CN106744798A - A kind of method and its application that hard carbon is prepared using carbon containing biological mass shell - Google Patents
A kind of method and its application that hard carbon is prepared using carbon containing biological mass shell Download PDFInfo
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- CN106744798A CN106744798A CN201611140134.9A CN201611140134A CN106744798A CN 106744798 A CN106744798 A CN 106744798A CN 201611140134 A CN201611140134 A CN 201611140134A CN 106744798 A CN106744798 A CN 106744798A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The present invention relates to a kind of method for preparing hard carbon using carbon containing biological mass shell, comprise the following steps：According to the alkali in alkaline solution：The mass ratio of carbon containing biological mass shell powder is (1 20):1 amount, to carbon containing biological mass shell powder is added in alkaline solution, is designated as solution A；Solution A is injected in stainless steel cauldron and seals hydro-thermal, taken out after product cools to room temperature with the furnace, the carbon containing biological mass shell powder for being pre-processed；The carbon containing biological mass shell powder of pretreatment that will be obtained adds enough acid cleaning, and removes unnecessary inorganic salt impurities ion, obtains hard carbon presoma；The hard carbon presoma that will be obtained is carbonized under inert gas atmosphere, obtains B substance；The hard carbon material that will be obtained first removes silicon with enough acid, then is dried, and obtains hard carbon.The beneficial effects of the invention are as follows：With low in raw material price, abundant, industrialization degree is high, low cost of manufacture, it is easy to commercially produce, excellent performance, the characteristics of practicality is high.
Description
Technical field
The present invention relates to a kind of method and its application that hard carbon is prepared using carbon containing biological mass shell.
Background technology
A large amount of burnings of conventional fossil fuel cause energy crisis and serious environmental pollution, and renewable and clean energy resource is opened
Send out and utilize very urgent.However, though the renewable and clean energy resource such as new energy cleaning such as solar energy, wind energy is renewable,
Influenceed, than larger, have the shortcomings that unstable, discontinuous and uncontrollable, it is necessary to develop supporting storage by time period and weather etc.
Energy device is come the stability to ensure to generate electricity, power.Compared with other electrochemical energy storages, lithium ion battery has energy
Metric density is big, have extended cycle life, operating voltage is high, memory-less effect, the advantages of self discharge is small, operating temperature range is wide, just
Take formula electronic equipment, communication apparatus, static energy storage and the application in electric automobile field widely.But in large-scale energy storage side
Face, lithium ion battery is faced with high cost, short life, there are problems that, with lithium electricity industry development, to lithium
Demand it is increasing, and abundance of the lithium in the earth's crust is only 0.0065wt%, and skewness, exploitation are difficult, thereby result in
Lithium cost is raised, it is impossible to the need for meeting growing energy-storage battery.
Sodium is in same main group with lithium, and positioned at the lower section of lithium, therefore both physicochemical properties are closely similar.With lithium
Compare, abundance of the sodium in the earth's crust is 2.74wt%, aboundresources, exploitation is convenient, with low cost, safe.Meanwhile, sodium from
Sub- battery energy density is high, low cost, non-environmental-pollution, is very suitable for extensive stored energy application.Electrode material is sodium ion
The important component of battery.By the end of current, a series of development of positive electrodes has caused high-performance sodium-ion battery
Using being possibly realized.It is still a great challenge to find suitable anode material of lithium-ion battery.Graphite is with its work electricity
Position low, good cycling stability, excellent conductivity and it is cheap many advantages, such as, be always lithium ion battery negative material
Main flow.However, due to thermodynamic one, embedding sodium capacity of the graphite in traditional lipid electrolyte is but very low (35mAh/g).Its
His sodium cell negative pole material such as alloy, oxide, organic compound etc. exist structure collapses, capacity it is low, it is first effect low, electrical conductivity it is low
Problem, it is difficult to realize the application in lithium ion battery.Hard carbon anode material of lithium-ion battery reversible capacity is high, charging/discharging voltage
Platform is low, cycle performance is excellent, is expected to turn into the main flow negative material of sodium-ion battery.
The presoma of hard carbon mainly has high molecular polymer, and the hard carbon for obtaining is pyrolyzed using high molecular polymer, and performance is excellent
Different but expensive, the commercialization to it in sodium-ion battery is unfavorable.
The content of the invention
The technical problems to be solved by the invention be to provide it is a kind of using carbon containing biological mass shell prepare hard carbon method and its
Using to overcome above-mentioned deficiency of the prior art.
The technical scheme that the present invention solves above-mentioned technical problem is as follows：A kind of side that hard carbon is prepared using carbon containing biological mass shell
Method, comprises the following steps：
Step one, according to the alkali in alkaline solution：The mass ratio of carbon containing biological mass shell powder is (1-20):1 amount, to alkali
Carbon containing biological mass shell powder is added in property solution, solution A is designated as；
Step 2, by solution A inject stainless steel cauldron in, in 30 DEG C to 200 DEG C seal hydro-thermal 1h to 20h, treat product
Taken out after cooling to room temperature with the furnace, the carbon containing biological mass shell powder for being pre-processed；
The carbon containing biological mass shell powder of step 3, the pretreatment that will be obtained in step 2 adds enough acid cleaning, then with pure
Water washing removes unnecessary inorganic salt impurities ion to neutrality, obtains hard carbon presoma；
Step 4, the hard carbon presoma that will be obtained in step 3 under inert gas atmosphere, are carbonized in 800 DEG C to 1500 DEG C
2h to 10h, obtains B substance；
Step 5, the B substance that will be obtained in step 4 first remove silicon with enough acid, then are washed till neutrality with a large amount of clear water,
Finally dried, obtained hard carbon.
A kind of hard carbon as sodium-ion battery negative pole material application.
The beneficial effects of the invention are as follows：With low in raw material price, enrich, industrialization degree is high, low cost of manufacture, it is easy to
Commercially produce, excellent performance, the characteristics of practicality is high.
Brief description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph using the preparation-obtained hard carbon of the method for the invention；
Fig. 2 is the circulation tested after anode material of lithium-ion battery is made using preparation-obtained hard carbon of the invention
Figure；
Fig. 3 is the charging and discharging curve of obtained sodium-ion battery.
Specific embodiment
Principle of the invention and feature are described below in conjunction with accompanying drawing, example is served only for explaining the present invention, and
It is non-for limiting the scope of the present invention.
Embodiment one, as shown in figure 1, a kind of method for preparing hard carbon using carbon containing biological mass shell, comprises the following steps：
S01, the crushing of 20g mangosteen shells pulverizer is weighed, obtain mangosteen shell powder, and the mangosteen shell powder that will be obtained is uniform
It is dispersed in the sodium hydroxide solution that 100mL to 200mL concentration is 0.2M to 2M, wherein, the concentration of sodium hydroxide solution is optional
It is 0.2M, 0.4M, 0.7M, 0.82M, 0.9M, 1.2M, 1.43M, 1.7M, 1.9M, 2.0M, due to using mangosteen shell, by mountain
The influence of bamboo shell self-molecules present composition, the concentration of sodium hydroxide solution is preferably 0.9M, obtains solution A；
S02, by solution A inject stainless steel cauldron in, in 120 DEG C to 180 DEG C seal hydro-thermal 6h to 12h, the temperature of hydro-thermal
Degree can be 30 DEG C, 120 DEG C, 126.2 DEG C, 130.7 DEG C, 144.1 DEG C, 159.5 DEG C, 167.8 DEG C, 173.4 DEG C, 180 DEG C, 200 DEG C,
According to the concentration of preferred sodium hydroxide solution, drawn at this concentration by testing repeatedly, the temperature of hydro-thermal reaction it is optimal
It is 144.1 DEG C to be worth, and now, the reaction between mangosteen shell and NaOH is the most active, the hydro-thermal time can for 1h, 6h, 6.5h,
7.2h, 8.4h, 9.6h, 10.1h, 11.7h, 12h, 20h, but according to the concentration and hydro-thermal of optimal sodium hydroxide solution
Temperature, by test repeatedly draw this concentration and at a temperature of, hydro-thermal time optimal be 10.1h, treat that product cools to room with the furnace
Taken out after temperature, the mangosteen shell powder for being pre-processed；
S03, the mangosteen shell powder of the pretreatment that will be obtained in S02 add enough watery hydrochloric acid cleanings, then use pure water washing
To neutrality, and unnecessary inorganic salt impurities ion is removed, obtain hard carbon presoma；
S04, the hard carbon presoma that will be obtained in S03 are in N2Or under Ar atmosphere, be carbonized 2h to 10h in 800 DEG C to 1500 DEG C,
The temperature of carbonization can be 800 DEG C, 924 DEG C, 1011 DEG C, 1147 DEG C, 1265 DEG C, 1371 DEG C, 1424 DEG C, 1500 DEG C, by repeatedly
Experiment show that the hard carbon presoma obtained by mangosteen shell is 1265 DEG C in the Optimal Temperature value being carbonized, and carbonization time can be
2h, 3.2h, 4.7h, 6.1h, 7.4h, 8.6h, 9.3,10h, according to optimal carburizing temperature, draw, herein by testing repeatedly
At a temperature of carbonization time it is optimal be 7.4h, obtain B substance；
S05, the B substance that will be obtained in S04 first remove silicon with enough hydrofluoric acid, in being then washed till with a large amount of clear water again
Property, finally dried, obtain hard carbon.
Embodiment two：As shown in figure 1, a kind of method for preparing hard carbon using carbon containing biological mass shell, comprises the following steps：
S01, the crushing of 20g walnut shells pulverizer is weighed, obtain walnut shell powder, and the walnut shell powder that will be obtained is uniform
It is dispersed in the sodium hydroxide solution that 100mL to 200mL concentration is 0.2M to 2M, wherein, the concentration of sodium hydroxide solution is optional
It is 0.2M, 0.4M, 0.7M, 0.82M, 0.9M, 1.2M, 1.43M, 1.7M, 1.9M, 2.0M, due to using walnut shell, by core
The influence of peach shell self-molecules present composition, the concentration of sodium hydroxide solution is preferably 1.2M, obtains solution A；
S02, by solution A inject stainless steel cauldron in, in 120 DEG C to 180 DEG C seal hydro-thermal 6h to 12h, the temperature of hydro-thermal
Degree can be 30 DEG C, 120 DEG C, 126.2 DEG C, 130.7 DEG C, 144.1 DEG C, 159.5 DEG C, 167.8 DEG C, 173.4 DEG C, 180 DEG C, 200 DEG C,
According to the concentration of preferred sodium hydroxide solution, drawn at this concentration by testing repeatedly, the temperature of hydro-thermal reaction it is optimal
It is 126.2 DEG C to be worth, and now, the reaction between mangosteen shell and NaOH is the most active, the hydro-thermal time can for 1h, 6h, 6.5h,
7.2h, 8.4h, 9.6h, 10.1h, 11.7h, 12h, 20h, but according to the concentration and hydro-thermal of optimal sodium hydroxide solution
Temperature, by test repeatedly draw this concentration and at a temperature of, hydro-thermal time optimal be 11.7h, treat that product cools to room with the furnace
Taken out after temperature, the walnut shell powder for being pre-processed；
S03, the walnut shell powder of the pretreatment that will be obtained in S02 add enough watery hydrochloric acid cleanings, then use pure water washing
To neutrality, and unnecessary inorganic salt impurities ion is removed, obtain hard carbon presoma；
S04, the hard carbon presoma that will be obtained in S03 are in N2Or under Ar atmosphere, be carbonized 2h to 10h in 800 DEG C to 1500 DEG C,
The temperature of carbonization can be 800 DEG C, 924 DEG C, 1011 DEG C, 1147 DEG C, 1265 DEG C, 1371 DEG C, 1424 DEG C, 1500 DEG C, by repeatedly
Experiment show that the hard carbon presoma obtained by walnut shell is 1424 DEG C in the Optimal Temperature value being carbonized, and carbonization time can be
2h, 3.2h, 4.7h, 6.1h, 7.4h, 8.6h, 9.3h, 10h, according to optimal carburizing temperature, draw, herein by testing repeatedly
At a temperature of carbonization time it is optimal be 8.6h, obtain B substance；
S05, the B substance that will be obtained in S04 first remove silicon with enough hydrofluoric acid, in being then washed till with a large amount of clear water again
Property, finally dried, obtain hard carbon.
When raw material is mangosteen shell, after the temperature of hydro-thermal reaction is to final gained hard carbon first specific capacity and circulation 100 times
The influence of specific capacity, by testing repeatedly, draws following data, as shown in table 1：
Table 1
When raw material is walnut shell, after the temperature of hydro-thermal reaction is to final gained hard carbon first specific capacity and circulation 100 times
The influence of specific capacity, by testing repeatedly, draws following data, as shown in table 2：
Table 2
Hard carbon obtained by embodiment one or two is prepared into anode material of lithium-ion battery, and carries out experimental test, institute
As shown in Figure 2 and Figure 3, after 150mA/g current densities circulate 100 times, specific capacity is about 320mAhg-1 to the data for measuring.
Although embodiments of the invention have been shown and described above, it is to be understood that above-described embodiment is example
Property, it is impossible to limitation of the present invention is interpreted as, one of ordinary skill in the art within the scope of the invention can be to above-mentioned
Embodiment is changed, changes, replacing and modification.
Claims (10)
1. the method that a kind of carbon containing biological mass shell of utilization prepares hard carbon, it is characterised in that comprise the following steps：
Step one, according to the alkali in alkaline solution：The mass ratio of carbon containing biological mass shell powder is (1-20):1 amount, it is molten to alkalescence
Carbon containing biological mass shell powder is added in liquid, solution A is designated as；
Step 2, by solution A inject stainless steel cauldron in, in 30 DEG C to 200 DEG C seal hydro-thermal 1h to 20h, treat product with stove
Taken out after being cooled to room temperature, the carbon containing biological mass shell powder for being pre-processed；
Step 3, the carbon containing biological mass shell powder of the pretreatment that will be obtained in step 2 add enough acid cleaning, then use pure washing
Wash to neutrality, and remove unnecessary inorganic salt impurities ion, obtain hard carbon presoma；
Under inert gas atmosphere, the 2h that is carbonized in 800 DEG C to 1500 DEG C is arrived for step 4, the hard carbon presoma that will be obtained in step 3
10h, obtains B substance；
Step 5, the B substance that will be obtained in step 4 first remove silicon with enough acid, then are washed till neutrality with a large amount of clear water, finally
Dried, obtained hard carbon.
2. the method that a kind of carbon containing biological mass shell of utilization according to claim 1 prepares hard carbon, it is characterised in that the step
In rapid one, carbon containing biological mass shell is mangosteen shell.
3. the method that a kind of carbon containing biological mass shell of utilization according to claim 1 prepares hard carbon, it is characterised in that the step
In rapid one, carbon containing biological mass shell is walnut shell.
4. the method that a kind of carbon containing biological mass shell of utilization according to claim 1 prepares hard carbon, it is characterised in that the step
In rapid one, the alkali is NaOH.
5. the method that a kind of carbon containing biological mass shell of utilization according to claim 1 prepares hard carbon, it is characterised in that the step
In rapid two, hydrothermal temperature is 120 DEG C to 180 DEG C.
6. the method that a kind of carbon containing biological mass shell of utilization according to claim 1 prepares hard carbon, it is characterised in that the step
In rapid two, the hydro-thermal time is 1h to 20h.
7. the method that a kind of carbon containing biological mass shell of utilization according to claim 1 prepares hard carbon, it is characterised in that the step
In rapid three, the acid for being used is watery hydrochloric acid.
8. the method that a kind of carbon containing biological mass shell of utilization according to claim 1 prepares hard carbon, it is characterised in that the step
In rapid four, the acid for being used is hydrofluoric acid.
9. the method that a kind of carbon containing biological mass shell of utilization according to claim 1 prepares hard carbon, it is characterised in that the step
In rapid four, the inert gas atmosphere includes N2Or Ar.
10. it is a kind of according to any hard carbon of claim 1 to 9 as sodium-ion battery negative pole material application.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107681137A (en) * | 2017-09-20 | 2018-02-09 | 齐鲁工业大学 | A kind of sodium-ion battery C/C70/ CaS composite negative pole materials and preparation method thereof |
| CN107879323A (en) * | 2017-11-15 | 2018-04-06 | 上海空间电源研究所 | A kind of hard carbon material and its preparation method and application |
| CN108682815A (en) * | 2018-05-11 | 2018-10-19 | 浙江大学 | A kind of efficient hard carbon material and its preparation method and application |
| CN109467068A (en) * | 2018-11-01 | 2019-03-15 | 南昌航空大学 | A kind of preparation method of biological material Ba Danmu base porous carbon materials and its application in terms of anode of microbial fuel cell |
| WO2020208341A1 (en) * | 2019-04-09 | 2020-10-15 | Faradion Limited | Process for preparing and use of hard-carbon containing materials |
| CN114864934A (en) * | 2022-04-11 | 2022-08-05 | 温州大学碳中和技术创新研究院 | Preparation method and application of hazelnut shell hard carbon material for sodium ion battery cathode |
| CN116314730A (en) * | 2023-05-22 | 2023-06-23 | 江苏传艺科技股份有限公司 | Biomass-based carbon electrode material for sodium ion battery |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109467068A (en) * | 2018-11-01 | 2019-03-15 | 南昌航空大学 | A kind of preparation method of biological material Ba Danmu base porous carbon materials and its application in terms of anode of microbial fuel cell |
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| CN116314730A (en) * | 2023-05-22 | 2023-06-23 | 江苏传艺科技股份有限公司 | Biomass-based carbon electrode material for sodium ion battery |
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