CN110429264A - A method of preparing rice husk base negative electrode material - Google Patents
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- CN110429264A CN110429264A CN201910743855.6A CN201910743855A CN110429264A CN 110429264 A CN110429264 A CN 110429264A CN 201910743855 A CN201910743855 A CN 201910743855A CN 110429264 A CN110429264 A CN 110429264A
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- 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
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- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
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- H01M4/625—Carbon or graphite
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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Abstract
A method of rice husk base negative electrode material is prepared, biomass energy chemical field, specific steps are belonged to are as follows: (1) rice husk is crushed, prepares xylose solution and hydrolysis residue in 100 DEG C of -120 DEG C of dilute acid hydrolysis 0.5h-1h；(2) hydrolysis residue prepares primary negative electrode material through zinc chloride dipping, activation；(3) the porous negative electrode material of C/SiO2 is prepared through electrode pitch modification.Compared with prior art, method advantage of the invention is as follows: (1) using agricultural and sideline product rice husk as raw material, it is pre-processed using dilute acid hydrolysis, regulate and control the ratio of carbon and silicon, it solves ectonexine silica and charcoal in pyrolytic carbon to be unevenly distributed, internal layer bulk charcoal exists, and causes the asynchronous problem for reducing specific capacity of embedding and removing because of microstructure difference；(2) bitumen treatment primary negative electrode material is utilized, electric conductivity is improved；Carbon structure is strengthened, productive technique is improved；Surface functional group is covered, leakage current is avoided, improves cyclical stability.
Description
Technical field
The invention belongs to biomass energy chemical fields, specifically disclose a kind of method for preparing rice husk base negative electrode material.
Background technique
Currently, environmental crisis and energy consumption increasingly increase due to petroleum fuel shortage, researcher is promoted to find more
Cleaning and better electrochemical energy converting system.In such systems, as a kind of novel energy, lithium ion battery
(LIBs) since its high energy density, good cycle performance and long-term cycle life have caused comprehensive concern.
Therefore, LIBs can satisfy the development of electric car and plug-in hybrid electric vehicle.
From the point of view of negative electrode material angle, as LIBs cathode, the theoretical specific capacity of Current commercial graphite is low, is
372mAh.g-1, this has become the limitation of its broader applications.
In the past few years, silicon Si has had received widespread attention, because of its rich reserves, lower on earth
Operating potential and known highest theoretical specific capacity (4200mAh.g-1).But during embedding de- lithium, the volume of silicon Si
Expansion is very serious (>=300%), and it is cracked that this will lead to electrode interior, loses and is in electrical contact and then increases impedance, will lead to appearance
Rapid decay is measured, this significantly limits the business application of LIBs.
Recently nano silica (SiO2) is used as negative electrode material, because of its theoretical specific volume with higher
Amount: 1961mAh.g-1 and with lower discharge voltage similar in silicon Si.But lithium ion (Li during initial lithiation+)
Inert Li2O and Li4SiO4 can be generated by being embedded into SiO2, can be used as buffer composition, be alleviated to a certain extent
Volumetric expansion.Therefore, compared with Si negative electrode material, SiO2 negative electrode material shows preferable cyclical stability.
But the most important defect for limiting SiO2 business application is its poorly conductive.Therefore, researcher is preparing charcoal
A lot of research work is carried out in terms of silicon dioxide composite material.CN105633406A disclose it is a kind of prepare silica/
The method of porous carbon lithium ion battery negative material, by sodium metasilicate, glucose and sodium chloride according to quality proportioning be dissolved in from
In sub- water；Configured solution is dry, be ground to fine-powder, calcine, obtain sodium metasilicate/carbon matrix precursor, by sodium metasilicate/
Carbon matrix precursor is placed in concentrated hydrochloric acid, is dried in 170 DEG C of baking ovens later, and it is multiple that silica/porous carbon is obtained after washing
Condensation material.CN105977470A discloses a kind of silicon dioxide activity carbon composite, preparation method and lead carbon battery and answers
With.Preparation method includes step are as follows: 1) impregnates rice husk inorganic strong acid solution, purification；2) that purified rice husk is dry,
Carbonization and primary activation processing, wherein three sections of heating cycle point, obtains carbonization rice husk；3) carbonization rice husk is put into inorganic strong alkali
In solution, it is then slowly added into dilute inorganic strong acid solution, obtains presoma after stirring, filtration washing；4) by presoma it is dry and
It activates again, obtains silicon dioxide activity carbon composite.It is compound more that CN105280879A discloses a kind of silicon/carbon dioxide
Pore electrod and preparation method thereof.Silica and dispersant are prepared into uniform silicon dioxide gel；Then by dioxy
SiClx colloidal sol is uniformly mixed with graphite additive is made mixed slurry；Mixed slurry is dried and crushed into powder again, and by powder
Shaping blank is made.CN107634190A discloses the nanocomposite of a kind of silica and carbon, which is by carbon packet
Cover the compound composition of nano SiO 2 particle, the method that above-mentioned silica and carbon composite are prepared by high-temperature heat treatment.
CN103035917A discloses a kind of preparation method of lithium ion battery silicon dioxide/carbon composite negative electrode material,
Using ethyl orthosilicate as silicon source, there is xerogel or aerogel structure using sol-gel method and the preparation of constant pressure and dry technique
Porous silica carries out ball-milling treatment to porous silica, and by carbon coating and heat treatment, prepares nano-silica
SiClx/carbon compound cathode materials.CN103730662A discloses a kind of negative electrode of lithium ion battery silicon/carbon dioxide composite material
And preparation method thereof.By silicon-containing compound under the conditions of the solution neutral and alkali containing organic formwork agent catalyzing hydrolysis, be prepared
Porous silica containing organic formwork agent；The porous silica containing organic formwork agent is filtered later, is washed
It washs；Crude product is placed in heat treatment under inert atmosphere and obtains silicon/carbon dioxide composite material.CN105742600A discloses one
The preparation method of kind lithium ion battery silicon/carbon dioxide nano composite aerogel, by carrying out carbon packet to aerosil
The problem of covering, being able to suppress the bulk effect and particle agglomeration of silica in cyclic process.CN104953097A discloses one
Kind silica carbon composite nano-fiber lithium ion battery negative material and preparation method.Firstly, weighing organic block polymer
Surfactant is dissolved in liquid solvent and forms the first solution as forming agent；Weighing silicon source again, to be separately dissolved in the liquid molten
Agent forms the second solution；The first solution is added in second solution, constant temperature stirs evenly, and forms third solution, then third is molten
Liquid evaporation at constant temperature is at gel；Finally, gel is heat-treated.A kind of negative electrode of lithium ion battery of CN105895880A is used
Silicon dioxide composite material preparation method, including [carbon nanotube/silica] composite material preparation, silica forerunner
Body preparation and silicon dioxide composite material prepare three big processes.CN104300124A discloses a kind of silicon/carbon dioxide compound
Preparation method and its application in lithium/sodium-ion battery, firstly, by biomass ash pulverize into be less than Centimeter Level other
Grain；Then at a temperature of 800 DEG C~1500 DEG C, under argon gas, nitrogen, carbon monoxide, hydrogen or steam atmosphere be heat-treated 4~
20h；Obtained product is cleaned in water or in diluted acid finally, is separated, it is dry, obtain silicon/carbon dioxide compound.
CN103474636A discloses a kind of silicon substrate lithium ion battery negative material and preparation method thereof, at room temperature, by surface-active
Agent is added in deionized water and stirs；It is stirred after silicon powder suspension is added again；Above-mentioned mixed solution is heated to 40~50 DEG C,
3- aminopropyl triethoxysilane, ethyl orthosilicate are respectively dropped into, stirred；70~90 DEG C are then heated to, heat preservation 15~48
Hour；Centrifugation collecting reaction product, then washed respectively with ethyl alcohol and deionized water, it is dry；Acetonitrile is added in products therefrom
Hydrochloric acid mixed solution stirs 4~8 hours, after cleaned again with deionized water, it is dry, material can be obtained.
CN105098183A discloses a kind of preparation method of lithium ion battery micropore carbon negative pole material, by charred rice husk,
Pickling, activation removal silica prepare porous carbon cathode material.CN103647043A discloses a kind of lithium ion secondary battery
The preparation method of negative electrode material carbonizes, 700 under the atmosphere of hydrogen or/and argon gas using rice husk as raw material through 200~700 DEG C
~1000 DEG C of high-temperature process prepare electrode material.It is negative that CN106848249A discloses SiO2@C nucleocapsid complex lithium ion battery
Charred rice husk, pickling, ball milling are prepared negative electrode material by the preparation method of pole material.
Above-mentioned each scheme stresses to have studied the preparation method of charcoal and silicon dioxide composite material, and preparation process is complicated, dioxy
The distribution of SiClx and charcoal is controlled by reaction condition.Therefore up to the present, there is a problem in that:
(1) although smaller than the coefficient of expansion of silicon, there is still a need for certain swollen during lithium ion insertion silica
Swollen space.
(2) with graphite-phase ratio, there is the shortcomings that poorly conductive, constrain charcoal and silica is multiple in charcoal and silica
Condensation material is as negative electrode material application.
Therefore a kind of new technical solution is needed to solve these problems in the prior art.
Summary of the invention
The object of the present invention is to provide a kind of methods for preparing rice husk base negative electrode material, are original with agricultural and sideline product rice husk
Material, is pre-processed using dilute acid hydrolysis, regulates and controls the ratio of carbon and silicon, solves ectonexine silica and charcoal distribution in pyrolytic carbon
Unevenly, cause the asynchronous problem for reducing specific capacity of embedding and removing because of microstructure difference；Then zinc chloride is utilized
As activator, porous ion channel is prepared, volume expansion provides cushion space in charge and discharge process for silica；Together
When to solve most important defect problem of the limitation silica as negative electrode material business application: poorly conductive, the present invention adopt
With electrode pitch modification porous C/SiO2 negative electrode material.
To achieve the above object, the invention proposes a kind of methods for preparing rice husk base negative electrode material, which is characterized in that
Include the following steps:
Step 1: raw rice husk being sieved and is cleaned, and being crushed to partial size is 10mm-20mm, obtains powdered rice hulls, spare；
Step 2: the rice husk after smashing is added in reaction kettle, and concentration is added in the ratio of butt 1Kg:(5-10) L
For the sulfuric acid solution of 1wt%-10wt%, be warming up to 100 DEG C -120 DEG C, catalyzing hydrolysis 0.5h-2h, prepare xylose aqueous solution and
Hydrolysis residue；Xylose solution send furfural Workshop Production furfural；
Step 3: pressing dry weight ratio 1:2, the obtained hydrolysis residue of step 2 uniformly mixed with zinc chloride, and casket is added
In alms bowl, it is placed in tube furnace, is warming up to 500 DEG C -600 DEG C, 1h-2h is activated, discharges after being cooled to room temperature, with the salt of 0.5M concentration
Acid solution impregnates 2h-6h, and filtering is washed to no chloride ion, primary negative electrode material is prepared in 110 DEG C of dryings；
Step 4: the primary negative electrode material in step 3 is uniformly mixed to dispersion 0.5h-1h with electrode pitch, is prepared
Pitch/primary negative electrode material mixed-powder；
Step 5: the mixed-powder of step 4 is transferred in tube furnace, under nitrogen protection, is warming up to 150 DEG C -250
DEG C constant temperature is heat-treated 1h-2h, then is warming up to 600 DEG C of -1000 DEG C of constant temperature heat treatment 1h-2h, and cooling breaks up, prepares C/SiO2
Porous negative electrode material.
Preferably, the pitch in the step 4/primary negative electrode material mixed-powder preparation method is: electrode is dripped
Green powder is added in solvent, is dispersed with stirring 0.5h-2h, obtains pitch suspension or solution；Primary negative electrode material is added to drip
In green suspension or solution, it is dispersed with stirring 0.5h-1h, heating recovery solvent, solid is placed in drying box, 85 DEG C of dry 5h-
12h prepares pitch/primary negative electrode material mixed-powder.
The solvent is cyclohexanol, dehydrated alcohol, acetone, tetrahydrofuran, hexamethylene, a kind of in n-hexane or two kinds
Mixture.
Preferably, pitch/primary negative electrode material mixed-powder preparation method that goes out in the step 4 is: by electrode
Asphalt powder and primary negative electrode material uniformly mix, and the partial size through airslide disintegrating mill grinding dispersion to primary negative electrode material is 10 μ
M-15 μm, prepare pitch/primary negative electrode material mixed-powder.
Electrode pitch and the mass ratio of primary negative electrode material are (10-30) in the step 4: 100.
The solid-to-liquid ratio of the pitch and solvent is (1-15) Kg:100L.
Through the above design, the present invention can be brought the following benefits:
1, after rice husk is carbonized under proper condition, silica is uniformly coated by unformed charcoal, without the carbon of any complexity
Coating technology.Therefore, using rice husk as raw material, preparation porous C/SiO2 composite material is shown as the negative electrode material of LIBs
Huge development potentiality.
2, using regulation hydrolysis temperature and time, the ratio of silica and carbon in presoma is adjusted, controls negative electrode material
The ratio and distribution of middle C/SiO2 improves coulombic efficiency.
3, the present invention carries out carbonization-activation to hydrolysis rice husk as activator using zinc chloride ZnCl2, controls activation temperature
And activation time, change aperture and the hole Rong great little of negative electrode material, to obtain the porous C/SiO2 cathode with high-specific surface area
Material, main purpose is to increase electrolyte and C/SiO2 negative electrode material contact area, to promote Li+It is fast on its interface
Speed diffusion.
4, the porous C obtained /SiO2 negative electrode material, specific discharge capacity can be greater than under the current density of 0.1A.g-1
1100mAh/g, higher than the porous C prepared using chemical reagent as raw material /SiO2 negative electrode material (in 0.1A/g for 635.7mAh/
g).This method is simple, energy-efficient, and strong operability, cost of material is low, being capable of large-scale industrial production.
5, silica silicium cathode material can generate biggish volume change in charge and discharge process, and electrode is caused to crack
Dusting, especially using rice husk pyrolytic carbon as negative electrode material, the wherein short texture of charcoal, productive technique is poor, and it is steady to reduce circulation
It is qualitative.The present invention takes electrode pitch uniformly penetrating to particle surface, and charcoal internal combustion is after heat treatment greatly improved
Power improves productive technique.
It 6, is the difficulty of its poorly conductive to solve limitation SiO2 as the most important defect of negative electrode material business application
Topic, the present invention use electrode pitch modification C/SiO2, improve cyclical stability, prevent side reaction, solve leakage current
Problem.
7, hydrolyzate prepares furfural, has not only handled hydrolyzed waste water, but also produces high added value furfural product, reduces simultaneously
The cost of negative electrode material.
Specific embodiment
In order to illustrate more clearly of the present invention, below with reference to preferred embodiment, the present invention is described further.Ability
Field technique personnel should understand that.Specifically described content is illustrative and be not restrictive below, this should not be limited with this
The protection scope of invention.
Embodiment 1
Step 1: raw rice husk being sieved and is cleaned, and being crushed to partial size is 10mm-20mm, spare；
Step 2: the rice husk after smashing is added in reaction kettle, and concentration is added in the ratio of butt 1Kg:10L and is
The sulfuric acid solution of 3wt% is warming up to 120 DEG C, catalyzing hydrolysis 1h, prepares xylose aqueous solution and hydrolysis that concentration is 12wt%
Slag；
Step 3: the catalyst sulfuric acid solution of 2mol/L is added in reactor, is passed through 200 DEG C in reactor bottom
Nitrogen is heated to catalyst solution reflux, adds NaCl to being saturated, stirring, which forms one, to be had fixed concentration catalyst and help
Then the xylose solution that obtained concentration is 12wt% is added in reactor by the rotation liquid level of catalyst by certain speed spray,
Xylose dehydration is carried out in liquid levels layer, generates furfural；
Embodiment 2
Step 1: dry weight ratio 1:2 is pressed, the obtained hydrolysis residue of step 2 in embodiment 1 is uniformly mixed with zinc chloride
It closes, is added in saggar, is placed in tube furnace, be warming up to 600 DEG C, activate 1.5h, room temperature discharging is down to, with the hydrochloric acid of 0.5M concentration
Solution impregnates 6h, and filtering is washed to no chloride ion, primary negative electrode material is prepared in 110 DEG C of dryings；
Step 2: primary negative electrode material being mixed with electrode pitch/alcohol suspending liquid, is dispersed with stirring 0.5h-1h, heating
Withdrawal liquid, solid are placed in drying box, and 85 DEG C of dry 5h-12h prepare pitch/primary negative electrode material mixed-powder；
Step 3: pitch/primary negative electrode material mixed-powder is transferred in tube furnace, under nitrogen protection, is warming up to
200 DEG C of constant temperature are heat-treated 1h, then are warming up to 800 DEG C of constant temperature heat treatment 1h, and cooling breaks up, prepares the porous cathode material of C/SiO2
Material.
Embodiment 3
The primary negative electrode material and electrode pitch powder for preparing step 1 in embodiment 2 according to mass ratio 2:10 are uniform
Mixing, the partial size through airslide disintegrating mill grinding dispersion to primary negative electrode material be 10 μm -15 μm, prepare mixed uniformly pitch/
Primary negative electrode material mixed-powder, is transferred in tube furnace, under nitrogen protection, is warming up to 200 DEG C of constant temperature heat treatment 1h, then
800 DEG C of constant temperature heat treatment 1h are warming up to, cooling breaks up, prepares asphalt modification negative electrode material.
Obviously, the above description of the embodiment is only used to help understand the method for the present invention and its core ideas, but right
For those skilled in the art, the spirit of claims of the present invention and the feelings of principle can not departed from
A variety of variations, modification and replacement, these improvement and modification are carried out to these embodiments under condition and also fall into the claims in the present invention
Within protection scope.
Claims (6)
1. a method of prepare rice husk base negative electrode material, which comprises the steps of:
Step 1: raw rice husk being sieved and is cleaned, and being crushed to partial size is 10mm-20mm, spare；
Step 2: the rice husk after smashing is added in reaction kettle, and concentration is added in the ratio of butt 1Kg:(5-10) L and is
The sulfuric acid solution of 1wt%-10wt%, is warming up to 100 DEG C -120 DEG C, and catalyzing hydrolysis 0.5h-2h prepares xylose aqueous solution and hydrolysis
Slag；Xylose solution send furfural Workshop Production furfural；
Step 3: pressing dry weight ratio 1:2, the obtained hydrolysis residue of step 2 uniformly mixed with zinc chloride, is added in saggar,
It is placed in tube furnace, is warming up to 500 DEG C -600 DEG C, 1h-2h is activated, discharges after being cooled to room temperature, with the hydrochloric acid solution of 0.5M concentration
2h-6h is impregnated, filtering is washed to no chloride ion, primary negative electrode material is prepared in 110 DEG C of dryings；
Step 4: by the primary negative electrode material in step 3 with electrode pitch uniformly mix dispersion 0.5h-1h, prepare pitch/
Primary negative electrode material mixed-powder；
Step 5: the pitch of step 4/primary negative electrode material mixed-powder is transferred in tube furnace, under nitrogen protection, is risen
Temperature to 150 DEG C of -250 DEG C of constant temperature are heat-treated 1h-2h, then are warming up to 600 DEG C of -1000 DEG C of constant temperature heat treatment 1h-2h, and cooling is broken up,
Prepare the porous negative electrode material of C/SiO2.
2. a kind of method for preparing rice husk base negative electrode material according to claim 1, which is characterized in that in the step 4
Pitch/primary negative electrode material mixed-powder preparation method be: by electrode pitch powder be added solvent in, be dispersed with stirring
0.5h-2h obtains pitch suspension or solution；Primary negative electrode material is added in pitch suspension or solution, is dispersed with stirring
0.5h-1h, heating recovery solvent, solid are placed in drying box, and 85 DEG C of dry 5h-12h prepare pitch/primary negative electrode material
Mixed-powder.
3. a kind of method for preparing rice husk base negative electrode material according to claim 2, which is characterized in that it is characterized in that,
The solvent is cyclohexanol, dehydrated alcohol, acetone, tetrahydrofuran, hexamethylene, a kind of in n-hexane or two kinds of mixture.
4. a kind of method for preparing rice husk base negative electrode material according to claim 1, which is characterized in that in the step 4
Go out pitch/primary negative electrode material mixed-powder preparation method be: by electrode pitch powder and primary negative electrode material uniformly mix
It closes, the partial size through airslide disintegrating mill grinding dispersion to primary negative electrode material is 10 μm -15 μm, prepares pitch/primary negative electrode material
Mixed-powder.
5. a kind of method for preparing rice husk base negative electrode material according to claim 1,2 or 4, which is characterized in that the step
Electrode pitch and the mass ratio of primary negative electrode material are (10-30) in rapid four: 100.
6. a kind of method for preparing rice husk base negative electrode material according to claim 2, which is characterized in that the electrode pitch
Solid-to-liquid ratio with solvent is (1-15) Kg:100L.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111072014A (en) * | 2019-12-26 | 2020-04-28 | 安徽理工大学 | Preparation method of graphene |
| CN112397701A (en) * | 2020-11-20 | 2021-02-23 | 江苏科技大学 | Rice husk-based silicon oxide/carbon composite negative electrode material and preparation method and application thereof |
| CN113178564A (en) * | 2021-04-25 | 2021-07-27 | 陈庆 | Silicon dioxide-carbon composite material and preparation method and application thereof |
| CN114874527A (en) * | 2022-05-19 | 2022-08-09 | 合肥略邦信息技术有限公司 | Bio-based controllable degradable mulching film and production method thereof |
Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101130793A (en) * | 2007-08-20 | 2008-02-27 | 吉林大学 | Novel method for producing fuel alcohol by rice hull and comprehensive utilization of resource |
| CN102071267A (en) * | 2010-12-15 | 2011-05-25 | 广东石油化工学院 | Method for coproducing xylose, white carbon black and active carbon from rice hulls |
| CN102509781A (en) * | 2011-10-27 | 2012-06-20 | 上海交通大学 | Silicon-carbon composite anode material and preparing method thereof |
| CN103579596A (en) * | 2013-11-08 | 2014-02-12 | 合肥国轩高科动力能源股份公司 | Preparation method of lithium ion battery cathode material |
| CN104037396A (en) * | 2014-05-27 | 2014-09-10 | 中南大学 | Carbon-carbon multi-component negative electrode material and preparation method thereof |
| US20160031843A1 (en) * | 2013-03-15 | 2016-02-04 | The Regents Of The University Of California | Synthesis of novel ionic liquids from lignin-derived compounds |
| CN105870422A (en) * | 2016-06-01 | 2016-08-17 | 大连海事大学 | C@SiOx material, preparation method thereof and application of C@SiOx material taken as negative electrode material of lithium ion battery |
| CN105932240A (en) * | 2016-05-11 | 2016-09-07 | 武汉科技大学 | Nano-silicon-carbon compound and preparation method and application thereof |
| JP2017091822A (en) * | 2015-11-10 | 2017-05-25 | 三重県 | Negative electrode active material for nonaqueous electrolyte secondary battery using chaff or rice straw carbide |
| CN106981644A (en) * | 2017-05-24 | 2017-07-25 | 华中科技大学 | A kind of porous carbon based on biomass/sulphur composite material and preparation method thereof and its application |
| CN109761235A (en) * | 2018-11-01 | 2019-05-17 | 南昌航空大学 | A kind of synthetic method of biological material walnut shell carbon material nitrating and its application in terms of anode of microbial fuel cell |
-
2019
- 2019-08-13 CN CN201910743855.6A patent/CN110429264B/en active Active
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101130793A (en) * | 2007-08-20 | 2008-02-27 | 吉林大学 | Novel method for producing fuel alcohol by rice hull and comprehensive utilization of resource |
| CN102071267A (en) * | 2010-12-15 | 2011-05-25 | 广东石油化工学院 | Method for coproducing xylose, white carbon black and active carbon from rice hulls |
| CN102509781A (en) * | 2011-10-27 | 2012-06-20 | 上海交通大学 | Silicon-carbon composite anode material and preparing method thereof |
| US20160031843A1 (en) * | 2013-03-15 | 2016-02-04 | The Regents Of The University Of California | Synthesis of novel ionic liquids from lignin-derived compounds |
| CN103579596A (en) * | 2013-11-08 | 2014-02-12 | 合肥国轩高科动力能源股份公司 | Preparation method of lithium ion battery cathode material |
| CN104037396A (en) * | 2014-05-27 | 2014-09-10 | 中南大学 | Carbon-carbon multi-component negative electrode material and preparation method thereof |
| JP2017091822A (en) * | 2015-11-10 | 2017-05-25 | 三重県 | Negative electrode active material for nonaqueous electrolyte secondary battery using chaff or rice straw carbide |
| CN105932240A (en) * | 2016-05-11 | 2016-09-07 | 武汉科技大学 | Nano-silicon-carbon compound and preparation method and application thereof |
| CN105870422A (en) * | 2016-06-01 | 2016-08-17 | 大连海事大学 | C@SiOx material, preparation method thereof and application of C@SiOx material taken as negative electrode material of lithium ion battery |
| CN106981644A (en) * | 2017-05-24 | 2017-07-25 | 华中科技大学 | A kind of porous carbon based on biomass/sulphur composite material and preparation method thereof and its application |
| CN109761235A (en) * | 2018-11-01 | 2019-05-17 | 南昌航空大学 | A kind of synthetic method of biological material walnut shell carbon material nitrating and its application in terms of anode of microbial fuel cell |
Non-Patent Citations (4)
| Title |
|---|
| JINLONG CUI等: "High surface area C/SiO2 composites from rice husks as a high-performance anode for lithium ion batteries", 《POWDER TECHNOLOGY》 * |
| ZHAOFENG WANG等: "Versatile Nanostructures from Rice Husk Biomass for Energy Applications", 《ANGEWANDTE CHEMIE-INTERNATIONAL EDITION 》 * |
| 刘树和 等: "稻壳制备硅/碳复合材料及储锂性能", 《材料导报》 * |
| 李玉姣: "生物质炭及其复合材料的制备及应用性能研究", 《中国优秀博硕士学位论文全文数据库(博士)工程科技Ⅰ辑》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111072014A (en) * | 2019-12-26 | 2020-04-28 | 安徽理工大学 | Preparation method of graphene |
| CN112397701A (en) * | 2020-11-20 | 2021-02-23 | 江苏科技大学 | Rice husk-based silicon oxide/carbon composite negative electrode material and preparation method and application thereof |
| CN113178564A (en) * | 2021-04-25 | 2021-07-27 | 陈庆 | Silicon dioxide-carbon composite material and preparation method and application thereof |
| CN113178564B (en) * | 2021-04-25 | 2023-01-03 | 陈庆 | Silicon dioxide-carbon composite material and preparation method and application thereof |
| CN114874527A (en) * | 2022-05-19 | 2022-08-09 | 合肥略邦信息技术有限公司 | Bio-based controllable degradable mulching film and production method thereof |
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