CN111439738A - Biomass hard carbon, lithium ion battery, preparation method and application thereof - Google Patents
Biomass hard carbon, lithium ion battery, preparation method and application thereof Download PDFInfo
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- H01M10/05—Accumulators with non-aqueous electrolyte
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Abstract
The invention discloses a biomass hard carbon and lithium ion battery, a preparation method and application thereof, the preparation method comprises the following steps of dipping biomass powder in a mixed solution, filtering, washing to be neutral and drying to obtain a material A, pre-carbonizing and crushing the material A to obtain carbon-containing biomass powder with the D50 of 5-8 mu m, carbonizing a mixture of the carbon-containing biomass powder, a lithium-containing compound, an N-containing compound and a P-containing compound to obtain the biomass hard carbon and lithium ion battery, wherein the concentration of a substance for removing silicon in the mixed solution is 1-10 mol/L, the concentration of a substance for removing metal in the mixed solution is 1-10 mol/L, the dipping time is 5-72h, and the mass ratio of the carbon-containing biomass powder, the lithium-containing compound, the N-containing compound and the P-containing compound is 120 (6-48) to (6-48).
Description
Technical Field
The invention relates to a biomass hard carbon and lithium ion battery, and a preparation method and application thereof.
Background
Biomass hard charcoal is one of hard carbon materials, which is a material of particular interest in the environmental and energy fields in recent years, and has gained a great deal of research and application in terms of energy storage and conversion, and the like. The biomass is a natural precursor for preparing the carbon material, and has the advantages of wide source, low price, easy acquisition, environmental friendliness and the like. The hard carbon material is widely used as a high-performance lithium ion battery cathode material due to high capacity and good rate performance. However, the hard carbon material has loose and porous surface, is easy to absorb moisture and oxygen in the air, forms various C-H functional groups on the surface, and lithium ions are easy to react with the functional groups to cause the loss of the lithium ions, increase the irreversible capacity, reduce the first efficiency, and further hinder the wide application of the hard carbon material.
However, the biomass hard carbon prepared by the preparation method of the biomass hard carbon negative electrode material disclosed in patent document CN 106299365 a has large irreversible specific capacity and low first efficiency. Therefore, the problem to be solved is to find a biomass hard carbon with smaller irreversible capacity and higher first efficiency.
Disclosure of Invention
The invention aims to overcome the defects of large irreversible capacity and low first efficiency of the conventional hard carbon material, and provides a novel biomass hard carbon and lithium ion battery, and a preparation method and application thereof. The preparation method has the advantages of low raw material price, rich sources, low energy consumption, low equipment requirement, low cost, safety, reliability, simple process and suitability for industrial production. The hard carbon material prepared by the preparation method has the advantages of higher first charge-discharge specific capacity, smaller irreversible capacity, higher first efficiency, better rate capability and higher capacity retention rate.
The invention solves the technical problems through the following technical scheme:
the invention provides a preparation method of biomass hard carbon, which comprises the following steps:
(1) soaking biomass powder in the mixed solution, filtering, washing to neutrality and drying to obtain material A;
(2) pre-carbonizing and crushing the material A to obtain carbon-containing biomass powder D50 of 5-8 mu m;
(3) carbonizing the mixture of the carbon-containing biomass powder, the lithium-containing compound, the N-containing compound and the P-containing compound to obtain the lithium-containing biomass powder;
in the step (1), the mixed solution contains an aqueous solution of a silicon-removing substance and a metal-removing substance, the silicon-removing substance is HF, and the metal-removing substance is HCl or H2SO4、H3PO4And HNO3The concentration of the silicon-removing substances in the mixed solution is 1-10 mol/L, the concentration of the metal-removing substances in the mixed solution is 1-10 mol/L, and the soaking time is 5-72 h;
in the step (3), the mass ratio of the carbon-containing biomass powder to the lithium-containing compound to the N-containing compound to the P-containing compound is 120 (6-48) to (6-48).
In the step (1), the biomass powder may be a powder of biomass in the prior art, preferably one or more of peanut shell powder, walnut shell powder, coconut shell powder and pistachio nut shell powder, and more preferably peanut shell powder.
In the step (1), the metal removing substance is preferably HCl.
In the step (1), the ratio of the concentration of the silicon-removing substance to the concentration of the metal-removing substance in the mixed solution is preferably 0.5:1 to 2:1, and may be, for example, 1: 1.
In step (1), the time for the impregnation is preferably 20 to 28 hours, and may be 24 hours, for example.
In the step (1), the drying temperature may be 80 to 100 ℃. The drying may be vacuum drying. The drying time may be, for example, 8 to 10 hours.
In step (2), the temperature and time of the pre-carbonization may be conventional in the art. The temperature of the pre-carbonization can be, for example, 400-700 ℃ or 500 ℃. The pre-carbonization time can be 1-6h, and can also be 1-2 h. The pre-carbonization may be carried out in a shaft furnace as is conventional in the art.
In the step (2), the pulverization is preferably ball milling.
In step (3), the lithium-containing compound may be a lithium salt conventional in the art, and may be, for example, L iNO3。
In step (3), the N-containing compound may be a nitrogen-doping substance conventionally used in the art for hard carbon, and may be, for example, a nitrogen-containing organic substance, preferably urea and/or hexamethylenetetramine, more preferably urea or hexamethylenetetramine.
In step (3), the P-containing compound may be a phosphorus-doped substance conventionally used in the art for hard carbon, and may be, for example, a phosphorus-containing salt, preferably one or more of ammonium dihydrogen phosphate, ammonium phosphate, and diammonium hydrogen phosphate, and more preferably ammonium dihydrogen phosphate or ammonium phosphate.
In the step (3), the mass ratio of the carbon-containing biomass powder, the lithium-containing compound, the N-containing compound and the P-containing compound is preferably 120 (23-25): (23-25): 23-25), and may be 120:24:24:24, for example.
In the step (3), the mixture may be, for example, the carbon-containing biomass powder, the lithium-containing compound, the N-containing compound, and the P-containing compound, which are ball-milled and mixed uniformly.
In step (3), the carbonization atmosphere may be an inert atmosphere conventional in the art, for example, a nitrogen atmosphere. The temperature and time of the carbonization may be conventional in the art. The carbonization temperature may be, for example, 900 ℃ to 1200 ℃ or 1000 ℃. The carbonization time can be 2-6 h. The carbonization may be carried out in a tube furnace as is conventional in the art.
In a preferred embodiment of the above preparation method, in step (1), the biomass powder is peanut shell powder, the metal removing substance is HCl, the ratio of the concentration of the silicon removing substance to the concentration of the metal removing substance in the mixed solution is 0.5:1-2:1 (for example, 1:1), the immersion time is 20-28h (for example, 24h), and in step (3), the lithium-containing compound is L iNO3What is, what isThe N-containing compound is urea, the P-containing compound is ammonium dihydrogen phosphate, and the mass ratio of the carbon-containing biomass powder, the lithium-containing compound, the N-containing compound and the P-containing compound is 120 (23-25): 23-25) (for example, 120:24: 24). Wherein, more preferably, the D50 of the carbon-containing biomass powder is 8 μm.
The invention also provides biomass hard carbon prepared by the preparation method of the biomass hard carbon.
The invention also provides a lithium ion battery prepared from the biomass hard carbon.
The invention also provides application of the biomass hard carbon as a negative electrode material of a lithium ion battery.
The above preferred conditions can be arbitrarily combined to obtain preferred embodiments of the present invention without departing from the common general knowledge in the art.
The reagents and starting materials used in the present invention are commercially available.
The preparation method has the advantages of low raw material price, rich sources, low energy consumption, low equipment requirement, low cost, safety, reliability, simple process and suitability for industrial production. The hard carbon material prepared by the preparation method has the advantages of higher first charge-discharge specific capacity, smaller irreversible capacity, higher first efficiency, better rate capability and higher capacity retention rate.
Detailed Description
The invention is further illustrated by the following examples, which are not intended to limit the scope of the invention. The experimental methods without specifying specific conditions in the following examples were selected according to the conventional methods and conditions, or according to the commercial instructions.
In the following examples, button cells were fabricated by mixing the negative electrode materials of the cells prepared in examples 1-3 and comparative examples 1-5 with conductive agent and SBR in a ratio of 85:12:3, respectively, coating the mixture on a copper foil, vacuum drying the mixture to obtain a negative electrode, using lithium metal as a counter electrode, using a mixture of 1M L iPF6 Ethylene Carbonate (EC) and dimethyl carbonate (DMC) in a mass ratio of 1:1 as an electrolyte, and using a PE/PP/PE composite membrane as a separator under test conditions of charging and discharging at a current density of 0.1C and a charging voltage of 0.005-2V.
Example 1
The preparation method of the biomass hard charcoal comprises the following steps:
(1) weighing 600g of peanut shells, crushing the peanut shells by using a crusher to obtain peanut shell powder, uniformly dispersing the obtained peanut shell powder in a mixed solution, soaking the mixed solution in an aqueous solution containing HF and HCl, wherein the concentration of HF is 2 mol/L and is 2 mol/L, filtering, washing to be neutral, and vacuum-drying at 100 ℃ for 8 hours to obtain a material A;
(2) putting the material A into a shaft furnace, pre-carbonizing at 500 ℃ for 1h, and then ball-milling to obtain carbonaceous biomass powder with D50 of 8 mu m;
(3) 120g of carbonaceous biomass powder, 24g of L iNO324g of urea and 24g of ammonium dihydrogen phosphate, ball-milling and uniformly mixing, transferring to a tube furnace, and carbonizing for 2 hours at 1000 ℃ in a flowing nitrogen atmosphere to obtain the biomass hard carbon.
Example 2
The preparation method of the biomass hard charcoal comprises the following steps:
(1) weighing 600g of peanut shells, crushing the peanut shells by using a crusher to obtain peanut shell powder, uniformly dispersing the obtained peanut shell powder in a mixed solution, soaking for 72 hours, filtering, washing to be neutral, and vacuum-drying for 8 hours at 100 ℃ to obtain a material A, wherein the mixed solution is an aqueous solution containing HF and HCl, and the concentration of the HF is 1 mol/L and is 10 mol/L;
(2) putting the material A into a shaft furnace, pre-carbonizing for 2h at 500 ℃, and then ball-milling to obtain carbonaceous biomass powder with D50 of 6 microns;
(3) 120g of carbonaceous biomass powder, 48g of L iNO3And uniformly mixing 48g of urea and 48g of ammonium phosphate by ball milling, transferring the mixture into a tube furnace, and carbonizing the mixture for 6 hours at 1200 ℃ in a flowing nitrogen atmosphere to obtain the biomass hard carbon.
Example 3
The preparation method of the biomass hard carbon comprises the following steps:
(1) weighing 600g of peanut shells, crushing the peanut shells by using a crusher to obtain peanut shell powder, uniformly dispersing the obtained peanut shell powder in a mixed solution, soaking for 5 hours, filtering, washing to be neutral, and vacuum-drying for 8 hours at 100 ℃ to obtain a material A, wherein the mixed solution is an aqueous solution containing HF and HCl, and the concentration of the HF is 10 mol/L and is 1 mol/L;
(2) putting the material A into a shaft furnace, pre-carbonizing at 500 ℃ for 1h, and then ball-milling to obtain carbonaceous biomass powder with D50 of 5 microns;
(3) 120g of carbonaceous biomass powder, 6g of L iNO3And 6g of hexamethylenetetramine and 6g of ammonium phosphate are ball-milled and uniformly mixed, transferred into a tube furnace and carbonized for 2 hours at 900 ℃ in a flowing nitrogen atmosphere to obtain the biomass hard carbon.
Comparative example 1
The preparation method of the biomass hard carbon of the comparative example is the same as that of the example 1 except that the step (3) is different from the example 1, and the steps and conditions are the same as those of the example 1, wherein the step (3) is specifically as follows:
120g of carbonaceous biomass powder, 24g of L iNO3And 24g of ammonium dihydrogen phosphate, ball-milling and mixing uniformly, transferring to a tubular furnace, and carbonizing for 2h at 1000 ℃ in a flowing nitrogen atmosphere to obtain the biomass hard carbon.
Comparative example 2
The preparation method of the biomass hard carbon of the comparative example is the same as that of the example 1 except that the step (3) is different from the example 1, and the steps and conditions are the same as those of the example 1, wherein the step (3) is specifically as follows:
120g of carbonaceous biomass powder, 24g of L iNO3And 24g of urea, transferring the urea into a tube furnace, and carbonizing the urea for 2 hours at 1000 ℃ in a flowing nitrogen atmosphere to obtain the biomass hard carbon.
Comparative example 3
The preparation method of the biomass hard carbon of the comparative example is the same as that of the example 1 except that the step (3) is different from the example 1, and the steps and conditions are the same as those of the example 1, wherein the step (3) is specifically as follows:
and (3) uniformly mixing 120g of carbon-containing biomass powder, 24g of hexamethylenetetramine-containing biomass powder and 24g of ammonium dihydrogen phosphate by ball milling, transferring the mixture to a tubular furnace, and carbonizing the mixture for 2 hours at 1000 ℃ in a flowing nitrogen atmosphere to obtain the biomass hard carbon.
Comparative example 4
The preparation method of the biomass hard carbon of the comparative example is the same as that of the example 1 except that the step (3) is different from the example 1, and the steps and conditions are the same as those of the example 1, wherein the step (3) is specifically as follows:
120g of carbonaceous biomass powder and 24g of L iNO3And ball-milling and mixing uniformly, transferring the mixture into a tube furnace, and carbonizing the mixture for 2 hours at 1000 ℃ in a flowing nitrogen atmosphere to obtain the biomass hard carbon.
Comparative example 5
The preparation method of biomass hard carbon of the comparative example has the same steps (1) and (2) as example 1, but does not have step (3).
Comparative example 6
The preparation method of the biomass hard charcoal comprises the following steps:
(1) weighing 600g of peanut shells, crushing the peanut shells by using a crusher to obtain peanut shell powder, putting the obtained peanut shell powder into a well type furnace, pre-carbonizing the peanut shell powder for 1 hour at 500 ℃, and then ball-milling the peanut shell powder to obtain a material A with D50 of 8 mu m;
(2) uniformly dispersing the obtained material A in a mixed solution, wherein the mixed solution is an aqueous solution containing HF and HCl, the concentration of the HF is 2 mol/L and the concentration of the HF is 2 mol/L, soaking for 24 hours, filtering, washing to be neutral, and vacuum drying for 8 hours at 100 ℃ to obtain carbon-containing biomass powder;
(3) 120g of carbonaceous biomass powder, 24g of L iNO324g of urea and 24g of ammonium phosphate, ball-milling and mixing uniformly, transferring the mixture into a tube furnace, and carbonizing the mixture for 2 hours at 1000 ℃ in a flowing nitrogen atmosphere to obtain the biomass hard carbon.
Comparative example 7
The preparation method of the biomass hard charcoal comprises the following steps:
weighing 600g of peanut shells, crushing the peanut shells by using a crusher to obtain peanut shell powder, heating the peanut shells to 500 ℃ at the speed of 2 ℃/min in a well type furnace under the protection of Ar atmosphere (the flow rate of argon is 80sccm), preserving heat and presintering for 2h, cooling the peanut shells to room temperature along with the furnace, removing ions, cleaning, filtering and removing impurities, and performing vacuum drying at 120 ℃; then, heating to 1200 ℃ at the speed of 2 ℃/min, carrying out heat preservation and calcination for 2h, and cooling to room temperature along with the furnace to obtain an intermediate product;
placing the obtained intermediate product in a KOH solution with the concentration of 30 wt% for stirring and soaking for 2h (the stirring speed is 200rpm), filtering and taking out, placing the intermediate product in hydrochloric acid with the concentration of 3 mol/L for stirring and soaking for 12h (the stirring speed is 200rpm), then repeatedly washing with deionized water and filtering until the filtered washing water is neutral, placing the washed material in a vacuum drying oven for drying for 10h at the temperature of 120 ℃ to obtain a purified product;
placing the obtained purified product in a microwave oven, and performing microwave vacuum activation for 10s under 2000W microwave power and vacuum degree of 0.01Pa to obtain an activated product;
120g of the obtained activated product, 24g of L iNO324g of urea and 24g of ammonium dihydrogen phosphate, ball-milling and uniformly mixing, transferring to a tube furnace, and carbonizing for 2 hours at 1000 ℃ in a flowing nitrogen atmosphere to obtain the biomass hard carbon.
TABLE 1 electrochemical Performance test results of examples and comparative examples
From the test results in the table, the battery made of the biomass hard carbon prepared by the preparation method has the advantages of higher first charge-discharge specific capacity, higher first efficiency, better rate capability and higher capacity retention rate compared with the battery made of non-prelithiation and non-doping.
Claims (10)
1. The preparation method of the biomass hard carbon is characterized by comprising the following steps:
(1) soaking biomass powder in the mixed solution, filtering, washing to neutrality and drying to obtain material A;
(2) pre-carbonizing and crushing the material A to obtain carbon-containing biomass powder D50 of 5-8 mu m;
(3) carbonizing the mixture of the carbon-containing biomass powder, the lithium-containing compound, the N-containing compound and the P-containing compound to obtain the lithium-containing biomass powder;
in the step (1), the mixed solution contains an aqueous solution of a silicon-removing substance and a metal-removing substance, the silicon-removing substance is HF, and the metal-removing substance is HCl or H2SO4、H3PO4And HNO3The concentration of the silicon-removing substances in the mixed solution is 1-10 mol/L, the concentration of the metal-removing substances in the mixed solution is 1-10 mol/L, and the soaking time is 5-72 h;
in the step (3), the mass ratio of the carbon-containing biomass powder to the lithium-containing compound to the N-containing compound to the P-containing compound is 120 (6-48) to (6-48).
2. The method for preparing biomass hard carbon according to claim 1, wherein in the step (1), the biomass powder is one or more of peanut shell powder, walnut shell powder, coconut shell powder and pistachio nut shell powder, preferably peanut shell powder.
3. The method for preparing biomass hard carbon according to claim 1, wherein in the step (1), the metal removing substance is HCl.
4. The method for preparing biomass hard carbon according to claim 1, wherein in the step (1), the ratio of the concentration of the silicon-removing substance to the concentration of the metal-removing substance in the mixed solution is 0.5:1 to 2:1, preferably 1: 1;
and/or, in the step (1), the soaking time is 20-28h, preferably 24 h.
5. The method for preparing biomass hard carbon according to claim 1, wherein in the step (3), the lithium-containing compound is lithium salt, preferably L iNO3；
And/or, in the step (3), the N-containing compound is a nitrogen-containing organic substance, preferably urea and/or hexamethylenetetramine, more preferably urea or hexamethylenetetramine;
and/or, in the step (3), the P-containing compound is a phosphorus-containing salt, preferably one or more of ammonium dihydrogen phosphate, ammonium phosphate and diammonium hydrogen phosphate, and more preferably ammonium dihydrogen phosphate or ammonium phosphate;
and/or in the step (3), the mass ratio of the carbon-containing biomass powder, the lithium-containing compound, the N-containing compound and the P-containing compound is 120 (23-25) to (23-25) and preferably 120:24: 24.
6. The method for preparing biomass hard carbon according to claim 1, wherein in the step (1), the drying temperature is 80-100 ℃;
and/or, in the step (1), the drying is vacuum drying;
and/or, in the step (1), the drying time is 8-10 h;
and/or, in the step (2), the temperature of the pre-carbonization is 400-700 ℃, preferably 500 ℃;
and/or, in the step (2), the pre-carbonization time is 1-6h, preferably 1-2 h;
and/or, in the step (2), the crushing is ball milling;
and/or, in the step (3), the mixture is obtained by ball milling and uniformly mixing the carbon-containing biomass powder, the lithium-containing compound, the N-containing compound and the P-containing compound;
and/or in the step (3), the carbonization atmosphere is a nitrogen atmosphere;
and/or, in the step (3), the temperature of the carbonization is 900-1200 ℃, preferably 1000 ℃;
and/or in the step (3), the carbonization time is 2-6 h.
7. The method for preparing biomass hard carbon according to claim 1, wherein in the step (1), the biomass powder is peanut shell powder, the metal removing substance is HCl, and the mixed solution isThe ratio of the concentration of the silicon-removing substance to the concentration of the metal-removing substance is 0.5:1-2:1, the immersion time is 20-28h, and in the step (3), the lithium-containing compound is L iNO3The N-containing compound is urea, the P-containing compound is ammonium dihydrogen phosphate, and the mass ratio of the carbon-containing biomass powder, the lithium-containing compound, the N-containing compound and the P-containing compound is 120 (23-25): 23-25) (23-25); wherein, the D50 of the carbon-containing biomass powder is preferably 8 μm.
8. The biomass hard carbon is characterized by being prepared by the preparation method of the biomass hard carbon as claimed in any one of claims 1 to 7.
9. A lithium ion battery, wherein the lithium ions comprise the biomass hard carbon of claim 8.
10. Use of the biomass hard carbon of claim 8 as a negative electrode material for lithium ion batteries.
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| CN112687877A (en) * | 2020-12-24 | 2021-04-20 | 李树成 | Preparation method of super-high-magnification negative electrode material |
| CN115124025A (en) * | 2022-08-16 | 2022-09-30 | 中国石油大学(华东) | Hard carbon material, preparation method thereof and application thereof in sodium-ion battery |
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| CN115124025B (en) * | 2022-08-16 | 2023-07-21 | 中国石油大学(华东) | Hard carbon material, preparation method thereof and application thereof in sodium ion battery |
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