CN106099089A - A kind of preparation method of anode material of lithium-ion battery biological carbon - Google Patents
A kind of preparation method of anode material of lithium-ion battery biological carbon Download PDFInfo
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- CN106099089A CN106099089A CN201610532952.7A CN201610532952A CN106099089A CN 106099089 A CN106099089 A CN 106099089A CN 201610532952 A CN201610532952 A CN 201610532952A CN 106099089 A CN106099089 A CN 106099089A
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- 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
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/133—Electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses the preparation method of a kind of anode material of lithium-ion battery biological carbon, pomelo peel is cleaned and is removed surface impurity by (1), shreds to obtain homogeneous bulky A；(2) homogeneous bulky A is carried out lyophilization and obtain block B；(3) carry out homogeneous reaction after adding concentrated sulphuric acid in block B, obtain product C；(4) move into carbonization in tube-type atmosphere furnace after being dried by product C sucking filtration, obtain carbonized product D；(5) by carbonized product D respectively with deionized water and soaked in absolute ethyl alcohol, washing sucking filtration, then it is dried, obtains the anode material of lithium-ion battery of chondritic.The biological carbon composition that the inventive method prepares is homogeneous, and purity is higher, and for finely dispersed chondritic, this kind of structure can effectively shorten sodium ion the evolving path, improves capacity and the stable circulation performance of sodium-ion battery.The raw material pomelo peel green non-pollution that the present invention uses, can realize turning waste into wealth, and preparation method is simple, and reaction temperature is low, and the response time is short, it is not necessary to subsequent treatment, environmentally friendly.
Description
Technical field
The invention belongs to anode material of lithium-ion battery preparation field, be specifically related to a kind of anode material of lithium-ion battery and use
The preparation method of biological carbon.
Background technology
The advantages such as lithium ion battery has that energy density is big, has extended cycle life, memory-less effect and be widely used in just
Take formula electronic market.But aggravation lithium ion battery relied on along with the industry such as the vehicles and large-scale power system, the whole world
Lithium resource will be unable to effectively meet the great demand of power lithium-ion battery, thus will raise further and lithium associated materials
Price, increases battery cost, the final development hindering New Energy Industry.Therefore, other cheap alternative lithium ion battery is developed
Relevant energy storage technology the most crucial.Sodium in the earth reserves than lithium high 4～5 orders of magnitude, and widely distributed, therefore use
Sodium-ion battery replaces lithium ion battery can alleviate the shortage of resources problem of lithium.Meanwhile, sodium element and elemental lithium are positioned at element week
The same main group of phase table, has similar physicochemical properties, and sodium-ion battery has the work similar with lithium ion battery
Make principle so that use similar compound to be possibly realized as electrode material in the two system.But due to sodium ion
Radius ratio lithium ion big, cause reversible capacity and high rate performance to reduce.What sodium-ion battery was studied it is critical only that novel height
The exploitation of performance electrode material, successful experience based on lithium ion battery, current research is concentrated mainly on positive electrode, as
The research of fruit lifting anticathode material will be greatly improved the performance of sodium-ion battery.
Fructus Citri grandis is one of first-class fruit of people's eating, belongs to Renewable resource, and ground is contained in China Guangxi, Sichuan, Hainan etc.
Produce, sell throughout all parts of the country.People the most only eat its meat, account for Fructus Citri grandis and weigh the pomelo peel of 54%～44% mostly by as useless
Material abandons, and not only pollutes environment, and wastes the resource being available for utilizing.Pomelo peel itself have abundant loose structure and in
Cellular characteristics, main component has pectin, cellulose and hemicellulose etc., is the precursor prepared of excellent biological carbon, has relatively
Organic plastid of large radius is possible not only to effectively increase the interlamellar spacing of material, for the quickly transmission offer condition of sodium ion, increases
The capacity of battery, it is also possible to form intramolecular hydrogen bond, the structure of stabilizing material, and then the cyclical stability of material can be improved.
If discarded pomelo peel can be recycled, preparing anode material of lithium-ion battery biological carbon, being possible not only to improve Fructus Citri grandis
The surcharge of son, reduce battery production cost, obtain considerable economic benefit, and can reduce because solid refuse brings
Environmental pollution.Additionally, biological carbon material prepared by pomelo peel also acts as lithium ion battery, sensor, ultracapacitor, have
Purposes widely and Research Prospects.
The method of preparation biological carbon mainly has at present is high temperature cabonization method.Lotfabad E M etc. with Pericarpium Musae as raw material,
In 1400 DEG C of tube furnaces, react 5h, more air-activated 3h in 300 DEG C of tube furnaces, obtain the sodium that specific capacity is 221mAh/g
Ion battery cathode material [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.].Luo W etc., with cellulose as raw material, react 2h in 1000 DEG C of tube furnaces, more air-activated under the conditions of 240 DEG C
8h, has obtained the anode material of lithium-ion battery that specific capacity is 176mAh/g.[Luo W.Carbon nanofibers
derived from cellulose nanofibers as a long-life anode material for
rechargeable sodium-ion batteries[J].J.mater.chem.a,2013,1(36):10662-10666.]。
Selvamani V etc., with Cortex Bulbus Allii as raw material, carry out pre-carbonization, afterwards carbonization 2h at 850 DEG C at 300 DEG C, are compared
Capacity be 145mAh/g anode material of lithium-ion battery [Selvamani V, Ravikumar R, Suryanarayanan V,
et al.Garlic peel derived high capacity hierarchical N-doped porous carbon
anode for sodium/lithium ion cell[J].Electrochimica Acta,2016,190:337-345.]。
Above-mentioned high temperature cabonization method needs to activate in atmosphere, or needs the process of impregnating active, there is course of reaction power consumption height, is difficult to
The shortcomings such as control, length reaction time, so finding a kind of simple, easily-controllable, method of Fast back-projection algorithm biomass carbon, to high-performance sodium
The research and development of ion battery cathode material is significant.
Summary of the invention
It is an object of the invention to provide the preparation method of a kind of anode material of lithium-ion battery biological carbon, on overcoming
Stating the defect that prior art exists, present invention process is simple to operate, reaction temperature is low, the cycle is short, the electrode obtained materials chemistry group
Become homogeneous, be uniformly dispersed.
For reaching above-mentioned purpose, the present invention adopts the following technical scheme that
The preparation method of a kind of anode material of lithium-ion battery biological carbon, comprises the following steps:
1) pomelo peel is cleaned removing surface impurity, shred to obtain homogeneous bulky A；
2) homogeneous bulky A is carried out lyophilization and obtain block B；
3) carry out homogeneous reaction after adding concentrated sulphuric acid regulation pH to 1～3 in block B, obtain product C；
4) move into carbonization under inert conditions in tube-type atmosphere furnace after being dried by product C sucking filtration, obtain carbonized product D；
5) carbonized product D is used deionized water and soak with ethanol, washing, then sucking filtration being dried, obtain mushy
Chondritic biological carbon.
Further, step 1) in homogeneous bulky A a diameter of 4～6mm.
Further, step 2) in cryodesiccated temperature be-9 DEG C～-5 DEG C, the time is 12～36h.
Further, step 3) in the concentration of concentrated sulphuric acid be 1～5mol L-1。
Further, step 3) in homogeneous reaction particularly as follows: with the heating rate of 6～15 DEG C/min by room temperature to
150 DEG C～200 DEG C and be incubated 12～24h, then naturally cool to room temperature.
Further, step 4) in carbonization particularly as follows: tube-type atmosphere furnace 10min is warmed up to 50 DEG C, 75min is warmed up to 500
～800 DEG C and be incubated 1～3h, then naturally cool to room temperature.
Further, step 5) in carbonized product D uses deionized water and soak with ethanol, washing particularly as follows: by carbonization
Product D first soaks 10min with deionized water, washs 5 times, uses soaked in absolute ethyl alcohol 10min the most again, washs 5 times.
Further, step 5) in the temperature that is dried be 80～110 DEG C, the time is 6～12h.
Compared with prior art, the present invention has a following useful technique effect:
The present invention uses pomelo peel to be raw material, use homogeneous, the preparation of carbonization two-step method is uniformly dispersed, uniform many
Hole spherical anode material of lithium-ion battery biological carbon.Homogeneous reaction can improve material to the absorption of energy and utilization rate, adds
Heat is uniformly and efficiency is higher, is substantially shorter manufacturing cycle, and concentrated sulphuric acid can hydrolyze the hemicellulose in pomelo peel, pectin, system
Pulp cellulose.The biological carbon prepared by the inventive method forms homogeneous, and purity is higher, for finely dispersed chondritic, this kind
Structure can effectively shorten sodium ion the evolving path, improve sodium-ion battery capacity and stable circulation performance.The present invention makes
Raw material pomelo peel green non-pollution, can realize turning waste into wealth, and preparation method is simple, reaction temperature is low, the response time
Short, it is not necessary to subsequent treatment, environmentally friendly.
Accompanying drawing explanation
Fig. 1 is that the scanning electron microscope (SEM) of the anode material of lithium-ion battery biological carbon of the embodiment of the present invention 1 preparation shines
Sheet；
Fig. 2 is the XRD figure spectrum of the anode material of lithium-ion battery of the embodiment of the present invention 1～4 preparation；
Fig. 3 is the anode material of lithium-ion battery of the embodiment of the present invention 1～4 preparation, under the electric current density of 50mA/g
Cycle performance figure, wherein YP500 represents that carburizing temperature is 500 DEG C, and YP600 represents that carburizing temperature is 600 DEG C, and YP700 represents carbon
Changing temperature is 700 DEG C, and YP800 represents that carburizing temperature is 800 DEG C.
Detailed description of the invention
Below embodiments of the present invention are described in further detail:
The preparation method of a kind of anode material of lithium-ion battery biological carbon, comprises the following steps:
1) by pomelo peel clean remove surface impurity, shred a diameter of 4～6mm homogeneous bulky A；
2) homogeneous bulky A is carried out lyophilization 12～36h at-9 DEG C～-5 DEG C and obtain block B；
3) adding concentration in block B is 1～5mol L-1Concentrated sulphuric acid regulation pH to 1～3 after, with 6～15 DEG C/min
Heating rate by room temperature to 150 DEG C～200 DEG C and be incubated 12～24h, then naturally cool to room temperature and obtain product
C；
4) carbonization under inert conditions in tube-type atmosphere furnace, tube-type atmosphere furnace are moved into after being dried by product C sucking filtration
10min is warmed up to 50 DEG C, and 75min is warmed up to 500～800 DEG C and is incubated 1～3h, then naturally cools to room temperature, obtains carbonization and produces
Thing D；
5) carbonized product D is first soaked 10min with deionized water, washs 5 times, use soaked in absolute ethyl alcohol 10min the most again,
Wash 5 times, then sucking filtration be dried 6～12h at 80～110 DEG C, obtain mushy chondritic biological carbon.
Below in conjunction with embodiment, the present invention is described in further detail:
Embodiment 1
(1) pomelo peel is cleaned removing surface impurity, shred to obtain a diameter of 4mm homogeneous bulky A；
(2) homogeneous bulky A is carried out lyophilization 12h temperature-9 DEG C and obtain block B；
(3) in block B, 2mol L is added-1Concentrated sulphuric acid, regulate pH to 1, then carry out homogeneous reaction, with 6 DEG C/min
Heating rate by room temperature to 150 DEG C and be incubated 12h, then naturally cool to room temperature, obtain product C；
(4) moving into logical nitrogen carbonization in tube-type atmosphere furnace after being dried by product C sucking filtration, carburizing temperature is by 10min liter
Temperature is to 50 DEG C, and 75min is warmed up to 500 DEG C, and is incubated 1h, then naturally cools to room temperature and obtains carbonized product D；
(5) carbonized product D is first soaked 10min with deionized water, wash 5 times, use soaked in absolute ethyl alcohol the most again
10min, washs 5 times.Then in 80 DEG C of vacuum drying ovens, it is dried 6h, obtains uniform concrete dynamic modulus chondritic biological carbon.
As seen from Figure 1, the biological carbon that prepared by this method for being uniformly dispersed, uniform chondritic.
Embodiment 2
(1) pomelo peel is cleaned removing surface impurity, shred to obtain a diameter of 6mm homogeneous bulky A；
(2) homogeneous bulky A is carried out lyophilization 18h temperature-8 DEG C and obtain block B；
(3) in block B, 3mol L is added-1Concentrated sulphuric acid, regulate pH to 2, then carry out homogeneous reaction, with 8 DEG C/min
Heating rate by room temperature to 160 DEG C and be incubated 16h, then naturally cool to room temperature, obtain product C；
(4) moving into logical nitrogen carbonization in tube-type atmosphere furnace after being dried by product C sucking filtration, carburizing temperature is by 10min liter
Temperature is to 50 DEG C, and 75min is warmed up to 600 DEG C, and is incubated 2h, then naturally cools to room temperature and obtains carbonized product D；
(5) carbonized product is first soaked 10min with deionized water, washs 5 times, use soaked in absolute ethyl alcohol 10min the most again,
Wash 5 times.Then in 90 DEG C of vacuum drying ovens, it is dried 8h, obtains concrete dynamic modulus chondritic biological carbon.
Embodiment 3
(1) pomelo peel is cleaned removing surface impurity, shred to obtain a diameter of 5mm homogeneous bulky A；
(2) homogeneous bulky A is carried out lyophilization 36h temperature-7 DEG C and obtain block B；
(3) in block B, 4mol L is added-1Concentrated sulphuric acid, regulate pH to 1, then carry out homogeneous reaction, with 10 DEG C/
The heating rate of min is by room temperature to 180 DEG C and is incubated 12h, then naturally cools to room temperature, obtains product C；
(4) moving into logical nitrogen carbonization in tube-type atmosphere furnace after being dried by product C sucking filtration, carburizing temperature is by 10min liter
Temperature is to 50 DEG C, and 75min is warmed up to 700 DEG C, and is incubated 1h, then naturally cools to room temperature and obtains carbonized product D；
(5) carbonized product is first soaked 10min with deionized water, washs 5 times, use soaked in absolute ethyl alcohol 10min the most again,
Wash 5 times.Then in 100 DEG C of vacuum drying ovens, it is dried 10h, obtains mushy chondritic biological carbon.
Embodiment 4
(1) pomelo peel is cleaned removing surface impurity, shred to obtain a diameter of 4mm homogeneous bulky A；
(2) homogeneous bulky A is carried out lyophilization 24h temperature-6 DEG C and obtain block B；
(3) in block B, 1mol L is added-1Concentrated sulphuric acid, regulate pH to 2, then carry out homogeneous reaction, with 12 DEG C/
The heating rate of min is by room temperature to 160 DEG C and is incubated 20h, then naturally cools to room temperature, obtains product C；
(4) moving into logical nitrogen carbonization in tube-type atmosphere furnace after being dried by product C sucking filtration, carburizing temperature is by 10min liter
Temperature is to 50 DEG C, and 75min is warmed up to 800 DEG C, and is incubated 2h, then naturally cools to room temperature and obtains carbonized product D；
(5) carbonized product is first soaked 10min with deionized water, washs 5 times, use soaked in absolute ethyl alcohol 10min the most again,
Wash 5 times.Then in 90 DEG C of vacuum drying ovens, it is dried 8h, obtains mushy chondritic biological carbon.
Embodiment 5
(1) pomelo peel is cleaned removing surface impurity, shred to obtain a diameter of 5mm homogeneous bulky A；
(2) homogeneous bulky A is carried out lyophilization 36h temperature-5 DEG C and obtain block B；
(3) in block B, 5mol L is added-1Concentrated sulphuric acid, regulate pH to 3, then carry out homogeneous reaction, with 15 DEG C/
The heating rate of min is by room temperature to 200 DEG C and is incubated 24h, then naturally cools to room temperature, obtains product C；
(4) moving into logical nitrogen carbonization in tube-type atmosphere furnace after being dried by product C sucking filtration, carburizing temperature is by 10min liter
Temperature is to 50 DEG C, and 75min is warmed up to 600 DEG C, and is incubated 3h, then naturally cools to room temperature and obtains carbonized product D；
(5) carbonized product is first soaked 10min with deionized water, washs 5 times, use soaked in absolute ethyl alcohol 10min the most again,
Wash 5 times.Then in 110 DEG C of vacuum drying ovens, it is dried 12h, obtains mushy chondritic biological carbon.
All there is a big peak bag, this explanation 2 θ ≈ about 24 ° in sample under different carburizing temperatures as seen from Figure 2
The material with carbon element of synthesis is made up of amorphous substance, belongs to amorphous carbon material.And in 44 ° of positions of X ray diffracting spectrum 2 θ ≈
One peak the shortest occurs, is similar to the peak of graphite.This material with carbon element synthesized by explanation belongs to amorphous carbon in terms of entirety,
But there is the trend of local graphite.This local graphite-like structure makes it have certain electric conductivity.From the figure 3, it may be seen that
The sodium-ion battery that under the carburizing temperature of 500～800 DEG C, this sample is made, after 500 circle circulations, capability retention is basically unchanged,
There is higher capacity and stable cycle performance.
Claims (8)
1. the preparation method of an anode material of lithium-ion battery biological carbon, it is characterised in that comprise the following steps:
1) pomelo peel is cleaned removing surface impurity, shred to obtain homogeneous bulky A；
2) homogeneous bulky A is carried out lyophilization and obtain block B；
3) carry out homogeneous reaction after adding concentrated sulphuric acid regulation pH to 1～3 in block B, obtain product C；
4) move into carbonization under inert conditions in tube-type atmosphere furnace after being dried by product C sucking filtration, obtain carbonized product D；
5) carbonized product D is used deionized water and soak with ethanol, washing, then sucking filtration being dried, obtain mushy spherical
Structure-biological carbon.
The preparation method of a kind of anode material of lithium-ion battery biological carbon the most according to claim 1, it is characterised in that
Step 1) in homogeneous bulky A a diameter of 4～6mm.
The preparation method of a kind of anode material of lithium-ion battery biological carbon the most according to claim 1, it is characterised in that
Step 2) in cryodesiccated temperature be-9 DEG C～-5 DEG C, the time is 12～36h.
The preparation method of a kind of anode material of lithium-ion battery biological carbon the most according to claim 1, it is characterised in that
Step 3) in the concentration of concentrated sulphuric acid be 1～5mol L-1。
The preparation method of a kind of anode material of lithium-ion battery biological carbon the most according to claim 1, it is characterised in that
Step 3) in homogeneous reaction particularly as follows: and be incubated by room temperature to 150 DEG C～200 DEG C with the heating rate of 6～15 DEG C/min
12～24h, then naturally cool to room temperature.
The preparation method of a kind of anode material of lithium-ion battery biological carbon the most according to claim 1, it is characterised in that
Step 4) in carbonization particularly as follows: tube-type atmosphere furnace 10min is warmed up to 50 DEG C, 75min be warmed up to 500～800 DEG C and be incubated 1～
3h, then naturally cools to room temperature.
The preparation method of a kind of anode material of lithium-ion battery biological carbon the most according to claim 1, it is characterised in that
Step 5) in use deionized water and soak with ethanol, washing particularly as follows: carbonized product D is first used deionized water carbonized product D
Soak 10min, wash 5 times, use soaked in absolute ethyl alcohol 10min the most again, wash 5 times.
The preparation method of a kind of anode material of lithium-ion battery biological carbon the most according to claim 1, it is characterised in that
Step 5) in be dried temperature be 80～110 DEG C, the time is 6～12h.
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Cited By (11)
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| CN107611435A (en) * | 2017-09-13 | 2018-01-19 | 陕西科技大学 | A kind of method that three-dimensional porous sodium-ion battery carbon material used as anode is prepared based on peanut coat |
| CN109244467A (en) * | 2018-11-30 | 2019-01-18 | 陕西科技大学 | A kind of method that herba setariae viridis grass prepares biological carbon negative pole material |
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| CN109592662B (en) * | 2018-11-30 | 2020-09-22 | 陕西科技大学 | Preparation method of biochar negative electrode material for lithium-sulfur battery |
| CN109546132A (en) * | 2018-11-30 | 2019-03-29 | 陕西科技大学 | A kind of preparation method of dandelion/sugar biological carbon composite construction |
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