CN109796004A - A kind of lithium cell cathode material and preparation method thereof and the lithium battery comprising the negative electrode material - Google Patents
A kind of lithium cell cathode material and preparation method thereof and the lithium battery comprising the negative electrode material Download PDFInfo
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- CN109796004A CN109796004A CN201910231665.6A CN201910231665A CN109796004A CN 109796004 A CN109796004 A CN 109796004A CN 201910231665 A CN201910231665 A CN 201910231665A CN 109796004 A CN109796004 A CN 109796004A
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- 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 lithium cell cathode material and preparation method thereof and comprising the lithium battery of the negative electrode material, the preparation method of the lithium cell cathode material is to choose protein content in the stalk material of 5%-12%, is dried for standby；Stalk material is handled into 1-4h in 80-150 DEG C of hydrochloric acid solution, obtains carbon matrix precursor；Carbon matrix precursor is mixed with KOH solution with the mass ratio of 1:3-6, impregnate 3-6h, then by carbon matrix precursor under 600-1000 DEG C of oxygen free condition high-temperature activation, be made carbonized product；Carbonized product is impregnated into 1-3h with hydrochloric acid solution again, it is dry after then being rinsed with deionized water to neutrality, it is made.The negative electrode material can effectively solve that specific capacity existing for existing carbon-based material is low, high rate performance decline and problem at high cost.
Description
Technical field
The invention belongs to electrode material manufacturing process areas, and in particular to a kind of lithium cell cathode material and preparation method thereof
With the lithium battery comprising the negative electrode material.
Background technique
As greenhouse effects lead to the lasting rising on sea level, the whole society is higher and higher to the attention rate of environment.It is same with this
When, demand of the expanding economy to the energy is increasing, and on the one hand the fossil energies such as traditional petroleum, coal, natural gas belong to
In non-renewable resources, on the other hand, their use brings serious environmental problem, and causing people urgently to need to develop can
The renewable sources of energy, to meet the sustainable development of economic society and environment.
Energy density is high, have extended cycle life and free of contamination lithium ion battery is exactly one of new energy sought by people.
Currently, in existing field of lithium, most of lithium ion battery negative materials be made of traditional carbon-based material, this
The traditional carbon-based material of kind is to be used to substituted metal lithium earliest as lithium ion battery negative material.And graphite is commodity
The carbon based negative electrodes material of change, theoretical capacity and high rate performance are lower, limit it in novel high-energy density lithium ion battery
In application.And the carbon-based material major part duct in single aperture is more tortuous, ionic pore conduction resistance is larger, and ion is mesoporous
Conduction resistance is smaller, and diffusion length is longer, and the above feature is all unfavorable for transmission of the ion in duct, ultimately causes electrode material
High rate performance decline.Moreover, the production technology of existing carbon-based material is complicated, and price per ton produces more than tens of thousands of members
Higher cost.
Biomass (lignocellulosics such as stalk, trees in agriculture and forestry production process in addition to grain, fruit, agricultural product
The substances such as processing industry leftover bits and pieces, agriculture and forestry organic waste material) energy, as a kind of important renewable energy, with relatively broad use
Way and good application value.How biomass is applied to field of lithium, is one of social assistant officer's problem to be solved now.
Summary of the invention
For the above-mentioned problems in the prior art, the present invention provides a kind of lithium cell cathode material and preparation method thereof
With the lithium battery comprising the negative electrode material, it is low which can effectively solve specific capacity existing for existing carbon-based material, times
The low and at high cost problem of rate performance.
To achieve the above object, the technical solution adopted by the present invention to solve the technical problems is:
A kind of preparation method of lithium cell cathode material, comprising the following steps:
(1) protein content is chosen in the stalk material of 5%-12% or more, is dried for standby；
(2) stalk material in step (1) is handled into 1-4h in 80-150 DEG C of acid solution, obtains carbon matrix precursor；
(3) carbon matrix precursor obtained in step (2) is mixed with KOH solution with the mass ratio of 1:3-6, impregnates 3-6h, so
After take out and activated under 600-1000 DEG C of oxygen free condition, carbonized product is made；
(4) carbonized product obtained in step (3) acid solution is impregnated into 1-3h, is then rinsed with deionized water into
Property after it is dry, be made.
Further, the stalk material in step (1) rich in protein is wheat stalk, rice straw, corn stover, oil
Dish stalk, cotton stalk or sugarcane stalk.
Further, the treatment process in step (2) is as follows: the stalk material in step (1) is taken, thereto with 1g stalk
Acid solution is added in the ratio that material corresponds to 80-150ml acid solution, then shakes under the conditions of 80-150 DEG C, 50-150r/min
1-4h is swung, finally, carbon matrix precursor is made in ultrasonic treatment 5-10min, filtering.
Further, the stalk material in step (1) is taken, 100ml acid solution is corresponded to 1g stalk material thereto
Acid solution is added in ratio, and 1.5-2.5h is then vibrated under the conditions of 115-125 DEG C, 80-120r/min, finally, ultrasonic treatment
Carbon matrix precursor is made in 5-8min, filtering.
Further, the acid solution is the hydrochloric acid solution of 0.5-2M.
Further, carbon matrix precursor obtained and the mass ratio of KOH solution are 1:3-4, dip time 3- in step (2)
4h, activation temperature is 700-900 DEG C to carbon matrix precursor under anaerobic.
Further, the concentration of KOH solution is 2-5M in step (3).
Adopt the lithium cell cathode material being prepared with the aforedescribed process.
A kind of lithium battery, including above-mentioned negative electrode material.
It is had the beneficial effect that caused by the present invention
1, it selects the higher stalk of protein content as biomass raw material in the present invention, is used to prepare Carbon anode material
Expect, handled in preparation process with acid solution, can avoid external world's doping process；The high stalk of protein content passes through KOH
After being reheated after solution processing, protein deformation therein, and poroid channel is formed in protein, so that stalk material
Three-dimensional porous carbon structure is formed, the performance of negative electrode material obtained is improved, the final specific capacity for improving carbon material, and
Preparation process of the invention is simple, and raw material is renewable, easily obtains, production cost can be reduced, at the same time it can also solve crop straw burning
The problem of bring environmental pollution.
2, it using KOH solution as activator in the present invention, is activated in the absence of oxygen, temperature increases, and KOH points
Solution is K2O is attached to the surface of carbon fiber, K2O starts to react in carbon fiber surface with carbon, finally etches in carbon fiber surface
Equally distributed micropore, the carbon for participating in reaction is released in the form of gaseous oxygen compound, while generating alkali metal potassium, metallic potassium
Continue to generate etching in unexposed carbon fiber, to increase the quantity of the microcellular structure of carbon fiber, and it is micro- to change carbon fiber
Fragrant planar structure and its electronics distribution situation in crystal, final metallic potassium gasify, and potassium vapor is micro- from what is etched
Hole is got among carbon-coating, and carbon-coating is made to bend, and is washed and be can remove metallic potassium, and curved carbon-coating just irrecoverable original state,
Finally obtain specific surface area increasing carbon fiber, lithium ion moved in the carbon fiber it is more smooth, finally, so that lithium-ion electric
The specific capacity and high rate performance in pond are improved.
3, stalk material is handled in the present invention using hydrochloric acid, can effectively remove be complexed on stalk existing potassium, calcium,
The metal cations such as sodium, magnesium, iron avoid above-mentioned metal cation from occupying vacancy in carbon material, prevent the insertion of lithium ion, shadow
Ring the trafficability performance of lithium ion；Meanwhile hydrochloric acid can remove hemicellulose and lignin etc. in biological material again, finally obtain
The relatively thin carbon matrix precursor of cell wall finally also can remove the alkaline matter generated during pore, improve the property of the negative electrode material
Energy.
Detailed description of the invention
Fig. 1 is the charge-discharge test figure of battery in embodiment 3；
Fig. 2 is the observation figure of negative electrode material under the microscope in embodiment 3.
Specific embodiment
Embodiment 1
A kind of preparation method of lithium cell cathode material, comprising the following steps:
(1) taking protein content is 5% corn stover, is dried for standby；
(2) hydrochloric acid is added with the ratio that 1g stalk corresponds to 80ml 0.5M hydrochloric acid into corn stover, then in 80 DEG C of conditions
1h is vibrated in the shaking table of lower 50r/min, finally, carbon matrix precursor is made in ultrasonic treatment 5min, filtering；
(3) carbon matrix precursor obtained in step (2) is mixed with 2M KOH solution with the mass ratio of 1:3, impregnates 3h, then
Taking-up activates 1h under 600 DEG C of oxygen free conditions, and carbonized product is made；
(4) it by carbonized product obtained in step (3) 0.5M salt acid soak 1h, is so rinsed with deionized water to neutrality
It is dry, it is made.
Embodiment 2
A kind of preparation method of lithium cell cathode material, comprising the following steps:
(1) taking protein content is 8% rice straw, is dried for standby；
(2) hydrochloric acid is added with the ratio that 1g stalk corresponds to 150ml 2M hydrochloric acid into rice straw, then in 150 DEG C of conditions
4h is vibrated in the shaking table of lower 150r/min, finally, carbon matrix precursor is made in ultrasonic treatment 10min, filtering；
(3) carbon matrix precursor obtained in step (2) is mixed with 5M KOH solution with the mass ratio of 1:6, impregnates 6h, then
Carbon matrix precursor is activated into 3h under 1000 DEG C of oxygen free conditions, carbonized product is made；
(4) it by carbonized product obtained in step (3) 2M salt acid soak 3h, is done after so being rinsed with deionized water to neutrality
It is dry, it is made.
A kind of lithium ion battery is made of above-mentioned negative electrode material.
Embodiment 3
A kind of preparation method of lithium cell cathode material, comprising the following steps:
(1) taking protein content is 12% wheat stalk, is dried for standby；
(2) hydrochloric acid is added with the ratio that 1g stalk corresponds to 100ml 1M hydrochloric acid into wheat stalk, then in 120 DEG C of conditions
2h is vibrated in the shaking table of lower 120r/min, finally, carbon matrix precursor is made in ultrasonic treatment 10min, filtering；
(3) carbon matrix precursor obtained in step (2) is mixed with 4M KOH solution with the mass ratio of 1:3, impregnates 4h, then
Taking-up activates 2h under 800 DEG C of oxygen free conditions, and carbonized product is made；
(4) it by carbonized product obtained in step (3) 1M salt acid soak 2h, is done after so being rinsed with deionized water to neutrality
It is dry, it is made.
Embodiment 4
A kind of preparation method of lithium cell cathode material, comprising the following steps:
(1) taking protein content is 10% cotton stalk, is dried for standby；
(2) hydrochloric acid is added with the ratio that 1g stalk corresponds to 130ml 1.5M hydrochloric acid into cotton stalk, then in 130 DEG C of items
3h is vibrated in the shaking table of 80r/min under part, finally, carbon matrix precursor is made in ultrasonic treatment 7min, filtering；
(3) carbon matrix precursor obtained in step (2) is mixed with 3M KOH solution with the mass ratio of 1:4, impregnates 5h, then
Taking-up activates 2h under 900 DEG C of oxygen free conditions, and carbonized product is made；
(4) it by carbonized product obtained in step (3) 1M salt acid soak 2h, is done after so being rinsed with deionized water to neutrality
It is dry, it is made.
Comparative example 1
A kind of preparation method of lithium cell cathode material, comprising the following steps:
(1) taking protein content is 12% wheat stalk, is dried for standby；
(2) hydrochloric acid is added with the ratio that 1g stalk corresponds to 60ml 0.8M hydrochloric acid into wheat stalk, then in 70 DEG C of conditions
2h is vibrated in the shaking table of lower 120r/min, finally, carbon matrix precursor is made in ultrasonic treatment 10min, filtering；
(3) carbon matrix precursor obtained in step (2) is mixed with 2M KOH solution with the mass ratio of 1:2, impregnates 4h, then
Taking-up activates 5h under 800 DEG C of oxygen free conditions, and carbonized product is made；
(4) it by carbonized product obtained in step (3) 1M salt acid soak 2h, is done after so being rinsed with deionized water to neutrality
It is dry, it is made.
Comparative example 2
A kind of preparation method of lithium cell cathode material, comprising the following steps:
(1) taking protein content is 12% wheat stalk, is dried for standby；
(2) hydrochloric acid is added with the ratio that 1g stalk corresponds to 100ml 1M hydrochloric acid into wheat stalk, then in 120 DEG C of conditions
2h is vibrated in the shaking table of lower 120r/min, finally, carbon matrix precursor is made in ultrasonic treatment 10min, filtering；
(3) carbon matrix precursor obtained in step (2) is mixed with 4M KOH solution with the mass ratio of 1:7, impregnates 4h, then
Taking-up activates 20min under 500 DEG C of oxygen free conditions, and carbonized product is made；
(4) it by carbonized product obtained in step (3) 1M salt acid soak 2h, is done after so being rinsed with deionized water to neutrality
It is dry, it is made.
Comparative example 3
A kind of preparation method of lithium cell cathode material, comprising the following steps:
(1) taking protein content is 12% wheat stalk, is dried for standby；
(2) phosphoric acid is added with the ratio that 1g stalk corresponds to 100ml 1M phosphoric acid into wheat stalk, then in 120 DEG C of conditions
2h is vibrated in the shaking table of lower 120r/min, finally, carbon matrix precursor is made in ultrasonic treatment 10min, filtering；
(3) carbon matrix precursor obtained in step (2) is mixed with 4M NaOH solution with the mass ratio of 1:3, impregnates 4h, so
After take out and activate 2h under 800 DEG C of oxygen free conditions, carbonized product is made；
(4) it by carbonized product obtained in step (3) 1M salt acid soak 2h, is done after so being rinsed with deionized water to neutrality
It is dry, it is made.
Negative electrode material made from above-described embodiment 1-4 and comparative example 1-3 is used to assemble lithium ion battery, was specifically assembled
Journey is as follows: using the porous carbon materials of preparation as active material, Kynoar (PVDF) is used as adhesive, and acetylene black is used as and leads
Electric agent, is sufficiently mixed by the mass ratio of 80:10:10, and a certain amount of N methyl pyrrolidone (NMP) is then added as solvent, fills
Divide and is mixed into slurry.Slurry is uniformly coated on copper foil with scraper, electrode plates are made after rolling in drying.By manufactured electricity
Pole piece uses metal lithium sheet as to electrode, being assembled into 2032 mould of bipolar electrode button in glove box as negative electrode of lithium ion battery
Quasi- battery, is made.
Test example
Experiment one, loop test experiment
Loop test carried out respectively to lithium battery obtained in embodiment 1-4 and comparative example 1-3, voltage regime when test
For 0-3V, current density 0.1A/g.Specific testing result is shown in Table 1 and Fig. 1.
Table 1:
It is learnt by table 1, the initial discharge specific capacity of lithium battery obtained in 1-4 of the embodiment of the present invention, after circulation 100 times
Specific discharge capacity, initial charge specific capacity and circulation 100 times after charge specific capacity be superior to the lithium in comparative example 1-3 electricity
Pond, it was demonstrated that according to lithium battery specific capacity with higher obtained in the present invention.
As can be seen that the specific capacity of the battery in the embodiment of the present invention 3 is higher in Fig. 1.
Experiment two, high rate performance experiment
To lithium battery obtained in embodiment 1-4 and comparative example 1-3 respectively in the voltage range of 0-3V, 0.1A/g-5A/g
Current density under the multiplying powers charge-discharge test such as carry out, the results are shown in Table 2.
Learnt by table 2, the reversible specific capacity in embodiment 1-4 it is bigger than the reversible specific capacity in comparative example 1-3, and
Reversible specific capacity decrease speed in embodiment 1-4 is slower than reversible specific capacity decrease speed in comparative example 1-3, it was demonstrated that embodiment
The high rate performance of 1-4 is better than comparative example, and the high rate performance of especially embodiment 3 is optimal.
Claims (9)
1. a kind of preparation method of lithium cell cathode material, which comprises the following steps:
(1) protein content is chosen in the stalk material of 5%-12%, is dried for standby；
(2) stalk material in step (1) is handled into 1-4h in 80-150 DEG C of acid solution, obtains carbon matrix precursor；
(3) carbon matrix precursor obtained in step (2) is mixed with KOH solution with the mass ratio of 1:3-6, impregnates 3-6h, then takes
1-3h is activated under 600-1000 DEG C of oxygen free condition out, carbonized product is made；
(4) carbonized product obtained in step (3) acid solution is impregnated into 1-3h, is then rinsed with deionized water to neutrality
It is dry, it is made.
2. the preparation method of lithium cell cathode material as described in claim 1, which is characterized in that step is rich in described in (1)
The stalk material of protein is wheat stalk, rice straw, corn stover, rape stalk, cotton stalk or sugarcane stalk.
3. the preparation method of lithium cell cathode material as described in claim 1, which is characterized in that processed in step (2)
Journey is as follows: taking the stalk material in step (1), is added thereto with the ratio that 1g stalk material corresponds to 80-150ml acid solution
Then acid solution vibrates 1-4h under the conditions of 80-150 DEG C, 50-150r/min, finally, ultrasonic treatment 5-10min, filtering,
Carbon matrix precursor is made.
4. the preparation method of lithium cell cathode material as claimed in claim 3, which is characterized in that take the stalk in step (1)
Acid solution is added thereto with the ratio that 1g stalk material corresponds to 100ml acid solution in material, then at 115-125 DEG C,
1.5-2.5h is vibrated under the conditions of 80-120r/min, finally, carbon matrix precursor is made in ultrasonic treatment 5-8min, filtering.
5. the preparation method of lithium cell cathode material as described in claim 3 or 4, which is characterized in that the acid solution is
The hydrochloric acid solution of 0.5-2M.
6. the preparation method of lithium cell cathode material as described in claim 1, which is characterized in that carbon obtained in step (2)
Presoma and the mass ratio of KOH solution are 1:3-4, and dip time 3-4h, activation temperature is carbon matrix precursor under anaerobic
700-900℃。
7. the preparation method of lithium cell cathode material as described in claim 1 or 6, which is characterized in that KOH is molten in step (3)
The concentration of liquid is 2-5M.
8. the lithium cell cathode material being prepared using the described in any item methods of claim 1-7.
9. a kind of lithium battery, which is characterized in that including negative electrode material according to any one of claims 8.
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Cited By (2)
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| CN110615436A (en) * | 2019-09-27 | 2019-12-27 | 内蒙古科技大学 | Method for preparing N-doped porous carbon composite lithium battery negative electrode material by utilizing coal humic acid extraction residues |
| CN111453730A (en) * | 2020-04-10 | 2020-07-28 | 电子科技大学 | Preparation method of biomass derived carbon nanosheet and supercapacitor thereof |
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| EP2060535A1 (en) * | 2007-04-04 | 2009-05-20 | Sony Corporation | Porous carbon materials and production process thereof,and adsorbents, masks, adsorbing sheets and carriers |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110615436A (en) * | 2019-09-27 | 2019-12-27 | 内蒙古科技大学 | Method for preparing N-doped porous carbon composite lithium battery negative electrode material by utilizing coal humic acid extraction residues |
| CN111453730A (en) * | 2020-04-10 | 2020-07-28 | 电子科技大学 | Preparation method of biomass derived carbon nanosheet and supercapacitor thereof |
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