CN107204430A - A kind of method that utilization wheat stalk prepares sodium ion battery electrode material - Google Patents
A kind of method that utilization wheat stalk prepares sodium ion battery electrode material Download PDFInfo
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- CN107204430A CN107204430A CN201710544760.2A CN201710544760A CN107204430A CN 107204430 A CN107204430 A CN 107204430A CN 201710544760 A CN201710544760 A CN 201710544760A CN 107204430 A CN107204430 A CN 107204430A
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- ion battery
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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
- H01M4/04—Processes of manufacture in general
- H01M4/0471—Processes of manufacture in general involving thermal treatment, e.g. firing, sintering, backing particulate active material, thermal decomposition, pyrolysis
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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
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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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
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Abstract
The invention discloses a kind of method that utilization wheat stalk prepares sodium ion battery electrode material, specifically comprise the following steps：The discarded wheat stalk of collection is cleaned with water and ethanol respectively, it is repeated 4 times, each scavenging period is 30min, the subsequent forced air drying 12h at 80 DEG C, obtain totally dry wheat stalk, blend to be put into chitosan Zn silicon powder modified solutions and soak 48 hours, then forced air drying 12h at 80 DEG C, obtain modified wheat stalk, modified wheat stalk is calcined in carbon monoxide and nitrogen mixed gas, product is collected after natural cooling, after resulting materials are refined through high-energy ball milling, energy ball milling refinement, obtained solid powder is stand-by sodium ion battery electrode material.
Description
Technical field
The present invention relates to a kind of method that utilization wheat stalk prepares sodium ion battery electrode material.
Background technology
On the one hand traditional fossil energy causes the continuous decline of gross reserves, the opposing party with being continuously increased for its yield
The Environment pollution problem that face is caused in use is also increasingly serious, it is therefore necessary to develop new cleaning fuel to meet the mankind
The demand of development.From nineteen ninety, lithium ion battery is able to popularization, the energy storage device is just because it has high capacity density, power close
Spend, can be recycled and obtained widespread adoption many advantages, such as environmentally friendly.Current lithium resource distribution uneven and
High price turns into the bottleneck that limiting lithium ion cell further develops, and is considered as best with sodium of the lithium in same main group
Alternate resources.Sodium is similar with the chemical property of lithium, and the rich reserves of sodium, it can thus be appreciated that exploitation and design high-performance sodium ion
Battery turns into the most important thing of future studies.
Carbon material is due to itself having higher electric conductivity in numerous electrode materials, and pattern and structure are adjustable, and surely
The qualitative advantage such as extremely strong turns into one of popular electrode material.Carbon material is prepared by raw material of bio-waste and is applied
Research in secondary cell system, has just been risen in recent years and most of work are concentrated on lithium ion battery.By biological waste
Carbon material prepared by thing is generally hard carbon, and carbon material prepared by conventional method is assembled into after sodium-ion battery usual high rate performance and followed
Ring performance is preferable not to the utmost.The most effectual way of carbon material storage sodium performance is improved for the defect of increase material and porous material two is prepared
Kind：The defect of material surface can help to store sodium ion and increase the fake capacitance behavior on surface to improve overall capacity, and
Loose structure can then promote the abundant contact of active material and electrolyte to ensure that material has preferable high rate performance.
Wheat is a kind of important cereal crops, all a large amount of plantations in worldwide.But produced by plantation wheat
The process problem of wheat stalk annoying people always.The conventional method of current people's processing wheat stalk is burning and burial
Two ways, these modes not only cause the waste of resource while also being damaged to a certain extent to environment.Find suitable
Method wheat stalk is changed into can provide the sodium ion battery electrode material of energy for we and meanwhile solve energy crisis and
Environmental pollution provides good direction.
The content of the invention
Wheat stalk is utilized to prepare sodium ion electricity using one kind in view of the above-mentioned problems of the prior art, the present invention is provided
The method of pond electrode material, realize discarded wheat stalk is changed into high-performance sodium ion battery electrode material, it is necessary to it is main
Step is as follows：
Step one：The discarded wheat stalk of collection is cleaned with water and ethanol respectively, is repeated 4 times, when cleaning every time
Between be 30min, then the forced air drying 12h at 80 DEG C, obtain totally dry wheat stalk, blend and be put into chitosan-Zn- silicon
Soaked in micronization modified solution 48 hours, then forced air drying 12h at 80 DEG C, obtains modified wheat stalk,
Step 2：Modified wheat stalk is calcined 1 hour in carbon monoxide and nitrogen mixed gas, 900 DEG C of temperature is naturally cold
But product is collected afterwards.
Step 3：After resulting materials are refined through high-energy ball milling, 200 mesh sieve are crossed, it is stand-by.
Step 4：Step 3 product is transferred in high energy ball mill, high-energy ball milling refinement, product crosses 100-200 mesh sieves
Son, obtained solid powder is stand-by sodium ion battery electrode material.
The method that a kind of 2 utilization wheat stalks according to claim 1 prepare sodium ion battery electrode material, it is special
Levy and be, product should be subjected to micronization processes before step one cleaning, the matter of distilled water/ethanol solution and wheat stalk during cleaning
Amount is than being 50:1, the time is 10-30min, cleaning process 3-5 times repeatedly.
The method that a kind of 3 utilization wheat stalks according to claim 1 prepare sodium ion battery electrode material, it is special
Levy and be, chitosan-Zn- silicon powder material preparation methods are as follows：Silicon powder is dispersed in water, 5h is stirred at room temperature, is stood
Supernatant is taken after 8h；
Step 2, chitosan is dissolved in 60 DEG C of heating water baths processing 1h in 3 parts of (v/w) acetums;
Step 3, by the above-mentioned chitosan-acetic acid solution handled well with per minute 30 drop speed be added dropwise to silicon powder supernatant
In liquid, continue stirring reaction 5h under 60 DEG C of water-baths;
Step 4, it is then centrifuged for and is washed with pure water, finally shake and be dispersed in again in 200ml ultra-pure waters under vacuum tank, obtains shell and gather
Sugar-silicon powder；
Step 5, zinc powder is subjected to hot alkali treatment：Manganese powder is handled into 1h first under hot-air to go out to sweep impurity, is then being transferred to
1h is soaked in 10 parts of NaOH solution;
Step 6 and then the zinc powder that hot alkali treatment is crossed is added in solution stirs 1h at room temperature;
Step 7, above-mentioned solution is transferred in ptfe autoclave, titanate coupling agent is then added dropwise, in nitrogen atmosphere,
260 DEG C, 2h is reacted under 0.5kpa;
Step 8, the zinc solution handled well is added to above-mentioned solution, obtains chitosan-Zn- silicon powder modified solutions,
The method that a kind of 4 utilization wheat stalks according to claim 1 prepare sodium ion battery electrode material, its feature exists
In, material is refined using high-energy ball milling in step 5, controlled during ball milling abrading-ball and product mass ratio be 50:1, rotating speed
For 350 rpms, Ball-milling Time is 1h, and evenly, subsequent sieving processing makes last production to product grain after high-energy ball milling
Thing is more conducive to assembled battery.
The method that a kind of 5 utilization wheat stalks according to claim 1 prepare sodium ion battery electrode material, its
It is characterised by, in described step two, nitrogen is 2-5 with carbon dioxide volume ratio:1.
The present invention includes following beneficial effect：Discarded wheat stalk is changed into sodium ion battery electrode material by the present invention
Preparation method is simple, low raw-material cost, favorable repeatability, can also obtain storing the high-performance of energy while environmental protection
Sodium-ion battery.This method is greatly improved by the way that stalk is immersed in into modification in chitosan-Zn- silicon powder material solutions
The activity of stalk after calcining so that the carbon material prepared maintains its porous characteristic while having more defect,
This characteristic is conducive to improving the storage sodium capacity of assembled sodium-ion battery, strengthens the cyclical stability of battery and forthright again
Energy.The battery that the sodium ion battery electrode material that discarded wheat stalk changes is assembled into by this method is in 1000mA/g electric currents
Remain to keep 200mAh/g capacitance through 1000 weeks under density after circulating.
Brief description of the drawings
Fig. 1 is the TEM figures of the electrode material of wheat stalk preparation in embodiment 1.
Embodiment
Embodiment 1：
Step one：The discarded wheat stalk of collection is cleaned with water and ethanol respectively, is repeated 4 times, when cleaning every time
Between be 30min, then the forced air drying 12h at 80 DEG C, obtain totally dry wheat stalk, blend and be put into chitosan-Zn- silicon
Soaked in micronization modified solution 48 hours, then forced air drying 12h at 80 DEG C, obtains modified wheat stalk,
Step 2：Modified wheat stalk is calcined 1 hour in carbon monoxide and nitrogen mixed gas, nitrogen and carbon dioxide body
Product is than being 3:1,900 DEG C of temperature collects product after natural cooling.
Step 3：After resulting materials are refined through high-energy ball milling, 200 mesh sieve are crossed, it is stand-by,
Step 4：Step 3 product is transferred in high energy ball mill, high-energy ball milling refinement, product is crossed 100-200 mesh sieve, obtained
The solid powder arrived is stand-by sodium ion battery electrode material.
Above-mentioned chitosan-Zn- silicon powder material preparation methods are as follows：
Silicon powder is dispersed in water, 5h is stirred at room temperature, supernatant is taken after standing 8h；
Step 2, chitosan is dissolved in 60 DEG C of heating water baths processing 1h in 2 parts of (v/w) acetums;
Step 3, by the above-mentioned chitosan-acetic acid solution handled well with per minute 30 drop speed be added dropwise to silicon powder supernatant
In liquid, continue stirring reaction 5h under 60 DEG C of water-baths;
Step 4, it is then centrifuged for and is washed with pure water, finally shake and be dispersed in again in 200ml ultra-pure waters under vacuum tank, obtains shell and gather
Sugar-silicon powder；
Step 5, zinc powder is subjected to hot alkali treatment：Manganese powder is handled into 1h first under hot-air to go out to sweep impurity, is then being transferred to
1h is soaked in 10 parts of NaOH solution;
Step 6 and then the zinc powder that hot alkali treatment is crossed is added in solution stirs 1h at room temperature;
Step 7, above-mentioned solution is transferred in ptfe autoclave, titanate coupling agent is then added dropwise, in nitrogen atmosphere,
260 DEG C, 2h is reacted under 0.5kpa;
Step 8, the zinc solution handled well is added to above-mentioned solution, obtains chitosan-Zn- silicon powder modified solutions.
Sodium ion battery electrode material is assembled, wherein electrolyte uses ethylene carbonate：Diethyl carbonate（Volume ratio is 1:1）
+ 5% fluorinated ethylene carbonate.
The sodium-ion battery of assembling, test result is：Capacity is maintained at 451mAh/g under 100mA/g current density, and
Under 1000mA/g current density 325mAh/g is still maintained at after 1000 weeks circulate.Prepared by this method indicated above
Battery electrode material has excellent storage sodium performance.TEM figures confirm that the particle size of the material is further refined and distribution is equal
It is even.The pore size distribution of material is more homogeneous.Mesoporous is uniformly distributed the abundant contact for being conducive to electrolyte and electrode material, and tiny
Particle size can strengthen the high rate performance of battery.
Comparative example 1：
Preparation technology is same as Example 1, and difference is, in step one, and wheat stalk changes without chitosan-Zn- silicon powders
The modification of property solution.
The sodium-ion battery of assembling, test result is：Capacity is in 251mAh/g under 100mA/g current density, and
Under 1000mA/g current density 205mAh/g is maintained at after 1000 weeks circulate.
Comparative example 2：
Preparation technology is same as Example 1, and difference is, in step one, and wheat stalk is in chitosan-silicon powder modified solution
Silicon powder is dispersed in water by immersion, its chitosan-silicon powder modified solution preparation method, and 5h is stirred at room temperature, is stood after 8h
Take supernatant；
Step 2, chitosan is dissolved in 60 DEG C of heating water baths processing 1h in 2 parts of (v/w) acetums;
Step 3, by the above-mentioned chitosan-acetic acid solution handled well with per minute 30 drop speed be added dropwise to silicon powder supernatant
In liquid, continue stirring reaction 5h under 60 DEG C of water-baths;
Step 4, it is then centrifuged for and is washed with pure water, finally shake and be dispersed in again in 200ml ultra-pure waters under vacuum tank, obtains shell and gather
Sugar-silicon powder,
The sodium-ion battery of assembling, test result is：Capacity is in 275mAh/g under 100mA/g current density, and in 1000mA/
Under g current density 221mAh/g is maintained at after 1000 weeks circulate.
Comparative example 3：
Preparation technology is same as Example 1, and difference is, in step 2, and nitrogen is 1 with carbon dioxide volume ratio:1.
The sodium-ion battery of assembling, test result is：Capacity is in 247mAh/g under 100mA/g current density, and
Under 1000mA/g current density 212mAh/g is maintained at after 1000 weeks circulate.
Comparative example 4：
Preparation technology is same as Example 1, and difference is, in step 2, and nitrogen is 1 with carbon dioxide volume ratio:3.
The sodium-ion battery of assembling, test result is：Capacity is in 217mAh/g under 100mA/g current density, and
Under 1000mA/g current density 192mAh/g is maintained at after 1000 weeks circulate.
Comparative example 5：
Preparation technology is same as Example 1, and difference is, in step one, chitosan-Zn- silicon powder modified solution preparation methods
Difference, its preparation method is as follows：Silicon powder is dispersed in water, 5h is stirred at room temperature, supernatant is taken after standing 8h；
Step 2, chitosan is dissolved in 60 DEG C of heating water baths processing 1h in 2 parts of (v/w) acetums;
Step 3, by the above-mentioned chitosan-acetic acid solution handled well with per minute 30 drop speed be added dropwise to silicon powder supernatant
In liquid, continue stirring reaction 5h under 60 DEG C of water-baths;
Step 4, it is then centrifuged for and is washed with pure water, finally shake and be dispersed in again in 200ml ultra-pure waters under vacuum tank, obtains shell and gather
Sugar-silicon powder；
Step 5, above-mentioned solution is transferred in ptfe autoclave, titanate coupling agent is then added dropwise, in nitrogen atmosphere,
260 DEG C, 2h is reacted under 0.5kpa;
Step 6, common zinc solution is added to above-mentioned solution, obtains chitosan-Zn- silicon powder modified solutions.
Sodium ion battery electrode material is assembled, wherein electrolyte uses ethylene carbonate：Diethyl carbonate（Volume ratio is 1:1）
+ 5% fluorinated ethylene carbonate.
The sodium-ion battery of assembling, test result is：Capacity is maintained at 241mAh/g under 100mA/g current density, and
Under 1000mA/g current density 227mAh/g is still maintained at after 1000 weeks circulate.
Embodiment and comparative example show that chitosan-Zn- silicon powders modification is for preparing the sodium ion electricity using wheat as raw material
Pole material has critically important influence.
Claims (5)
1. a kind of method that utilization wheat stalk prepares sodium ion battery electrode material, it is characterised in that
Comprise the following steps：
Step one：The discarded wheat stalk of collection is cleaned with water and ethanol respectively, is repeated 4 times, when cleaning every time
Between be 30min, then the forced air drying 12h at 80 DEG C, obtain totally dry wheat stalk, blend and be put into chitosan-Zn- silicon
Soaked in micronization modified solution 48 hours, then forced air drying 12h at 80 DEG C, obtains modified wheat stalk,
Step 2：Modified wheat stalk is calcined 1 hour in carbon monoxide and nitrogen mixed gas, 900 DEG C of temperature is naturally cold
But product is collected afterwards,
Step 3：After resulting materials are refined through high-energy ball milling, 200 mesh sieve are crossed, it is stand-by,
Step 4：Step 3 product is transferred in high energy ball mill, high-energy ball milling refinement, product is crossed 100-200 mesh sieve, obtained
The solid powder arrived is stand-by sodium ion battery electrode material.
2. the method that a kind of utilization wheat stalk according to claim 1 prepares sodium ion battery electrode material, its feature
It is, product should be subjected to micronization processes before step one cleaning, the quality of distilled water/ethanol solution and wheat stalk during cleaning
Than for 50:1, the time is 10-30min, cleaning process 3-5 times repeatedly.
3. the method that a kind of utilization wheat stalk according to claim 1 prepares sodium ion battery electrode material, its feature
It is, chitosan-Zn- silicon powder material preparation methods are as follows：Silicon powder is dispersed in water, 5h is stirred at room temperature, 8h is stood
After take supernatant；
Step 2, chitosan is dissolved in 60 DEG C of heating water baths processing 1h in 3 parts of (v/w) acetums;
Step 3, by the above-mentioned chitosan-acetic acid solution handled well with per minute 30 drop speed be added dropwise to silicon powder supernatant
In liquid, continue stirring reaction 5h under 60 DEG C of water-baths;
Step 4, it is then centrifuged for and is washed with pure water, finally shake and be dispersed in again in 200ml ultra-pure waters under vacuum tank, obtains shell and gather
Sugar-silicon powder；
Step 5, zinc powder is subjected to hot alkali treatment：Manganese powder is handled into 1h first under hot-air to go out to sweep impurity, is then being transferred to
1h is soaked in 10 parts of NaOH solution;
Step 6 and then the zinc powder that hot alkali treatment is crossed is added in solution stirs 1h at room temperature;
Step 7, above-mentioned solution is transferred in ptfe autoclave, titanate coupling agent is then added dropwise, in nitrogen atmosphere,
260 DEG C, 2h is reacted under 0.5kpa;
Step 8, the zinc solution handled well is added to above-mentioned solution, obtains chitosan-Zn- silicon powder modified solutions.
4. the method that a kind of utilization wheat stalk according to claim 1 prepares sodium ion battery electrode material, its feature
It is, is refined material using high-energy ball milling in step 4, the mass ratio that abrading-ball and product are controlled during ball milling is 50:1, turn
Speed is 350 rpms, and Ball-milling Time is 1h, and evenly, subsequent sieving processing makes last product grain after high-energy ball milling
Product is more conducive to assembled battery.
5. the method that a kind of utilization wheat stalk according to claim 1 prepares sodium ion battery electrode material, its feature
It is, in described step two, nitrogen is 2-5 with carbon dioxide volume ratio:1.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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