CN110054177A - Graphene multi-stage porous carbon material and preparation method thereof and lithium ion battery - Google Patents
Graphene multi-stage porous carbon material and preparation method thereof and lithium ion battery Download PDFInfo
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- CN110054177A CN110054177A CN201810231697.1A CN201810231697A CN110054177A CN 110054177 A CN110054177 A CN 110054177A CN 201810231697 A CN201810231697 A CN 201810231697A CN 110054177 A CN110054177 A CN 110054177A
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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
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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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
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/32—Size or surface area
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- 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
- Y02E60/10—Energy storage using batteries
Abstract
The present invention provides a kind of graphene multi-stage porous carbon material and preparation method thereof.The preparation method includes under an inert atmosphere, the carbonate of lignin and alkali metal being carried out calcination processing, so that sp in the lignin3Carbon atom is eliminated, and obtains the first product；Carrying out washing treatment several times is carried out to first product using acid solution, the carbonate of the alkali metal is removed, obtains graphene multi-stage porous carbon material.This method one-step calcination obtains graphene multi-stage porous carbon material, on the one hand realizes the high-value-use of lignin, on the other hand simply and efficiently obtains graphene multi-stage porous carbon material, is beneficial to energy conservation consumption reduction, and the graphene multi-stage porous carbon material obtained.Based on its higher electric conductivity, in conjunction with its biggish specific surface area and good porous performance, by power-assisted, it is applied to the energy storages fields such as lithium ion battery and electrode material for super capacitor.The graphene more a greater amount of preparation of low price is realized in this research, and opens up and expand application of the biomass in electrochemical energy.
Description
Technical field
The invention belongs to grapheme material technical fields, and in particular to a kind of graphene multi-stage porous carbon material and its preparation side
Method and lithium ion battery.
Background technique
Graphene is one kind by sp2Hydbridized carbon atoms it is tightly packed at hexangle type be in honeycomb lattice Two-dimensional Carbon nanometer material
Material, due to being widely used in material, micro-nano technology, the energy, biomedicine with characteristics such as excellent optics, electricity, mechanics
With the fields such as drug delivery.Graphene powder production method common at present is mechanical stripping method, oxidation-reduction method, SiC extension
Growth method；And graphene film production method is chemical vapour deposition technique (CVD), these production methods or technical process are cumbersome,
Equipment requirement height causes production cost high, therefore people attempt new graphene production method.
Application No. is 201410226474.8 Chinese invention patents, disclose a kind of three-dimensional classifying porous Carbon Materials of graphene
Preparation method, this method is by by the biomass materials such as coconut husk, palm shell and apricot shell and Ethylenedinitrilotetraacetic Acid disodium complexing agent
It is reacted in solution, and the obtained filter residue of reaction is handled with hydrogen peroxide, acetic acid, nitric acid, potassium chloride, and will be obtained
Product carries out carbonization and obtains carbonized material, is then activated carbonized material and composite activating agent, deionized water, obtains graphite
The three-dimensional classifying porous Carbon Materials of alkene.The preparation method, raw material is various, needs first hydro-thermal process raw material, to obtain carbonized material, then
Carbonized material is subjected to high-temperature process, reaction process is complicated, and technique is cumbersome, and production efficiency is low.
Summary of the invention
Cumbersome for current graphene preparation process, the problems such as production efficiency is low, it is more that the present invention provides a kind of graphene
Grade hole carbon material and preparation method thereof.
Further, the present invention also provides a kind of lithium ion batteries.
For achieving the above object, technical scheme is as follows:
A kind of preparation method of graphene multi-stage porous carbon material, at least includes the following steps:
Under an inert atmosphere, the carbonate of lignin and alkali metal is subjected to calcination processing, so that sp in the lignin3
Carbon atom is eliminated, and obtains the first product；
Carrying out washing treatment several times is carried out to first product using acid solution, is removed the carbonate of the alkali metal,
Obtain graphene multi-stage porous carbon material.
Correspondingly, a kind of graphene multi-stage porous carbon material, the graphene multi-stage porous carbon material use stone as described above
The preparation method of black alkene multi-stage porous carbon material is prepared.
Further, a kind of lithium ion battery, the positive conductive agent of the lithium ion battery and/or cathode conductive agent are using upper
State the graphene multi-stage porous carbon material that the preparation method of graphene multi-stage porous carbon material is prepared.
The beneficial effects of the present invention are: compared with the existing technology, the present invention is using lignin as raw material, with alkali metal carbonic acid
Salt is catalyst, and one-step calcination obtains graphene multi-stage porous carbon material, on the one hand realizes the high-value-use of lignin, another party
Face simply and efficiently obtains graphene multi-stage porous carbon material, is beneficial to energy conservation consumption reduction, and the graphene multi-stage porous carbon materials obtained
Material possesses biggish specific surface area and good porous performance, and by power-assisted, it is applied to lithium ion battery and super capacitor electrode
The energy storages such as pole material field.The graphene more a greater amount of preparation of low price is realized in this research, and opens up and expand biomass
Application in electrochemical energy.This preparation method simple process, it is low for equipment requirements, it is suitble to large-scale production.
Detailed description of the invention
It to describe the technical solutions in the embodiments of the present invention more clearly, below will be to needed in the embodiment
Attached drawing is briefly described, it should be apparent that, drawings in the following description are only some embodiments of the invention, for ability
For the those of ordinary skill of domain, without creative efforts, it can also be obtained according to these attached drawings other attached
Figure.
Fig. 1 is the SEM figure of graphene multi-stage porous carbon material prepared by the embodiment of the present invention 1；
Fig. 2 is the SEM figure of graphene multi-stage porous carbon material prepared by the embodiment of the present invention 2；
Fig. 3 is the SEM figure of graphene multi-stage porous carbon material prepared by the embodiment of the present invention 3；
Fig. 4 is the SEM figure of graphene multi-stage porous carbon material prepared by the embodiment of the present invention 4；
Fig. 5 is the Raman map of graphene multi-stage porous carbon material prepared by the embodiment of the present invention 4 and unsetting carbon；
Fig. 6 is graphene multi-stage porous carbon material graph of pore diameter distribution prepared by the embodiment of the present invention 4；
Fig. 7 is graphene multi-stage porous carbon material nitrogen adsorption desorption curve prepared by the embodiment of the present invention 4.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.It should be appreciated that described herein, specific examples are only used to explain the present invention, not
For limiting the present invention.
Present example provides a kind of preparation method of graphene multi-stage porous carbon material, at least includes the following steps:
Under an inert atmosphere, the carbonate of lignin and alkali metal is subjected to calcination processing, so that sp in the lignin3
Carbon atom is eliminated, and obtains the first product；
Carrying out washing treatment several times is carried out to first product using acid solution, is removed the carbonate of the alkali metal,
Obtain graphene multi-stage porous carbon material.
Technical solution of the present invention is further explained in detail below.
One of raw material of the invention lignin, it is preferable that it is wooden to can be alkali lignin, lignosulfonates, sulfonation alkali
Element, sulfonation enzymolysis xylogen, carboxylated alkali lignin, carboxylated enzymolysis xylogen, ammonium choline lignin, ammonium enzymolysis xylogen
At least one of.Used lignin is eventually converted into graphene multi-stage porous carbon material, but also may be implemented in graphite
The elements such as nitrogen are adulterated in alkene multi-stage porous carbon material.The electric conductivity and stability of graphene can be improved, simultaneously in graphene nitrating
The active sites of graphene surface adsorbing metal particles can be increased, to enhance the interaction of metallic and graphene.It is logical
It crosses and graphene multi-stage porous carbon material is obtained to lignin progress calcination processing, realize the high-value-use of lignin, while being also stone
Black alkene material provides new preparation method.
Preferably, the carbonate of alkali metal is at least one of lithium carbonate, sodium carbonate, potassium carbonate.The carbonic acid of alkali metal
Salt during the reaction, plays the role of catalyst, when the carbonate mixture of lignin and alkali metal is in atmosphere of inert gases
In and at 600 DEG C of temperature or more, due to the sp in lignin3The activity of hydbridized carbon atoms is higher than sp2The work of hydbridized carbon atoms
Property, it can be prior to sp2Hydbridized carbon atoms react with catalyst, and during the reaction, the carbonate of alkali metal is reduced to gold
While belonging to simple substance, sp3Hydbridized carbon atoms are removed in the form of carbon monoxide, remove sp3Carbon graphite after hydbridized carbon atoms
Crystallite can be moved freely in the molten state and be reset, and be combined into graphene skeleton.
It is further preferred that according to mass ratio, the lignin: the carbonate of alkali metal=(1~2): (2~3).
Before calcining, preferably to be calcined, first the carbonate of lignin and alkali metal is mixed, is ground, is made
Reaction raw materials come into full contact with.
Preferably, calcination temperature is 600~1000 DEG C.When temperature reaches 600 DEG C or more, the sp in lignin3Hydridization
Carbon atom can be prior to sp2Hydbridized carbon atoms react with catalyst, and during the reaction, the carbonate of alkali metal is reduced to
While metal simple-substance, sp3Hydbridized carbon atoms are removed in the form of carbon monoxide, remove sp3Carbon graphite after hydbridized carbon atoms
Change crystallite can move freely in the molten state to be reset, and graphene skeleton is combined into.
It is further preferred that being first warming up to 600~650 DEG C according to 10~15 DEG C/min in calcination process, 2~3h is kept the temperature,
900 DEG C or more then are heated to the heating rate of 10~20 DEG C/min again, maintains at least 5h, it is naturally cold under an inert atmosphere
But.
Preferably, the acid solution is any one of dilute sulfuric acid, dilute hydrochloric acid, dust technology.Dilute sulfuric acid, dilute hydrochloric acid, dust technology
The carbonate contained in the material obtained with calcining reacts, so that carbonate and graphene multi-stage porous carbon material occur to divide
From to achieve the purpose that elution.
And when due to being eluted using acid solution to graphene multi-stage porous carbon material, graphene multi-stage porous carbon material becomes acid
Property, it is not available, further includes being cleaned repeatedly using deionized water to the graphene multi-stage porous carbon material after acid solution washing, clearly
It is washed till eluate to be in neutrality, then it is assumed that graphene multi-stage porous carbon material is qualified.
The preparation method of the graphene multi-stage porous carbon material of the above-mentioned offer of the present invention, using alkali carbonate as catalyst,
One-step calcination obtains graphene multi-stage porous carbon material, on the one hand realizes the high-value-use of lignin, on the other hand simply and efficiently
Obtain graphene multi-stage porous carbon material, be beneficial to energy conservation consumption reduction, and the graphene multi-stage porous carbon material of acquisition possess it is biggish
Specific surface area and good porous performance, by power-assisted, it is applied to the energy such as lithium ion battery and electrode material for super capacitor
Field of storage.The graphene more a greater amount of preparation of low price is realized in this research, and opens up and expand biomass in electrochemical energy
In application.The preparation method simple process, it is low for equipment requirements, it is suitble to large-scale production.
Specifically, a kind of lithium ion battery, positive conductive agent and/or cathode conductive agent are the above method of the present invention preparation
Obtain graphene multi-stage porous carbon material.Due to the graphene multi-stage porous carbon material that lithium ion battery is obtained using the present invention, gather around
Have bigger specific surface area and hole so that lithium ion battery electric conductivity more preferably, lithium ion mobility it is more efficient so that
Lithium ion battery shows good chemical property.
More effectively to illustrate technical solution of the present invention, technology of the invention is illustrated below by multiple specific embodiments
Scheme.
Embodiment 1
A kind of preparation method of graphene multi-stage porous carbon material, comprising the following steps:
(1) the pre- carbonization treatment of alkali lignin: in a nitrogen atmosphere, alkali lignin is added with the heating rate of 10 DEG C/min
Heat keeps the temperature 2h to 650 DEG C, and at 650 DEG C；
(2) alkali lignin after 10g being carbonized in advance is mixed with 20g Anhydrous potassium carbonate, and mixed material is obtained after milled processed；
(3) in a nitrogen atmosphere, mixed material step (2) obtained carries out calcination processing, and heating rate is 10 DEG C/
Min is warming up to 900 DEG C, and keeps the temperature 12h at 900 DEG C, then cooled to room temperature under nitrogen atmosphere, obtains black powder
End；
(4) it is cleaned repeatedly 3 times using the black powder that dilute hydrochloric acid obtains step (3), then using deionized water cleaning 3
Secondary, pH test paper is detected to neutrality, naturally dry, obtains graphene multi-stage porous carbon material, for use.
Embodiment 2
A kind of preparation method of graphene multi-stage porous carbon material, comprising the following steps:
(1) the pre- carbonization treatment of alkali lignin: in a nitrogen atmosphere, alkali lignin is added with the heating rate of 10 DEG C/min
Heat keeps the temperature 2h to 650 DEG C, and at 650 DEG C；
(2) alkali lignin after 10g being carbonized in advance is mixed with 20g Carbon Dioxide lithium, and mixed material is obtained after milled processed；
(3) in a nitrogen atmosphere, mixed material step (2) obtained carries out calcination processing, and heating rate is 10 DEG C/
Min is warming up to 900 DEG C, and keeps the temperature 12h at 900 DEG C, then cooled to room temperature under nitrogen atmosphere, obtains black powder
End；
(4) it is cleaned repeatedly 3 times using the black powder that dilute hydrochloric acid obtains step (3), then using deionized water cleaning 3
Secondary, pH test paper is detected to neutrality, naturally dry, obtains graphene multi-stage porous carbon material, for use.
Embodiment 3
A kind of preparation method of graphene multi-stage porous carbon material, comprising the following steps:
(1) the pre- carbonization treatment of alkali lignin: in a nitrogen atmosphere, alkali lignin is added with the heating rate of 10 DEG C/min
Heat keeps the temperature 2h to 650 DEG C, and at 650 DEG C；
(2) alkali lignin after 10g being carbonized in advance is mixed with 20g natrium carbonicum calcinatum, and mixed material is obtained after milled processed；
(3) in a nitrogen atmosphere, mixed material step (2) obtained carries out calcination processing, and heating rate is 10 DEG C/
Min is warming up to 900 DEG C, and keeps the temperature 12h at 900 DEG C, then cooled to room temperature under nitrogen atmosphere, obtains black powder
End；
(4) it is cleaned repeatedly 3 times using the black powder that dilute hydrochloric acid obtains step (3), then using deionized water cleaning 3
Secondary, pH test paper is detected to neutrality, naturally dry, obtains graphene multi-stage porous carbon material, for use.
Embodiment 4
A kind of preparation method of graphene multi-stage porous carbon material, comprising the following steps:
(1) it is ground after mixing 10g alkali lignin with 10g natrium carbonicum calcinatum, obtains mixed material；
(2) in a nitrogen atmosphere, mixed material step (1) obtained carries out calcination processing, according to the liter of 10 DEG C/min
Warm speed is warming up to 650 DEG C, keeps the temperature 2h, continues to be warming up to 900 DEG C with the heating rate of 10 DEG C/min, keeps the temperature 12h, then certainly
It is so cooled to room temperature, obtains black powder；
(3) it is cleaned repeatedly 3 times using the black powder that dilute hydrochloric acid obtains step (2), then using deionized water cleaning 3
Secondary, pH test paper is detected to neutrality, naturally dry, obtains graphene multi-stage porous carbon material, for use.
In order to verify the characteristic for the graphene multi-stage porous carbon material that embodiment 1,2,3,4 is prepared, it is carried out below
Relevant performance test.
(1) SEM is scanned
The graphene multi-stage porous carbon material that Examples 1 to 4 is prepared carries out SEM scanning, obtains as shown in figures 1-4
SEM picture, it can be seen that the carbon three that is surrounded by the diversified graphene of the sheet number of plies being largely cross-linked with each other from Fig. 1~4
Tie up structure.
(2) Raman spectrum
The unsetting carbon of lignin-base is drawn respectively after the graphene multi-stage porous carbon material obtain to embodiment 4 and pre- carbonization
The test of graceful spectrum, test results are shown in figure 5.
As can be seen from Figure 5, the graphene multi-stage porous carbon material that embodiment 4 obtains is clear that 1350cm-1(peak D),
1583cm-1(peak G), 1620cm-1(peak D '), 2440cm-1(peak T+D), 2699cm-1(peak 2D), 2947cm-1Peaks such as (peaks D+G).
Wherein the peak D, G, 2D is three mostly important graphene characteristic peaks.In contrast, what lignin-base was formed after being carbonized in advance is indefinite
Shape carbon only has 1350cm-1(peak D) and 1583cm-1(peak G) two obvious peaks and the faint peak T+D (2440cm-1)。
(3) aperture performance test
Pore-size distribution test is carried out to the graphene multi-stage porous carbon material that embodiment 4 obtains, test results are shown in figure 6.
As can be seen from Figure 6, there is the graphene obtained very flourishing micropore (< 2nm) to be distributed, in conjunction with the nitrogen adsorption desorption of Fig. 7
0.5-0.9P/P is appeared in curve0Hysteretic loop under opposite pressure conditions, there are also a large amount of mesoporous for the graphene shown
Distribution, demonstrates the property of its multi-stage porous.
(4) nitrogen adsorption desorption is tested
The test of nitrogen adsorption desorption, test result such as Fig. 7 institute are carried out to the graphene multi-stage porous carbon material that embodiment 4 obtains
Show.
As can be seen from Figure 7, the graphene multi-stage porous carbon material specific surface area obtained reaches 425m2/ g, Kong Rong reach 0.32cm3/
G, average pore size 3.0nm.The relatively high adsorption capacity that (P/P0 < 0.2) has under low opposite pressure conditions of its in Fig. 7 demonstrates
Its big specific surface area.
In the present invention, since the graphene multi-stage porous carbon material property homogeneity of the invention obtained is relatively good, embodiment
1,2,3 test for not carrying out Raman spectrum, aperture performance, nitrogen De contamination, only Example 4 is as representing.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc. within mind and principle should all include within protection scope of the present invention.
Claims (9)
1. a kind of preparation method of graphene multi-stage porous carbon material, which is characterized in that at least include the following steps:
Under an inert atmosphere, the carbonate of lignin and alkali metal is subjected to calcination processing, so that sp in the lignin3Carbon is former
Son is eliminated, and obtains the first product；
Carrying out washing treatment several times is carried out to first product using acid solution, the carbonate of the alkali metal is removed, obtains
Graphene multi-stage porous carbon material.
2. the preparation method of graphene multi-stage porous carbon material as described in claim 1, which is characterized in that the calcination temperature is
750~1000 DEG C.
3. such as the preparation method of the described in any item graphene multi-stage porous carbon materials of claim 1~2, which is characterized in that described
Lignin is alkali lignin, lignosulfonates, sulfonated wheat-strew lignin, sulfonation enzymolysis xylogen, carboxylated alkali lignin, carboxyl
Change at least one of enzymolysis xylogen, ammonium choline lignin, ammonium enzymolysis xylogen.
4. such as the preparation method of the described in any item graphene multi-stage porous carbon materials of claim 1~2, which is characterized in that described
The carbonate of alkali metal is at least one of lithium carbonate, sodium carbonate, potassium carbonate.
5. such as the preparation method of the described in any item graphene multi-stage porous carbon materials of claim 1~2, which is characterized in that according to
Mass ratio, the lignin: the carbonate of alkali metal=(1~2): (2~3).
6. such as the preparation method of the described in any item graphene multi-stage porous carbon materials of claim 1~2, which is characterized in that described
Inert gas used in inert atmosphere is any one of nitrogen, argon gas, helium, neon.
7. such as the preparation method of the described in any item graphene multi-stage porous carbon materials of claim 1~2, which is characterized in that described
Acid solution is any one of dilute hydrochloric acid, dilute sulfuric acid, dust technology.
8. a kind of graphene multi-stage porous carbon material, which is characterized in that the graphene multi-stage porous carbon material by such as claim 1~
The preparation method of 7 described in any item graphene multi-stage porous carbon materials is prepared.
9. a kind of lithium ion battery, which is characterized in that the positive conductive agent of the lithium ion battery and/or cathode conductive agent are by such as
The graphene multi-stage porous carbon that the preparation method of the described in any item graphene multi-stage porous carbon materials of claim 1~7 is prepared
Material provides.
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