CN105845937B - A kind of method that three-dimensional porous carbon skeleton/graphene composite structure is constructed in original position - Google Patents
A kind of method that three-dimensional porous carbon skeleton/graphene composite structure is constructed in original position Download PDFInfo
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Abstract
A kind of method that three-dimensional porous carbon skeleton/graphene composite structure is constructed in original position is washed till pH=7 by the skin of thin wall type plant after sulfuric acid impregnates, and filters, obtains product B after drying；By NaOH, KOH, Ca (OH)2、Na2CO3、NaHCO3、K2CO3、KHCO3In any two kinds with mass ratio 1:9~9:1 be uniformly mixed, obtain product C；It is washed till pH=7 after calcining 0.5~3h at 500~1300 DEG C after product C and product B are mixed with quality 1:3~3:1, filters, is dry.The aperture of multistage distribution of the invention is conducive to the insertion abjection of sodium ion, the graphene-structured of generation is conducive to be promoted the electric conductivity of carbon material, more storage spaces are provided for the insertion of sodium ion, the specific surface area of material is increased simultaneously, be conducive to coming into full contact with for electrolyte and material, to improve the cycle performance and high rate performance of sodium-ion battery.
Description
Technical field
The present invention relates to a kind of preparation methods of the sodium ion carbon material used as anode of morphology controllable, and in particular to a kind of original position structure
The method for building three-dimensional porous carbon skeleton/graphene composite structure.
Background technique
With the development of science and technology with the arrival of information-intensive society, the desired strength of electrochmical power source is gradually increased.Lithium-ion electric
Pond has the characteristics that high voltage, high-energy-density, therefore tremendous development is obtained in portable electrical power applications, but elemental lithium it is expensive and
Content is few in the earth's crust, and as it is gradually applied to electric car, the demand of lithium will be greatly increased.And lithium reserves it is limited and store up
Hiding is unevenly distributed, and can restrict extensive development [the Liu Chun Na foreign countries sodium-ion battery progress of long-life energy-storage battery
[J] power technology, 2014,38 (1): 12-13.].Therefore it is imperative other type batteries to be developed.
Sodium-ion battery is one of the battery of current most researching value.Compared with lithium ion battery, it is advantageous that its
Density is high, it means that their quality can store more greatly more energy, be suitable for extensive energy storage.Meanwhile raw material provides
Source is rich and easy to get, low in cost；It can be used to the lower electrolyte solvent of decomposition potential and electrolytic salt, the range of choice of electrolyte
It is wider；There is metastable chemical property, use is safer.Therefore, they can afford sustainable green energy resource exploitation
Important task, have powerful vitality and development potentiality [Ye Feipeng, Wang Li, Lian Fang etc. sodium-ion battery progress [J]
Work progress, 2013,32 (8): 1789-1795.].
But the screening of anode material of lithium-ion battery faces some problems.Since sodium ion radius is greater than lithium ion half
Diameter, the ion cathode material lithium graphite layers of traditional commodities are not appropriate for insertion and the abjection [Miao Yan of sodium ion away from too small
It is beautiful, the river Liu Xing anode material of lithium-ion battery progress [J] power technology, 2015,39 (2): 23-25.] it is necessary to have
Other storage sodium materials such as the carbon material and alloy of bigger interlamellar spacing or hole.In storage sodium negative electrode material, carbon based negative electrodes material is
Study most commonly used material.The carbon material of optimum sodium insertion in order to obtain, the assembling in addition to carrying out carbon using template, also
It can be prepared using naturally occurring plant.
Researchers have been found that peat moss [Jia D, Huanlei W, Zhi L, et al.Carbon at present
nanosheet frameworks derived from peat moss as high performance sodium ion
Battery anodes. [J] .Acs Nano, 2013,7 (12): 11004-11015.], banana skin [Lotfabad E M, Ding
J,Cui K,et al.High-Density Sodium and Lithium Ion Battery Anodes from Banana
Peels [J] .Acs Nano, 2014,8 (7): 7115-7129.], sucrose [Hong K L, Long Q, Zeng R, et
al.Biomass derived hard carbon used as a high performance anode material for
Sodium ion batteries [J] .J.mater.chem.a, 2014,2 (32): 12733-12738.], peanut shell [Lv W,
Wen F,Xiang J,et al.Peanut shell derived hard carbon as ultralong cycling
anodes for lithium and sodium batteries[J].Electrochimica Acta,2015,176:533-
541.] it etc. can be used to prepare the carbon negative pole material of suitable sodium ion insertion abjection.The advantages of this carbon material, is in original
There is the pore structure for forming multistage distribution on the basis of material, increases the contact area of electrolyte and material, promote carbon material
Chemical property.But its preparation process is complex, and is unordered accumulation between layer and layer, particle and particle, is unfavorable for electricity
Solve the complete infiltration of liquid.
Summary of the invention
The purpose of the present invention is using the thin wall types such as peanut skin, garlic skin, onion skin plant tissue as raw material, presoma is carried out acid
Immersion treatment and different types of alkali are activated, and by rationally controlling reaction temperature, obtain area load graphene-structured
Three-dimensional carbon skeleton porous material, the material are applied to sodium-ion battery and have good cycle performance.
To achieve the above object, The technical solution adopted by the invention is as follows:
A kind of method that three-dimensional porous carbon skeleton/graphene composite structure is constructed in original position, comprising the following steps:
(1) skin of thin wall type plant is obtained into suspending liquid A after sulfuric acid impregnates；
(2) it by suspending liquid A distilled water flushing to pH=7, filters, obtain product B after drying；
(3) by NaOH, KOH, Ca (OH)2、Na2CO3、NaHCO3、K2CO3、KHCO3In any two kinds with mass ratio 1:9
~9:1 is uniformly mixed, and obtains product C；
(4) it under argon gas protection, is forged at 500~1300 DEG C after product C and product B are mixed with quality 1:3~3:1
0.5~3h is burnt, product D is obtained；
(5) product D is washed till pH=7, filters, obtains three-dimensional porous carbon skeleton/graphene composite structure after drying.
The skin of thin wall type plant is peanut skin, garlic skin or onion skin in the step (1).
The concentration of sulfuric acid is 1mol/L~14mol/L in the step (1).
The ratio of the skin and sulfuric acid of thin wall type plant is 2.0~10.0g:50mL in the step (1).
The temperature impregnated in the step (1) is 80 DEG C, and the time is 0.1~5h.
It impregnates in the step (1) and carries out in an oven.
The flow velocity of argon gas is 0.1~0.5sccmmin in the step (4)-1。
With 1~40 DEG C of min in the step (4)-1Heating rate be warming up to 500~1300 DEG C.
Compared with prior art, the invention has the benefit that
(1) present invention by raw material of thin wall type plant prepares porous carbon materials, and thin wall type plant structure is simple, contain there are many
Organic matter is easy under the collective effect for being chemically treated and being heat-treated, and destroys its internal hemicellulose and partial lignin,
Its surface generates hole, forms three-dimensional porous stably and controllable structure；
(2) sulfuric acid, which impregnates, to carry out dehydration and pre- carbonization to thin wall type plant to a certain extent, and removes in plant
The organic matters such as glucose, xylose, furfural possessed by itself provide condition for the activation of later period alkali, reduce Post isothermal treatment
Required energy.
(3) it is activated using different alkali mixing, reaction ratio and different calcination temperatures by control alkali, due to
Alkali and carbon reaction rate at high temperature are different, on the basis of acid soak early period, can produce the aperture of multistage distribution and
In area load graphene-structured；
(4) aperture of multistage distribution is conducive to the insertion abjection of sodium ion, and the graphene-structured of generation is conducive to promote carbon
The electric conductivity of material provides more storage spaces for the insertion of sodium ion, while increasing the specific surface area of material, favorably
In coming into full contact with for electrolyte and material, to further increase the cycle performance and high rate performance of sodium-ion battery.
Detailed description of the invention
Fig. 1 is SEM figure of the product under low range under embodiment 2.
Fig. 2 is SEM figure of the product under high magnification under embodiment 2.
Fig. 3 is SEM figure of the product under low range under embodiment 4.
Fig. 4 is SEM figure of the product under high magnification under embodiment 4.
Fig. 5 is the sodium-ion battery cycle performance comparison diagram that under embodiment 2 and embodiment 4 prepared by product.
Specific embodiment
The present invention is described in detail with reference to the accompanying drawing.
Embodiment 1
(1) it by peanut skin cleaning, drying, is sealed；
(2) 5.0g peanut skin is weighed, is placed in a beaker, the sulfuric acid 50mL that concentration is 5mol/L is added, in 80 DEG C of baking oven
Middle immersion 2h, obtains suspending liquid A；
(3) it by product A distilled water flushing to pH=7, is filtered with suction filter pump, obtains product B after dry；
(4) KOH and NaOH is uniformly mixed to get product C with mass ratio 1:2；
(5) product B and product C 1:3 in mass ratio are placed in low temperature tube furnace, under protection of argon gas, and argon gas
Flow velocity is 0.1sccmmin-1, with 5 DEG C of min-1Heating rate be warming up to 800 DEG C of calcination temperature, and keep the temperature 3h, produced
Object D；
(6) by product D distilled water flushing to pH=7, filtered with suction filter pump, obtained after dry three-dimensional porous carbon skeleton/
Graphene composite structure.
Embodiment 2
(1) it by peanut skin cleaning, drying, is sealed；
(2) 6.0g peanut skin is weighed, is placed in a beaker, the sulfuric acid 50mL that concentration is 3mol/L is added, in 80 DEG C of baking oven
Middle immersion 2h, obtains suspending liquid A；
(3) it by product A distilled water flushing to pH=7, is filtered with suction filter pump, obtains product B after dry；
(4) by KOH and NaHCO3Product C is mixed to get with the mass ratio of 1:1；
(5) product C and product B are uniformly mixed with mass ratio 3:1, is placed in low temperature tube furnace, under protection of argon gas, and
And the flow velocity of argon gas is 0.3sccmmin-1, with 5 DEG C of min-1Heating rate be warming up to 900 DEG C of calcination temperature, and keep the temperature
2h obtains product D；
(5) by product D distilled water flushing to pH=7, filtered with suction filter pump, obtained after dry three-dimensional porous carbon skeleton/
Graphene composite structure.
Referring to Fig. 1 and Fig. 2, it can be seen that in control sulfuric acid concentration be 3mol/L, product C and product B from Fig. 1 and Fig. 2
When mass ratio is 3:1, in the surface of the carbon aperture different with internal generation size distribution, i.e. three-dimensional carbon skeleton structure, carbon surface
Lesser fold is generated, is graphene-structured, the graphene-structured size generated under this condition is smaller.
Embodiment 3
(1) it by onion skin cleaning, drying, is sealed；
(2) 7.0g onion skin is weighed, is placed in a beaker, the sulfuric acid 50mL that concentration is 10mol/L is added, in 80 DEG C of baking oven
1h is impregnated, suspending liquid A is obtained；
(3) it by product A distilled water flushing to pH=7, is filtered with suction filter pump, obtains product B after dry；
(4) by Ca (OH)2And Na2CO3Product C is uniformly mixed to get with mass ratio 1:1；
(5) product B and product C 1:2 in mass ratio are placed in low temperature tube furnace, under protection of argon gas, and argon gas
Flow velocity is 0.5sccmmin-1, with 5 DEG C of min-1Heating rate be warming up to 1000 DEG C of calcination temperature, and keep the temperature 1h, obtain
Product D；
(5) by product D distilled water flushing to pH=7, filtered with suction filter pump, obtained after dry three-dimensional porous carbon skeleton/
Graphene composite structure.
Embodiment 4
(1) it by peanut skin cleaning, drying, is sealed；
(2) 10.0g peanut skin is weighed, is placed in a beaker, the sulfuric acid 50mL that concentration is 6mol/L is added, in 80 DEG C of baking oven
Middle immersion 2h, obtains suspending liquid A；
(3) it by product A distilled water flushing to pH=7, is filtered with suction filter pump, obtains product B after dry；
(4) by KOH and NaHCO3It is mixed with the mass ratio of 1:1, obtains product C；
(5) product C and product B are uniformly mixed with mass ratio 1:1, is placed in low temperature tube furnace, under protection of argon gas, and
And the flow velocity of argon gas is 0.3sccmmin-1, with 5 DEG C of min-1Heating rate be warming up to 900 DEG C of calcination temperature, and keep the temperature
2h obtains product D；
(5) by product D distilled water flushing to pH=7, filtered with suction filter pump, obtained after dry three-dimensional porous carbon skeleton/
Graphene composite structure.
Referring to Fig. 3 and Fig. 4, it can be seen that in control sulfuric acid concentration be 6mol/L, product C and product B from Fig. 3 and Fig. 4
When mass ratio is 1:1, apertures equally different with internal generation size distribution on the surface of carbon, i.e. three-dimensional carbon skeleton structure, carbon
Surface generates biggish fold, i.e., the graphene-structured size generated under this condition is larger.
Referring to Fig. 5, three-dimensional carbon skeleton/graphene-structured material phase for being obtained under the conditions of embodiment 4 as can be seen from Figure 5
It is significantly mentioned than having in its high rate performance of three-dimensional carbon skeleton structural material and cycle performance for being obtained under the conditions of embodiment 2
It rises.It is 100mAg in current density-1Under conditions of, three-dimensional carbon skeleton/graphene-structured material capacity is 380mAhg-1, in 10Ag-1Still there is 200mAhg under current density-1, when current density returns to 100mAg-1, which remains to return to
Initial reversible capacity, and kept stable is remained to after the circle of circulation 220.
Embodiment 5
(1) in an oven, by garlic skin at 80 DEG C through 1mol/L sulfuric acid impregnate 0.1h after, obtain suspending liquid A；Wherein, garlic
The ratio of skin and sulfuric acid is 2g:50mL；
(2) it by suspending liquid A distilled water flushing to pH=7, filters, obtain product B after drying；
(3) by NaOH, NaHCO3It is uniformly mixed with mass ratio 1:9, obtains product C；
(4) under argon gas protection, and the flow velocity of argon gas is 0.1sccmmin-1, by product C and product B with quality 5:3 into
After row mixing, with 1 DEG C of min-1Heating rate be warming up to 500 DEG C, and calcine 3h at 500 DEG C, obtain product D；
(5) product D is washed till pH=7, filters, obtains three-dimensional porous carbon skeleton/graphene composite structure after drying.
Embodiment 6
(1) in an oven, by garlic skin at 80 DEG C through 14mol/L sulfuric acid impregnate 5h after, obtain suspending liquid A；Wherein, garlic skin
And the ratio of sulfuric acid is 3g:50mL；
(2) it by suspending liquid A distilled water flushing to pH=7, filters, obtain product B after drying；
(3) by NaOH, NaHCO3It is uniformly mixed with mass ratio 9:1, obtains product C；
(4) under argon gas protection, and the flow velocity of argon gas is 0.4sccmmin-1, by product C and product B with quality 7:3 into
After row mixing, with 30 DEG C of min-1Heating rate be warming up to 1300 DEG C, and calcine 0.5h at 1300 DEG C, obtain product D；
(5) product D is washed till pH=7, filters, obtains three-dimensional porous carbon skeleton/graphene composite structure after drying.
Embodiment 7
(1) in an oven, by peanut skin at 80 DEG C through 8mol/L sulfuric acid impregnate 0.5h after, obtain suspending liquid A；Wherein,
The ratio of peanut skin and sulfuric acid is 8g:50mL；
(2) it by suspending liquid A distilled water flushing to pH=7, filters, obtain product B after drying；
(3) by NaHCO3、KHCO3It is uniformly mixed with mass ratio 4:9, obtains product C；
(4) under argon gas protection, and the flow velocity of argon gas is 0.2sccmmin-1, by product C and product B with quality 2:1 into
After row mixing, with 15 DEG C of min-1Heating rate be warming up to 700 DEG C, and calcine 2h at 700 DEG C, obtain product D；
(5) product D is washed till pH=7, filters, obtains three-dimensional porous carbon skeleton/graphene composite structure after drying.
Embodiment 8
(1) in an oven, by garlic skin at 80 DEG C through 7mol/L sulfuric acid impregnate 3h after, obtain suspending liquid A；Wherein, garlic skin
And the ratio of sulfuric acid is 4g:50mL；
(2) it by suspending liquid A distilled water flushing to pH=7, filters, obtain product B after drying；
(3) by NaOH, NaHCO3It is uniformly mixed with mass ratio 5:9, obtains product C；
(4) under argon gas protection, and the flow velocity of argon gas is 0.5sccmmin-1, by product C and product B with quality 2:3 into
After row mixing, with 40 DEG C of min-1Heating rate be warming up to 1200 DEG C, and calcine 1h at 1200 DEG C, obtain product D；
(5) product D is washed till pH=7, filters, obtains three-dimensional porous carbon skeleton/graphene composite structure after drying.
Claims (5)
1. a kind of method that three-dimensional porous carbon skeleton/graphene composite structure is constructed in original position, which is characterized in that including following step
It is rapid:
(1) skin of thin wall type plant is obtained into suspending liquid A after 80 DEG C of sulfuric acid impregnates；
(2) it by suspending liquid A distilled water flushing to pH=7, filters, obtain product B after drying；
(3) by NaOH, KOH, Ca (OH)2、Na2CO3、NaHCO3、K2CO3、KHCO3In any two kinds with mass ratio 1:9~9:1
It is uniformly mixed, obtains product C；
(4) it under argon gas protection, is calcined at 500~1300 DEG C after product C and product B are mixed with mass ratio 1:3~3:1
0.5~3h obtains product D；
(5) product D is washed till pH=7, filters, obtains three-dimensional porous carbon skeleton/graphene composite structure after drying；
The skin of thin wall type plant is peanut skin, garlic skin or onion skin in the step (1)；
The concentration of sulfuric acid is 1mol/L~14mol/L in the step (1)；
The ratio of the skin and sulfuric acid of thin wall type plant is 2.0~10.0g:50mL in the step (1).
2. the method that three-dimensional porous carbon skeleton/graphene composite structure is constructed in a kind of original position according to claim 1, special
Sign is that the temperature impregnated in the step (1) is 80 DEG C, and the time is 0.1~5h.
3. the method that three-dimensional porous carbon skeleton/graphene composite structure is constructed in a kind of original position according to claim 1 or 2,
It is carried out in an oven it is characterized in that, being impregnated in the step (1).
4. the method that three-dimensional porous carbon skeleton/graphene composite structure is constructed in a kind of original position according to claim 1, special
Sign is that the flow velocity of argon gas is 0.1~0.5sccm in the step (4).
5. the method that three-dimensional porous carbon skeleton/graphene composite structure is constructed in a kind of original position according to claim 1, special
Sign is, with 1~40 DEG C of min in the step (4)-1Heating rate be warming up to 500~1300 DEG C.
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| CN107039193B (en) * | 2017-04-14 | 2018-10-19 | 山东大学 | A kind of garlic skin matrix activated carbon electrode material and preparation method for ultracapacitor |
| CN107611437A (en) * | 2017-09-13 | 2018-01-19 | 陕西科技大学 | A kind of preparation method of bar-shaped sodium-ion battery carbon material used as anode |
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| CN107611436A (en) * | 2017-09-13 | 2018-01-19 | 陕西科技大学 | A kind of method for the sodium-ion battery carbon electrode material that multi-pore micron structure is prepared based on peanut coat |
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| CN107473206A (en) * | 2017-09-13 | 2017-12-15 | 陕西科技大学 | A kind of method that grapheme material is prepared based on peanut coat |
| CN107611438A (en) * | 2017-09-13 | 2018-01-19 | 陕西科技大学 | A kind of method that highly basic activation peanut coat prepares spherical sodium-ion battery carbon material used as anode |
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| CN110817867A (en) * | 2019-12-12 | 2020-02-21 | 山东大学 | Preparation method and application of garlic skin based super activated carbon |
| CN112299405B (en) * | 2020-11-19 | 2022-04-22 | 福州大学 | Preparation method of low-temperature easily-graphitized three-dimensional biomass porous carbon with high specific surface area |
| CN113594441A (en) * | 2021-07-21 | 2021-11-02 | 昆明理工大学 | Method for preparing 3D high-capacity cathode material by metal salt assisted chemical etching method |
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