CN110040710A - A kind of Chinese parasol tree fruit hard charcoal poromerics and preparation method thereof - Google Patents
A kind of Chinese parasol tree fruit hard charcoal poromerics and preparation method thereof Download PDFInfo
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- CN110040710A CN110040710A CN201811573683.4A CN201811573683A CN110040710A CN 110040710 A CN110040710 A CN 110040710A CN 201811573683 A CN201811573683 A CN 201811573683A CN 110040710 A CN110040710 A CN 110040710A
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- Prior art keywords
- tree fruit
- chinese parasol
- parasol tree
- poromerics
- hard charcoal
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
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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
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
-
- 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
-
- 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
-
- 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 invention belongs to Material Fields more particularly to a kind of Chinese parasol tree fruit hard charcoal poromerics and preparation method thereof.The preparation method of a kind of Chinese parasol tree fruit hard charcoal poromerics provided by the invention, comprising the following steps: step 1: after the distilled water supersound washing of Chinese parasol tree fruit, vacuum drying;Step 2: Chinese parasol tree fruit powder obtained in step 1 is broken, sieving obtains Chinese parasol tree fruit powder end;Step 3: Chinese parasol tree fruit powder end and inorganic salt solution being mixed, Chinese parasol tree fruit mixed-powder is dried to obtain;Step 4: the Chinese parasol tree fruit mixed-powder being carbonized to obtain Chinese parasol tree fruit hard charcoal poromerics.The present invention provides a kind of Chinese parasol tree fruit hard charcoal poromerics and preparation method thereof, solve in the prior art that structure is complicated for Chinese parasol tree fruit hard charcoal poromerics, the not strong technical problem of repeatability.
Description
Technical field
The invention belongs to Material Fields more particularly to a kind of Chinese parasol tree fruit hard charcoal poromerics and preparation method thereof.
Background technique
Lithium ion battery due to the advantages such as operating voltage with higher and energy density, the good, memory-less effect of safety,
Have become the important energy storage device of current portable electronic device and electric car first choice.But with electric car, intelligence electricity
The real arrival in net epoch, global lithium resource will be unable to the great demand for effectively meeting power lithium-ion battery and capacitor,
To will further raise price with lithium associated materials, increase cost, the final development for hindering New Energy Industry.Therefore, it opens
The related energy storage technology for sending out other cheap alternative lithium ion batteries is very crucial.
Therefore sodium reserves in earth 4-5 order of magnitude higher than lithium replaces lithium that can alleviate lithium resource shortage and asks with sodium
Topic.Since sodium is resourceful, development cost is low, and sodium and lithium are same major elements, has similar insertion mechanism, so that at this
It is possibly realized with similar compound as electrode material in two systems.Hard charcoal is used for lithium, anode material of lithium-ion battery
When discharge platform it is lower, specific capacity is higher, can carry out large current charge and electric discharge, can be used for power battery field.
Biomass carbon rich material resources, it is environmental-friendly, it is at low cost, in lithium ion battery and anode material of lithium-ion battery
In very competitive superiority cause repeatability not strong but due to its structure is complicated multiplicity.
Summary of the invention
The present invention provides a kind of Chinese parasol tree fruit hard charcoal poromerics and preparation method thereof, solve Chinese parasol tree fruit in the prior art
Structure is complicated for hard charcoal poromerics, the not strong technical problem of repeatability.
The present invention provides a kind of preparation methods of Chinese parasol tree fruit hard charcoal poromerics, comprising the following steps:
Step 1: after the distilled water supersound washing of Chinese parasol tree fruit, vacuum drying;
Step 2: Chinese parasol tree fruit powder obtained in step 1 is broken, sieving obtains Chinese parasol tree fruit powder end;
Step 3: Chinese parasol tree fruit powder end and inorganic salt solution being mixed, Chinese parasol tree fruit mixed-powder is dried to obtain;
Step 4: the Chinese parasol tree fruit mixed-powder being carbonized to obtain Chinese parasol tree fruit hard charcoal poromerics.
Preferably, the time of supersound washing described in step 1 is 30-60min.
Preferably, the number of supersound washing described in step 1 is 3-5 times.
Preferably, the Chinese parasol tree fruit powder diameter is 20~75 μm.
Preferably, the mass fraction of the inorganic salts is 0-50%.
Preferably, the temperature of the drying is 80~120 DEG C.
Preferably, the inorganic salts include NaHCO3、Na2CO3、KHCO3、K2CO3With Ca (HCO3)2One of or it is a variety of.
Preferably, the heating rate of the carbonization is 1-5 DEG C/min.
Preferably, the temperature of the carbonization is 700-1500 DEG C.
The present invention also provides a kind of Chinese parasol tree fruit hard charcoal poromerics, by the preparation side of above-mentioned Chinese parasol tree fruit hard charcoal poromerics
Method is made, and partial size is 5-10 μm.
Preparation method provided by the invention, as presoma, is crushed and heated using biomass waste material Chinese parasol tree fruit by physics
Labile inorganic salts different proportion solution blending, the method for high temperature pyrolysis is prepared with certain micropore ratio after point drying
Hard carbon material, solve biomass carbon material as structure it is different caused by the not high deficiency of repeatability.This method has behaviour
Make simple, at low cost, the high advantage of repeatability is easily accomplished scale production, and multiporous biological matter hard charcoal obtained as lithium from
When sub- battery and anode material of lithium-ion battery, there is excellent chemical property.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention without any creative labor, may be used also for those of ordinary skill in the art
To obtain other attached drawings according to these attached drawings.
Fig. 1 is the scanning electron microscope (SEM) photograph of 1-4 of the embodiment of the present invention;
Fig. 2 is the first charge-discharge curve graph of 1-4 of the embodiment of the present invention.
Specific embodiment
The embodiment of the invention provides a kind of preparation methods of hard charcoal poromerics, solve hard charcoal micropore in the prior art
The not strong technical problem of the complicated multiplicity repeatability of material structure.
In order to make the invention's purpose, features and advantages of the invention more obvious and easy to understand, below in conjunction with the present invention
Attached drawing in embodiment, technical scheme in the embodiment of the invention is clearly and completely described, it is clear that disclosed below
Embodiment be only a part of the embodiment of the present invention, and not all embodiment.Based on the embodiments of the present invention, this field
Those of ordinary skill's all other embodiment obtained without making creative work, belongs to protection of the present invention
Range.
Embodiment 1
It weighs 40g Chinese parasol tree fruit to be immersed in distilled water, ultrasonic 1h, wash 3 times.Then dry in 60 DEG C of air dry ovens
Then 12h dries 12h in 120 DEG C of vacuum ovens.It will be crushed in Chinese parasol tree fruit merging pulverizer after drying, be sieved, obtain
Chinese parasol tree fruit powder diameter is less than 75 μm.It takes 10g Chinese parasol tree fruit powder end to be placed in 500mL beaker, weighs bicarbonate according to 0wt% doping
Sodium powder end 0g is added 300mL distilled water and is blended, is heated to 100 DEG C and is evaporated.Continue the dry 12h in 60 DEG C of air dry ovens,
Then the dry 12h in 120 DEG C of vacuum ovens.Take 10g dry mixed-powder be placed in tube furnace, under nitrogen atmosphere with
3 DEG C/min heating rate is warming up to 1300 DEG C, keeps the temperature 3h, and cooled to room temperature obtains carbonized product.Add into carbonized product
Enter the washing of 200mL 1mol/L dilute hydrochloric acid, washs 3 times, neutrality is washed with distilled water to after suction filtration.It is well-dried to be had
The biomass hard carbon material (0wt%) of certain proportion micropore.
Embodiment 2
It takes smashed Chinese parasol tree fruit powder end in 10g example 1 to be placed in 500mL beaker, weighs bicarbonate according to 1wt% doping
Sodium powder end 0.1g is added 300mL distilled water and is blended, is heated to 100 DEG C and is evaporated.Continue the dry 12h in 60 DEG C of air dry ovens,
Then the dry 12h in 120 DEG C of vacuum ovens.The mixed-powder for taking 10g to dry is placed in tube furnace, under nitrogen atmosphere
1300 DEG C are warming up to 3 DEG C/min heating rate, keeps the temperature 3h, cooled to room temperature obtains carbonized product.To carbonized product
Middle addition 200mL 1mol/L dilute hydrochloric acid washing, washs 3 times, neutrality is washed with distilled water to after suction filtration.Well-dried acquisition
Biomass hard carbon material (1wt%) with certain proportion micropore.
Embodiment 3
It takes smashed Chinese parasol tree fruit powder end in 10g example 1 to be placed in 500mL beaker, weighs bicarbonate according to 5wt% doping
Sodium powder end 0.5g is added 300mL distilled water and is blended, is heated to 100 DEG C and is evaporated.Continue the dry 12h in 60 DEG C of air dry ovens,
Then the dry 12h in 120 vacuum ovens.The mixed-powder for taking 10g to dry is placed in tube furnace, with 3 under nitrogen atmosphere
DEG C/min heating rate is warming up to 1300 DEG C, 3h is kept the temperature, cooled to room temperature obtains carbonized product.Add into carbonized product
Enter the washing of 200mL 1mol/L dilute hydrochloric acid, washs 3 times, neutrality is washed with distilled water to after suction filtration.It is well-dried to be had
The biomass hard carbon material (5wt%) of certain proportion micropore.
Embodiment 4
It takes smashed Chinese parasol tree fruit powder end in 10g example 1 to be placed in 500mL beaker, weighs carbonic acid according to 10wt% doping
Hydrogen sodium powder end 1g is added 300mL distilled water and is blended, is heated to 100 DEG C and is evaporated.Continue the dry 12h in 60 DEG C of air dry ovens,
Then the dry 12h in 120 DEG C of vacuum ovens.Take 10g dry mixed-powder be placed in tube furnace, under nitrogen atmosphere with
3 DEG C/min heating rate is warming up to 1300 DEG C, keeps the temperature 3h, and cooled to room temperature obtains carbonized product.Add into carbonized product
Enter the washing of 200mL 1mol/L dilute hydrochloric acid, washs 3 times, neutrality is washed with distilled water to after suction filtration.It is well-dried to be had
The biomass hard carbon material (10wt%) of certain proportion micropore.
Pattern and structural analysis have been carried out to hard carbon material made from embodiment 1-4 using scanning electron microscope (SEM).
Using hard carbon material made from embodiment 1-4 as active material, electrochemistry is carried out after being assembled into sodium-ion battery
It can test, detailed process is as follows:
(1) hard carbon material of preparation, conductive black, styrene-butadiene latex (SBR) and sodium carboxymethylcellulose (CMC) are pressed into matter
Amount is coated on copper foil after mixing, places it in dry in 90 DEG C of convection ovens than being that 85:10:3:2 blendes together slurry
Negative electrode tab is made in 30min, tabletting and punching.
(2) button cell of 2430 models is assembled in the glove box of water content and oxygen content lower than 0.01ppm.Assemble sodium
When ion battery, using hard carbon material made from embodiment 1-4 as working electrode, metallic sodium is to electrode, and diaphragm is GF/F model
Fibreglass diaphragm, electrolyte be 1mol/L NaClO4EC:DEC (volume ratio 1:1) mixed solution.It will be assembled
Battery standing carries out charge-discharge test on blue electric battery test system after for 24 hours, and first charge-discharge curve is as shown in Figure 2.
The embodiment of the present invention 1 prepare biomass hard charcoal have it is laminar structured, particle size be 5-10 μm.
Know the hard charcoal with certain micropore ratio of inventive embodiments 1-4 preparation as sodium-ion battery cathode material by Fig. 2
When material, under 25mA/g current density, the charging and discharging curve of difference doping ratio is essentially identical, and platform section capacity is maintained at 300-
350mAh/g, with the increase of doping ratio, slope section capacity is varied widely, and when 5% sodium bicarbonate adulterates, is shown opposite
Optimal chemical property: charge specific capacity 381.0mAh/g, coulombic efficiency is 72.27% for the first time, higher than common biology
Matter hard charcoal.
The above, the above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations;Although referring to before
Stating embodiment, invention is explained in detail, those skilled in the art should understand that: it still can be to preceding
Technical solution documented by each embodiment is stated to modify or equivalent replacement of some of the technical features;And these
It modifies or replaces, the spirit and scope for technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution.
Claims (10)
1. a kind of preparation method of Chinese parasol tree fruit hard charcoal poromerics, which comprises the following steps:
Step 1: after the distilled water supersound washing of Chinese parasol tree fruit, vacuum drying;
Step 2: Chinese parasol tree fruit powder obtained in step 1 is broken, sieving obtains Chinese parasol tree fruit powder end;
Step 3: Chinese parasol tree fruit powder end and inorganic salt solution being mixed, Chinese parasol tree fruit mixed-powder is dried to obtain;
Step 4: the Chinese parasol tree fruit mixed-powder being carbonized to obtain Chinese parasol tree fruit hard charcoal poromerics.
2. the preparation method of Chinese parasol tree fruit hard charcoal poromerics according to claim 1, which is characterized in that described in step 1
The time of supersound washing is 30-60min.
3. the preparation method of Chinese parasol tree fruit hard charcoal poromerics according to claim 1, which is characterized in that described in step 1
The number of supersound washing is 3-5 times.
4. the preparation method of Chinese parasol tree fruit hard charcoal poromerics according to claim 1, which is characterized in that the Chinese parasol tree fruit powder
Last partial size is 20~75 μm.
5. the preparation method of Chinese parasol tree fruit hard charcoal poromerics according to claim 1, which is characterized in that the inorganic salts
Mass fraction is 0-50%.
6. the preparation method of Chinese parasol tree fruit hard charcoal poromerics according to claim 1, which is characterized in that the temperature of the drying
Degree is 80~120 DEG C.
7. the preparation method of Chinese parasol tree fruit hard charcoal poromerics according to claim 1, which is characterized in that the inorganic salts packet
Include NaHCO3、Na2CO3、KHCO3、K2CO3With Ca (HCO3)2One of or it is a variety of.
8. the preparation method of Chinese parasol tree fruit hard charcoal poromerics according to claim 1, which is characterized in that the liter of the carbonization
Warm rate is 1-5 DEG C/min.
9. the preparation method of Chinese parasol tree fruit hard charcoal poromerics according to claim 1, which is characterized in that the temperature of the carbonization
Degree is 700-1500 DEG C.
10. a kind of Chinese parasol tree fruit hard charcoal poromerics, by Chinese parasol tree fruit hard charcoal poromerics described in any one of claim 1 to 9
Preparation method, which is characterized in that its partial size be 5-10 μm.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN113948681A (en) * | 2021-09-29 | 2022-01-18 | 西安交通大学 | Biomass-based hard carbon compound composite material and preparation method and application thereof |
CN115007106A (en) * | 2022-04-24 | 2022-09-06 | 武汉理工大学 | Phoenix tree fruit hair modified coke demercuration adsorbent and preparation method thereof |
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CN106450317A (en) * | 2016-11-29 | 2017-02-22 | 陕西科技大学 | Flaky sodium battery negative electrode carbon electrode material and preparation method thereof |
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2018
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Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN106450317A (en) * | 2016-11-29 | 2017-02-22 | 陕西科技大学 | Flaky sodium battery negative electrode carbon electrode material and preparation method thereof |
Non-Patent Citations (1)
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN113948681A (en) * | 2021-09-29 | 2022-01-18 | 西安交通大学 | Biomass-based hard carbon compound composite material and preparation method and application thereof |
CN115007106A (en) * | 2022-04-24 | 2022-09-06 | 武汉理工大学 | Phoenix tree fruit hair modified coke demercuration adsorbent and preparation method thereof |
CN115007106B (en) * | 2022-04-24 | 2023-08-08 | 武汉理工大学 | Firmiana tree fruit hair modified burnt demercuration adsorbent and preparation method thereof |
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Application publication date: 20190723 |