaddock peel is cut into small pieces, washed, dried and ground into powder.
2) Dissolving 10g of shaddock peel powder and KOH solution according to the mass ratio of 1:4, stirring and filtering to obtain supernatant, adjusting the supernatant to be neutral, mixing ethanol and the obtained supernatant, and centrifuging and washing to obtain a mixture.
3) And (3) placing the mixture in a vacuum drying oven for vacuum drying, and performing vacuum drying at 70 ℃ for 8h to obtain a hemicellulose precursor.
4) Mixing hemicellulose precursor with activating agent H3PO4After mixing, the mixture is calcined at the high temperature of 600 ℃ for 2 hours to obtain the semi-fiber cubic carbon material.
Example 4:
a preparation method of a cubic carbon material from hemicellulose specifically comprises the following steps:
1) the shaddock peel is cut into small pieces, washed, dried and ground into powder.
2) Dissolving 10g of shaddock peel powder and KOH solution according to the mass ratio of 1:4, stirring and filtering to obtain supernatant, adjusting the supernatant to be neutral, mixing ethanol and the obtained supernatant, and centrifuging and washing to obtain a mixture.
3) And (3) placing the mixture in a vacuum drying oven for vacuum drying, and performing vacuum drying at 80 ℃ for 8h to obtain a hemicellulose precursor.
4) Mixing hemicellulose precursor with activating agent H3PO4After mixing, the mixture is calcined at a high temperature of 800 ℃ for 3 hours to obtain the semi-fibrous cubic carbon material.
Example 5:
a method of producing a cuboidal carbon material from hemicellulose, the method comprising the steps of:
1) cutting the shaddock peel into blocks, washing, drying, and grinding into powder to obtain shaddock peel powder;
2) adding shaddock peel powder into a KOH solution, wherein the mass ratio of the shaddock peel powder to an alkali solution is 1:1, uniformly stirring by magnetic force, wherein the stirring temperature is 55 ℃, the stirring time is 10 hours, and then filtering to obtain a supernatant;
3) adjusting the supernatant to be neutral, mixing the supernatant with ethanol, performing centrifugal washing, wherein the volume ratio of the ethanol to the supernatant is 2.5:1, and performing vacuum drying in a vacuum drying oven at the temperature of 60 ℃ for 12 hours to obtain a hemicellulose precursor;
4) mixing hemicellulose precursor with activating agent H3PO4Mixing the raw materials according to the mass ratio of 1:1, and then carrying out high-temperature calcination at the temperature of 900 ℃ for 2 hours to obtain the cubicA carbon material.
Example 6:
a method of producing a cuboidal carbon material from hemicellulose, the method comprising the steps of:
1) cutting the shaddock peel into blocks, washing, drying, and grinding into powder to obtain shaddock peel powder;
2) adding shaddock peel powder into a KOH solution, wherein the mass ratio of the shaddock peel powder to an alkali solution is 1:4, uniformly stirring by magnetic force, wherein the stirring temperature is 45 ℃, the stirring time is 15 hours, and then filtering to obtain a supernatant;
3) adjusting the supernatant to be neutral, mixing the supernatant with ethanol, performing centrifugal washing, wherein the volume ratio of the ethanol to the supernatant is 1.5:1, and performing vacuum drying in a vacuum drying oven at the temperature of 110 ℃ for 6 hours to obtain a hemicellulose precursor;
4) mixing hemicellulose precursor with activating agent H3PO4And mixing the materials according to the mass ratio of 1:2, and then carrying out high-temperature calcination at the high-temperature calcination temperature of 500 ℃ for 6 hours to obtain the cubic carbon material.
Example 7:
a method of producing a cuboidal carbon material from hemicellulose, the method comprising the steps of:
1) cutting the shaddock peel into blocks, washing, drying, and grinding into powder to obtain shaddock peel powder;
2) adding shaddock peel powder into a KOH solution, wherein the mass ratio of the shaddock peel powder to an alkali solution is 1:2, uniformly stirring by magnetic force, wherein the stirring temperature is 50 ℃, the stirring time is 12 hours, and then filtering to obtain a supernatant;
3) adjusting the supernatant to be neutral, mixing the supernatant with ethanol, performing centrifugal washing, wherein the volume ratio of the ethanol to the supernatant is 2:1, and performing vacuum drying in a vacuum drying oven at the temperature of 80 ℃ for 9 hours to obtain a hemicellulose precursor;
4) mixing hemicellulose precursor with activating agent H3PO4And mixing the materials according to the mass ratio of 1:1.5, and then carrying out high-temperature calcination at the high-temperature calcination temperature of 700 ℃ for 4 hours to obtain the cubic carbon material.
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. A method for producing a hemicellulose-derived cubic carbon material, comprising the steps of:
1) cutting the shaddock peel into blocks, washing, drying, and grinding into powder to obtain shaddock peel powder;
2) adding the shaddock peel powder into an alkali solution, uniformly stirring, filtering, and taking a supernatant;
3) adjusting the supernatant to be neutral, mixing the supernatant with ethanol, performing centrifugal washing, and drying to obtain a hemicellulose precursor;
4) and mixing the hemicellulose precursor with an activating agent, and then calcining at a high temperature to obtain the cubic carbon material.
2. The method for producing a hemicellulose-derived cubic carbon material as claimed in claim 1, wherein in step 2), the alkali solution is a KOH solution.
3. The method for preparing a hemicellulose-derived cuboidal carbon material according to claim 1, wherein in step 2), the mass ratio of the shaddock peel powder to the alkaline solution is 1 (1-4).
4. The method for preparing a hemicellulose-derived cuboidal carbon material according to claim 1, wherein in step 2), the stirring is magnetic stirring, the stirring temperature is 45-55 ℃, and the stirring time is 10-15 h.
5. The method for preparing a hemicellulose-derived cuboidal carbon material according to claim 1, wherein in step 3), the volume ratio of ethanol to supernatant is (1.5-2.5): 1.
6. The method for preparing a hemicellulose-derived cuboidal carbon material according to claim 1, wherein in step 3), the drying process is carried out in a vacuum drying oven, and the temperature in the drying process is 60-110 ℃ and the time is 6-12 h.
7. The method for producing a hemicellulose-derived cubic carbon material as claimed in claim 1, wherein the activating agent in step 4) is H3PO4。
8. The method for preparing a hemicellulose-derived cubic carbon material according to claim 1, wherein the mass ratio of the hemicellulose precursor to the activating agent in step 4) is 1 (1-2).
9. The method for preparing a cubic carbon material derived from hemicellulose as claimed in claim 1, wherein the temperature in the high temperature calcination process in step 4) is 500-900 ℃ for 2-6 h.
10. A cuboidal carbon material derived from hemicellulose, characterized in that it has been produced by a method according to any one of claims 1 to 9.
CN202010066547.7A 2020-01-20 2020-01-20 Cubic carbon material from hemicellulose and preparation method thereof Pending CN111072027A (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104743554A (en) * 2013-12-26 2015-07-01 济南圣泉集团股份有限公司 Active carbon preparation method and device
CN107424850A (en) * 2016-05-23 2017-12-01 中国海洋大学 It is a kind of to prepare the method for cellulose base porous carbon materials using hydro-thermal-activation-pyrolysismethod and be used for electrode of super capacitor
KR20180130946A (en) * 2017-05-31 2018-12-10 한국세라믹기술원 Manufacturing method of partially crystaline porous active carbon, supercapacitor using the active carbon and manufacturing method of the supercapacitor
CN109809403A (en) * 2019-03-18 2019-05-28 中国药科大学 A kind of preparation method and application of the biogas residue matrix activated carbon with high absorption property
CN109887762A (en) * 2019-02-15 2019-06-14 上海应用技术大学 A kind of preparation method of the nitrogen sulphur codope carbon material based on hemicellulose

Patent Citations (5)

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Publication number Priority date Publication date Assignee Title
CN104743554A (en) * 2013-12-26 2015-07-01 济南圣泉集团股份有限公司 Active carbon preparation method and device
CN107424850A (en) * 2016-05-23 2017-12-01 中国海洋大学 It is a kind of to prepare the method for cellulose base porous carbon materials using hydro-thermal-activation-pyrolysismethod and be used for electrode of super capacitor
KR20180130946A (en) * 2017-05-31 2018-12-10 한국세라믹기술원 Manufacturing method of partially crystaline porous active carbon, supercapacitor using the active carbon and manufacturing method of the supercapacitor
CN109887762A (en) * 2019-02-15 2019-06-14 上海应用技术大学 A kind of preparation method of the nitrogen sulphur codope carbon material based on hemicellulose
CN109809403A (en) * 2019-03-18 2019-05-28 中国药科大学 A kind of preparation method and application of the biogas residue matrix activated carbon with high absorption property

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林冠峰 等: ""磷酸活化法制备半纤维素基颗粒活性炭"", 《生物质化学工程》 *

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