CN103922328A - Method for preparing nitrogenous hierarchical pore three-dimensional graphene by using chitosan - Google Patents
Method for preparing nitrogenous hierarchical pore three-dimensional graphene by using chitosan Download PDFInfo
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- CN103922328A CN103922328A CN201410157667.2A CN201410157667A CN103922328A CN 103922328 A CN103922328 A CN 103922328A CN 201410157667 A CN201410157667 A CN 201410157667A CN 103922328 A CN103922328 A CN 103922328A
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Abstract
The invention discloses a method for preparing nitrogenous hierarchical pore three-dimensional graphene by using chitosan. The method comprises the following steps: preparing chitosan aerogel by using chitosan powder, carbonizing the chitosan aerogel to obtain nitrogenous carbon aerogel, and activating the nitrogenous carbon aerogel to obtain the nitrogenous hierarchical pore three-dimensional graphene. According to the method, a natural recyclable biopolymer chitosan is adopted as a raw material to prepare the nitrogenous hierarchical pore three-dimensional graphene, not only are requirements of sustainable development and environmental friendliness met, but also the cost of the raw material is effectively lowed; moreover, as the chitosan molecule contains nitrogen element, the nitrogenous graphene can be prepared without doping. Compared with a conventional method, the method disclosed by the invention has the advantages that a product is higher in specific surface area which is more than 2000m<2>g<-1>, is beneficial for transmission and conveying of ions of electrolyte inside, and has the potential to be an electrode material of an industrial super capacitor; the method is good in repeatability.
Description
Technical field
The present invention relates to a kind of preparation method of nitrogenous multi-stage porous three-dimensional grapheme, relate in particular to a kind of method of utilizing chitosan preparation to possess the nitrogenous Graphene of three-dimensional multistage pore structure, belong to field of material preparation.
Background technology
After Graphene is prepared first, because being subject to people, its unique structure and photoelectric property pay attention to widely.Graphene is by the tightly packed a kind of carbonaceous elementary cell with bi-dimensional cellular shape crystalline network forming of carbon atom, can be used to build the carbonaceous material of other dimension, as zero dimension soccerballene, and one dimension carbon nanotube or three-dimensional graphite.The two-dirnentional structure of Graphene uniqueness, make it show excellent electric property, good chemical stability and thermodynamic stability, and physicals and mechanical property, obtaining broad research and application aspect photoelectricity, senser element, energy reserves and conversion, biomaterial.Meanwhile, Graphene also has up to 2630m
2the specific surface area of/g and higher specific conductivity (64mS/cm), make it can be used as desirable electrode material for super capacitor.In order further to improve the specific capacitance of graphene-based ultracapacitor, investigators have improved Graphene structure by preparing hierarchical porous structure and doping improves its energy density.
The preparation method of Graphene mainly contains graphite and peels off (Novoselov, K.S., et al, Science, 2004 at present, 306,666), epitaxy (Forbeaux, I., et al, Appl.Surf.Sci., 2000,162-163,406), chemical Vapor deposition process (Ruoff, R.S., et al, Science, 2009,324:1312), graphite oxidation method (Hummers, W.S., et al, J.Am.Chem.Soc., 1958,80:133) etc.But aforesaid method is difficult to meet extensive, low-cost, the controlled requirements such as synthetic and preparation, and the Graphene obtaining is intrinsic Graphene substantially, and its specific surface area and surface tissue are all undesirable, and mostly by raw mineral materials, are transformed.Because environmental pollution is serious in the limited reserves of fossil resource and preparation process, using renewable natural polymer or agricultural product castoff to prepare Graphene is vital for Sustainable development and environment protection.Chitosan is the product of the de-N-ethanoyl of chitin, is natural reproducible biological polymer, not only cheap, environmental friendliness, and in chitosan molecule, contain nitrogen element, during application, do not need doping can obtain nitrogenous Graphene.Yet the method for utilizing chitosan preparation to possess the nitrogenous Graphene of three-dimensional multistage pore structure through retrieval have not been reported.
Summary of the invention
Problem for existing in current Graphene electrodes material preparation process, the present invention proposes a kind of method of utilizing chitosan to prepare nitrogenous multi-stage porous three-dimensional grapheme.
The method of utilizing chitosan to prepare nitrogenous multi-stage porous three-dimensional grapheme of the present invention, step is:
(1) utilize chitosan powder to make chitosan aerogel;
(2) carbonization chitosan aerogel, obtains nitrogenous carbon aerogels;
(3) activated carbon aerogel, obtains nitrogenous multi-stage porous three-dimensional grapheme;
It is characterized in that:
The described method of utilizing chitosan powder to make chitosan aerogel of step (1) is: chitosan powder be take to the ratio that massfraction is 2-4wt% and join in deionized water, stir 1-2h, then to add volume fraction be the acetic acid of 1-2% and be stirred to transparently, obtains colloidal sol; The standing 3-5h of colloidal sol is placed on to-80 ℃ of freezing 10-12h, then puts into the dry 48-52h of freeze drier, obtain chitosan aerogel;
The described carbonization chitosan of step (2) aerogel, the method that obtains nitrogenous carbon aerogels is: the chitosan aerogel that step (1) is obtained put into tube furnace under N2 protective atmosphere with the heat-up rate of 3 ℃/min in 700-1000 ℃ of carbonization 2-4h, obtain nitrogenous carbon aerogels;
The described activated carbon aerogel of step (3), the method that obtains nitrogenous multi-stage porous three-dimensional grapheme is: after the nitrogenous carbon aerogels that step (2) is obtained is pulverized, the amount that the mass ratio of NaOH and nitrogenous carbon aerogels of take is 3:1-5:1 joins the nitrogenous carbon aerogels powder making in the NaOH solution that concentration is 4-6wt%, stir 2-3h, obtain the mixed solution of nitrogenous carbon aerogels and NaOH; Then be placed on 80 ℃ dry until in mixed solution moisture evaporate completely, then proceed in tube furnace at N
2heat-up rate with 5 ℃/min under protective atmosphere activates 2-3h in 800-1000 ℃; With deionized water, the nitrogenous carbon aerogels suction filtration after activation is washed till to neutrality, then puts 50 ℃ and obtain nitrogenous multi-stage porous three-dimensional grapheme after dry.
Above-mentioned utilization in the method that chitosan prepares nitrogenous multi-stage porous three-dimensional grapheme: preferably 800 ℃ of carbonization temperatures described in step (2).
Above-mentioned utilization in the method that chitosan prepares nitrogenous multi-stage porous three-dimensional grapheme: described in step (3), the mass ratio of NaOH and nitrogenous carbon aerogels is preferably 3:1.
Above-mentioned utilization in the method that chitosan prepares nitrogenous multi-stage porous three-dimensional grapheme: preferably 900 ℃ of activation temperatures described in step (3).
The inventive method has following outstanding advantages and effect:
1. to have selected natural reproducible biological polymer chitosan be that raw material is prepared nitrogenous multi-stage porous three-dimensional grapheme in the present invention, not only meets the demand of Sustainable development and environment protection, and its source is abundant, cheap, effectively reduces raw-material cost.And owing to containing nitrogen element in chitosan molecule, do not need doping just can obtain nitrogenous Graphene.
2. classifying porous and nitrogenous Graphene product of the present invention obtains by simple lyophilize, carbonization and activating process, and preparation technology is simple, and environmental friendliness is suitable for large-scale production.
3. in the inventive method, utilize chitosan powder first to make chitosan aerogel, recarbonize chitosan aerogel, obtain carbon aerogels, and then activated carbon aerogel, obtain nitrogenous multi-stage porous three-dimensional grapheme, in obtaining the process of Graphene, just can obtain possessing the three-dimensional structure of multi-stage porous, a step forms, without extra pore-creating and doping step.The product specific surface area making compared with ordinary method is higher, reaches 2000m
2g
-1above, and reproducible, be conducive to ion portion's transmission within it and the transportation of electrolytic solution, be expected to become industrialized electrode material for super capacitor.
Accompanying drawing explanation
Fig. 1 is the Raman collection of illustrative plates of the nitrogenous multi-stage porous three-dimensional grapheme of preparation.
Fig. 2 is field emission scanning electron microscope (FESEM) photo of the nitrogenous multi-stage porous three-dimensional grapheme of preparation.
Fig. 3 is transmission electron microscope (TEM) photo of the nitrogenous multi-stage porous three-dimensional grapheme of preparation.
Wherein: (a) being the transmission electron microscope photo of Graphene, is (b) the high-resolution-ration transmission electric-lens photo of decolorizing carbon in (a) figure.
Fig. 4 is the N of the nitrogenous multi-stage porous three-dimensional grapheme of preparation
2absorption and pore size distribution curve.
Wherein: (a) be the N of three-dimensional grapheme
2adsorption curve, (b) is the pore size distribution curve of three-dimensional grapheme.
Fig. 5 is atomic force microscope (AFM) photo of the nitrogenous multi-stage porous three-dimensional grapheme of preparation.
Fig. 6 is the cyclic voltammetry curve of the nitrogenous multi-stage porous three-dimensional grapheme of preparation.
Embodiment
Embodiment 1:
1. the ratio that the massfraction of chitosan powder being take is 2wt% adds in 40ml deionized water, stirs 1h, and then to add volume fraction be 1% acetic acid and be stirred to transparently, obtains colloidal sol; The standing 3h of colloidal sol is placed on to-80 ℃ of freezing 10h, then puts into the dry 48h of freeze drier, obtain chitosan aerogel;
2. the chitosan aerogel 1. step being obtained is put into tube furnace at N
2under protective atmosphere with the heat-up rate of 3 ℃/min in 700 ℃ of carbonization 4h, obtain nitrogenous carbon aerogels;
3. after the nitrogenous carbon aerogels 2. step being obtained is pulverized, the amount that the mass ratio of NaOH and nitrogenous carbon aerogels of take is 3:1 joins the nitrogenous carbon aerogels powder making in the NaOH solution that concentration is 4wt%, stir 2h, obtain the mixed solution of nitrogenous carbon aerogels and NaOH; Then by its in 80 ℃ dry until in mixed solution moisture evaporate completely, then proceed in tube furnace at N
2heat-up rate with 5 ℃/min under protective atmosphere activates 2h in 800 ℃; With deionized water, the nitrogenous carbon aerogels suction filtration after activation is washed till to neutrality, puts 50 ℃ and obtained nitrogenous multi-stage porous three-dimensional grapheme after dry.
Embodiment 2:
1. the ratio that the massfraction of chitosan powder being take is 3wt% adds in 40ml deionized water, stirs 1.5h, and then to add volume fraction be 2% acetic acid and be stirred to transparently, obtains colloidal sol; The standing 4h of colloidal sol is placed on to-80 ℃ of freezing 11h, then puts into the dry 50h of freeze drier, obtain chitosan aerogel;
2. the chitosan aerogel 1. step being obtained is put into tube furnace at N
2under protective atmosphere with the heat-up rate of 3 ℃/min in 800 ℃ of carbonization 3h, obtain nitrogenous carbon aerogels;
3. after the nitrogenous carbon aerogels 2. step being obtained is pulverized, the amount that the mass ratio of NaOH and nitrogenous carbon aerogels of take is 4:1 joins the nitrogenous carbon aerogels powder making in the NaOH solution that concentration is 5wt%, stir 3h, obtain the mixed solution of nitrogenous carbon aerogels and NaOH; Then by its in 80 ℃ dry until in mixed solution moisture evaporate completely, then proceed in tube furnace at N
2heat-up rate with 5 ℃/min under protective atmosphere activates 3h in 900 ℃; With deionized water, the nitrogenous carbon aerogels suction filtration after activation is washed till to neutrality, puts 50 ℃ and obtained nitrogenous multi-stage porous three-dimensional grapheme after dry.
Embodiment 3:
1. the ratio that the massfraction of chitosan powder being take is 4wt% adds in 40ml deionized water, stirs 2h, and then to add volume fraction be 2% acetic acid and be stirred to transparently, obtains colloidal sol; The standing 5h of colloidal sol is placed on to-80 ℃ of freezing 12h, then puts into the dry 52h of freeze drier, obtain chitosan aerogel;
2. the chitosan aerogel 1. step being obtained is put into tube furnace at N
2under protective atmosphere with the heat-up rate of 3 ℃/min in 1000 ℃ of carbonization 2h, obtain nitrogenous carbon aerogels;
3. after the nitrogenous carbon aerogels 2. step being obtained is pulverized, the amount that the mass ratio of NaOH and nitrogenous carbon aerogels of take is 5:1 joins the nitrogenous carbon aerogels powder making in the NaOH solution that concentration is 6wt%, stir 3h, obtain the mixed solution of nitrogenous carbon aerogels and NaOH; Then by its in 80 ℃ of C dry until in mixed solution moisture evaporate completely, then proceed in tube furnace at N
2heat-up rate with 5 ℃/min under protective atmosphere activates 2h in 1000 ℃; With deionized water, the nitrogenous carbon aerogels suction filtration after activation is washed till to neutrality, puts 50 ℃ and obtained nitrogenous multi-stage porous three-dimensional grapheme after dry.
HR800 Raman analysis instrument analytic sample by the nitrogenous multi-stage porous three-dimensional grapheme of above-described embodiment gained with HORIBA Jobin Yvon company, finds that product is typical graphene-structured (Fig. 1).This sample is observed with field emission scanning electron microscope (Fig. 2) and the Japanese JEOL company's production JEM2100 type transmission electron microscope (Fig. 3) of HITACHI S-4800, from photo, can find out that the prepared Graphene number of plies is less, both there is the macropore that is greater than 50nm, also there is 2-50nm and the mesoporous and micropore that is less than 2nm.With Micromeritics ASAP2020 specific surface area and pore analysis instrument, further verified that it has the vesicular structure of classification (Fig. 4).By Bruker Dimension icon atomic force microscope, observe and thickness measurement, can find out that the Graphene of preparation is thinner (Fig. 5).With the CHI600C electrochemical workstation of Shanghai Chen Hua Instrument Ltd., tested its cyclic voltammetry curve (Fig. 6), found that it has desirable electrochemical behavior.
Claims (4)
1. utilize chitosan to prepare a method for nitrogenous multi-stage porous three-dimensional grapheme, step is:
(1) utilize chitosan powder to make chitosan aerogel;
(2) carbonization chitosan aerogel, obtains nitrogenous carbon aerogels;
(3) activated carbon aerogel, obtains nitrogenous multi-stage porous three-dimensional grapheme;
It is characterized in that:
The described method of utilizing chitosan powder to make chitosan aerogel of step (1) is: chitosan powder be take to the ratio that massfraction is 2-4wt% and join in deionized water, stir 1-2h, then to add volume fraction be the acetic acid of 1-2% and be stirred to transparently, obtains colloidal sol; The standing 3-5h of colloidal sol is placed on to-80 ℃ of freezing 10-12h, then puts into the dry 48-52h of freeze drier, obtain chitosan aerogel;
The described carbonization chitosan of step (2) aerogel, the method that obtains nitrogenous carbon aerogels is: the chitosan aerogel that step (1) is obtained is put into tube furnace at N
2under protective atmosphere with the heat-up rate of 3 ℃/min in 700-1000 ℃ of carbonization 2-4h, obtain nitrogenous carbon aerogels;
The described activated carbon aerogel of step (3), the method that obtains nitrogenous multi-stage porous three-dimensional grapheme is: after the nitrogenous carbon aerogels that step (2) is obtained is pulverized, the amount that the mass ratio of NaOH and nitrogenous carbon aerogels of take is 3:1-5:1 joins the nitrogenous carbon aerogels powder making in the NaOH solution that concentration is 4-6wt%, stir 2-3h, obtain the mixed solution of nitrogenous carbon aerogels and NaOH; Then be placed on 80 ℃ dry until in mixed solution moisture evaporate completely, then proceed in tube furnace at N
2heat-up rate with 5 ℃/min under protective atmosphere activates 2-3h in 800-1000 ℃; With deionized water, the nitrogenous carbon aerogels suction filtration after activation is washed till to neutrality, then puts 50 ℃ and obtain nitrogenous multi-stage porous three-dimensional grapheme after dry.
2. utilize according to claim 1 chitosan to prepare the method for nitrogenous multi-stage porous three-dimensional grapheme, it is characterized in that: described in step (2), carbonization temperature is 800 ℃.
3. utilize according to claim 1 chitosan to prepare the method for nitrogenous multi-stage porous three-dimensional grapheme, it is characterized in that: described in step (3), the mass ratio of NaOH and nitrogenous carbon aerogels is 3:1.
4. utilize according to claim 1 chitosan to prepare the method for nitrogenous multi-stage porous three-dimensional grapheme, it is characterized in that: described in step (3), activation temperature is 900 ℃.
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