CN106505218A - A kind of waste mushroom leftover prepares mesoporous carbon and FeS2The method of combination electrode material - Google Patents
A kind of waste mushroom leftover prepares mesoporous carbon and FeS2The method of combination electrode material Download PDFInfo
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- CN106505218A CN106505218A CN201610997813.1A CN201610997813A CN106505218A CN 106505218 A CN106505218 A CN 106505218A CN 201610997813 A CN201610997813 A CN 201610997813A CN 106505218 A CN106505218 A CN 106505218A
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- mesoporous carbon
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- combination electrode
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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
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/9075—Catalytic material supported on carriers, e.g. powder carriers
- H01M4/9083—Catalytic material supported on carriers, e.g. powder carriers on carbon or graphite
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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
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
Abstract
The invention discloses one kind prepares mesoporous carbon and FeS with waste mushroom leftover2The method of combination electrode material, the method comprise the steps:(One), carbon source pretreatment;(Two), prepare mesoporous carbon;(Three)Prepare mesoporous carbon and iron hydroxide mixed solution;(Four), prepare mesoporous carbon and FeS2With combination electrode material;Advantages of the present invention:(One), adopt above-mentioned preparation method, it is achieved that mesoporous carbon and FeS2The synthesis of combination electrode material;(Two), the present invention can effectively solving discarded object mushroom bran process problem, turn waste into wealth, reduce environmental pollution, it is achieved that the cyclic utilization of waste, reduce production cost;(Three), preparation process is simple, process conditions gentle, easy to operate;(Four), the present invention expanded the new approaches of synthesising mesoporous carbon composite;(Five), the present invention prepare mesoporous carbon and FeS2Combination electrode material, stability are preferable, it is adaptable to used as the cathod catalyst of fuel cell, are remarkably reinforced can battery performance.
Description
Technical field
The present invention relates to technical field of composite preparation, and in particular to a kind of waste mushroom leftover prepares mesoporous carbon and FeS2
The method of combination electrode material.
Background technology
Since finding from fullerene and CNT, the application of material with carbon element obtains extensive exploitation, and wherein mesoporous carbon has height
The advantages of specific surface area, regulatable pore structure, good chemical stability, is widely used in electrode material, fuel cell, catalysis
Agent carrier, adsorbent etc..After mesoporous carbon is compound with precious metals pt, with good electro catalytic activity, fuel cell electricity is widely used in
Pole material.But precious metals pt is expensive, cause battery high cost, be unfavorable for industrializing.And Transition-metal dichalcogenide exists
Oxygen reduction catalytic activity height, good stability, low production cost in acid medium, with preferable application prospect.FeS2With mesoporous
Carbon composite with mesoporous carbon and the advantage of Transition-metal dichalcogenide, electrocatalytic oxidation reducing property and good stability,
It is the up-and-coming cathode catalyst material of a class.The synthesis of mesoporous carbon is different according to adopted template, be divided into soft template method and
Two class of hard template method, using organic matters such as phenolic resin, sucrose, health alcohol more than carbon source, process conditions are complicated, are difficult graphitization, raw
Produce high cost.Therefore, simplify synthesis technique, reduce carbon source cost, become mesoporous carbon research field important goal.
At present, Edible Fungi Industry Development is rapid, and with the rapid expansion of edible fungus culturing scale, waste material of edible mushroom is also more next
More.To these waste material of edible mushroom, it is improper that process is utilized, and not only waste of resource, also results in pollution environment.Waste material of edible mushroom also known as
Mushroom bran contains abundant lignin, cellulose and mineral matter, is preferable cheap carbon source.Activated carbon is prepared using mushroom bran, only several
Piece document report, such as patent(Publication number CN104310394A)With(Publication number CN101993069A).But it is situated between using mushroom bran synthesis
Hole material with carbon element does not have document report.In conjunction with above analysis, selection waste mushroom leftover is carbon source, with a kind of simple method, is had
The mesoporous carbon of high-specific surface area and FeS2Combination electrode material, is the work of a particularly significant scientific meaning.
Content of the invention
It is an object of the invention to provide one kind prepares mesoporous carbon and FeS with waste mushroom leftover2The method of combination electrode material, solution
Certainly the process problem of discarded object mushroom bran, realizes resource circulation utilization, reduces carbon source cost.Meanwhile, solve prior art and prepare Jie
Hole carbon and FeS2Combination electrode material exist particle size is big, reaction ratio is uncontrollable and the harsh problem of process conditions.
The technical scheme is that for achieving the above object, a kind of waste mushroom leftover prepares mesoporous carbon and FeS2Compound electric
The method of pole material, comprises the following steps:
First, the pretreatment of carbon source:Waste mushroom leftover is taken for carbon source, is crushed, add 1.0mol/L hydrochloric acid, 40~60 min of ultrasound to take out
Filtration distilled water is cleaned, and 50 DEG C of dryings are then placed in 0.5 mol/LCoCl2In solution, after at the uniform velocity 60~90min of stirring, 40 DEG C true
Empty dry, control waste mushroom leftover and CoCl2Mass ratio be 10:1;
2nd, mesoporous carbon is prepared:Step one gained sample is put into tube furnace, under nitrogen atmosphere, gradient increased temperature roasting 3~4 hours,
Room temperature is cooled to, is added in 1~2mol/L hydrochloric acid solutions, stirring at low speed 3 hours, after filtration under diminished pressure, first with distillation water washing,
Washed with ethanol again, then 40 DEG C of 70~100 min of vacuum drying, mesoporous carbon had both been obtained;
3rd, mesoporous carbon and iron hydroxide mixed solution are prepared:Step 2 gained mesoporous carbon is added to volume fraction for 20~40%
In glycol water, iron chloride is subsequently added, the mass ratio for controlling the mesoporous carbon and iron chloride for adding is 1:2~1:4, at the uniform velocity
20~40 min of stirring, are simultaneously added dropwise NH3˙H2O sets up pH, and mesoporous carbon and iron hydroxide mixed solution is obtained;
4th, mesoporous carbon and FeS are prepared2With combination electrode material:By in step 3 gained mesoporous carbon and iron hydroxide mixed solution
Reducing agent thiocarbamide is added, under certain frequency after 10~40 min of ultrasound, 120~160 DEG C of temperature control back flow reaction 15 hours is taken out
Filter, washing, 40 DEG C of vacuum drying, the ratio for controlling the amount of the material of the thiocarbamide and iron chloride for adding are 2:1, that is, obtain mesoporous carbon with
FeS2Combination electrode material.
The step one add in 50 g waste mushroom leftovers hydrochloric acid amount be 80~100 mL, supersonic frequency be 30~
50kHz.
The gradient increased temperature of the step 2 is first to be warmed up to 300~400 DEG C of constant temperature 1 hour, then is warmed up to 800~900 DEG C
Constant temperature 2~3 hours, stirring at low speed speed are 50 ~ 100r/min.
The at the uniform velocity mixing speed of the step 3 is 150 ~ 200r/min, and NH is wherein added dropwise3˙H2O adjusts pH=8~10.
The supersonic frequency of the step 4 is 30~50kHz, and vacuum drying vacuum is met less than or equal to 50Pa.
The waste mushroom leftover is mushroom mushroom bran, asparagus mushroom bran, HUAZIGU mushroom bran, auricuralia auricular bran, glossy ganoderma mushroom bran, white fungus
In mushroom bran one or more.
Advantages of the present invention:First, above-mentioned preparation method is adopted, it is achieved that mesoporous carbon and FeS2The conjunction of combination electrode material
Into;2nd, the process problem of present invention energy effectively solving discarded object mushroom bran, turns waste into wealth, reduces environmental pollution, it is achieved that waste
Recycle, reduce production cost;3rd, preparation process is simple, process conditions are gentle, easy to operate;4th, the present invention is expanded
The new approaches of synthesising mesoporous carbon composite;5th, the mesoporous carbon and FeS that prepared by the present invention2Combination electrode material, stability compared with
Good, it is adaptable to as the cathod catalyst of fuel cell, to be remarkably reinforced can battery performance.
Description of the drawings
Fig. 1, Fig. 2, Fig. 3 are the mesoporous carbon and FeS that embodiment 1, embodiment 2 and embodiment 3 are obtained respectively2Combination electrode
The graph of pore diameter distribution of material.
Specific embodiment
In order to be better understood from the present invention, technical scheme is described below by specific embodiment.
Embodiment 1:A kind of waste mushroom leftover prepares mesoporous carbon and FeS2The method of combination electrode material, specifically by following
Step is completed:
First, the pretreatment of carbon source:50 g waste mushroom leftovers are taken, is crushed, add 1.0mol/L hydrochloric acid 80mL, under the frequency of 30kHz
60 min of ultrasound, suction filtration distilled water are cleaned, and 50 DEG C of dryings are subsequently adding 0.5 mol/LCoCl280 mL of solution, at the uniform velocity stirs 60
After min, 40 DEG C of vacuum drying control waste mushroom leftover and CoCl2Mass ratio be 10:1;
2nd, mesoporous carbon is prepared:Step one gained sample is put into tube furnace, under nitrogen atmosphere, 300 DEG C of constant temperature 1 is first warmed up to little
When, then it is warmed up to 800 DEG C of constant temperature 3 hours, room temperature is cooled to, adds 1mol/L hydrochloric acid solution 50mL, 50r/min to stir 3 hours,
After filtration under diminished pressure, first with distillation water washing, then washed with ethanol, then 40 DEG C of 70 min of vacuum drying, mesoporous carbon had both been obtained;
3rd, mesoporous carbon and iron hydroxide mixed solution are prepared:1 g step 2 gained graphitization mesoporous carbons are taken, 50mL volumes are added
Fraction is 20% glycol water, is subsequently added 2 g iron chloride, at the uniform velocity stirs 20 min, be simultaneously added dropwise NH3˙H2O adjusts pH=8,
Prepared mesoporous carbon and iron hydroxide mixed solution;
4th, mesoporous carbon and FeS are prepared2With combination electrode material:By in step 3 gained mesoporous carbon and iron hydroxide mixed solution
Reducing agent thiocarbamide is added, under the frequency of 30kHz after ultrasonic 40 min, 120 DEG C of temperature control back flow reaction 15 hours, suction filtration, washing,
40 DEG C of vacuum drying, that is, obtain mesoporous carbon and FeS2Combination electrode material.
The thiocarbamide added in the present embodiment is 1.88g.
At the uniform velocity stir in the present embodiment, i.e., rotating speed is 150r/min.
The mesoporous carbon obtained by the present embodiment and FeS2Combination electrode material carries out pore-size distribution test, obtains pore-size distribution
As shown in figure 1, pore-size distribution is in 20nm or so, in macropore range.
Embodiment 2:A kind of waste mushroom leftover prepares mesoporous carbon and FeS2The method of combination electrode material, specifically by following
Step is completed:
First, the pretreatment of carbon source:50 g waste mushroom leftovers are taken, is crushed, add 1.0mol/L hydrochloric acid 90mL, under the frequency of 40kHz
50 min of ultrasound, suction filtration distilled water are cleaned, and 50 DEG C of dryings are subsequently adding 0.5 mol/LCoCl280 mL of solution, at the uniform velocity stirs 70
After min, 40 DEG C of vacuum drying control waste mushroom leftover and CoCl2Mass ratio be 10:1;
2nd, mesoporous carbon is prepared:Step one gained sample is put into tube furnace, under nitrogen atmosphere, 350 DEG C of constant temperature 1 is first warmed up to little
When, then it is warmed up to 850 DEG C of constant temperature 3 hours, and room temperature is cooled to, 1.5mol/L hydrochloric acid solution 50mL are added, 70r/min stirrings 3 are little
When, after filtration under diminished pressure, first with distillation water washing, then washed with ethanol, then 40 DEG C of 80 min of vacuum drying, be both obtained mesoporous
Carbon;
3rd, mesoporous carbon and iron hydroxide mixed solution are prepared:1 g step 2 gained mesoporous carbons are taken, addition 50mL volume fractions are
30% glycol water, is subsequently added 3 g iron chloride, at the uniform velocity stirs 30 min, be simultaneously added dropwise NH3˙H2O adjusts pH=9, is obtained and is situated between
Hole carbon and iron hydroxide mixed solution;
4th, mesoporous carbon and FeS are prepared2With combination electrode material:By in step 3 gained mesoporous carbon and iron hydroxide mixed solution
Reducing agent thiocarbamide is added, under the frequency of 40kHz after ultrasonic 20 min, 140 DEG C of temperature control back flow reaction 15 hours, suction filtration, washing,
40 DEG C of vacuum drying, that is, obtain mesoporous carbon and FeS2Combination electrode material.
The thiocarbamide quality added in the present embodiment is 2.80g.
At the uniform velocity stir in the present embodiment, i.e., rotating speed is 180r/min.
The mesoporous carbon obtained by the present embodiment and FeS2Combination electrode material carries out pore-size distribution test, obtains pore-size distribution
As shown in Fig. 2 the aperture of mesoporous carbon is substantially in macropore range.
Embodiment 3:A kind of waste mushroom leftover prepares mesoporous carbon and FeS2The method of combination electrode material, specifically by following
Step is completed:
First, the pretreatment of carbon source:50 g waste mushroom leftovers are taken, is crushed, add 1.0mol/L hydrochloric acid 100mL, under the frequency of 50kHz
40 min of ultrasound, suction filtration distilled water are cleaned, and 50 DEG C of dryings are subsequently adding 0.5 mol/LCoCl280 mL of solution, at the uniform velocity stirs 90
After min, 40 DEG C of vacuum drying control waste mushroom leftover and CoCl2Mass ratio be 10:1;
2nd, mesoporous carbon is prepared:Step one gained sample is put into tube furnace, under nitrogen atmosphere, 400 DEG C of constant temperature 1 is first warmed up to little
When, then it is warmed up to 900 DEG C of constant temperature 2 hours, and room temperature is cooled to, 2.0mol/L hydrochloric acid solution 50mL are added, 100r/min stirrings 3 are little
When, after filtration under diminished pressure, first with distillation water washing, then washed with ethanol, then 40 DEG C of 100 min of vacuum drying, be both obtained mesoporous
Carbon;
3rd, mesoporous carbon and iron hydroxide mixed solution are prepared:1 g step 2 gained mesoporous carbons are taken, addition 50mL volume fractions are
30% glycol water, is subsequently added 4 g iron chloride, at the uniform velocity stirs 40 min, be simultaneously added dropwise NH3˙H2O adjusts pH=10, is obtained and is situated between
Hole carbon and iron hydroxide mixed solution;
4th, mesoporous carbon and FeS are prepared2With combination electrode material:By in step 3 gained mesoporous carbon and iron hydroxide mixed solution
Reducing agent thiocarbamide is added, under the frequency of 50kHz after ultrasonic 10 min, 160 DEG C of temperature control back flow reaction 15 hours, suction filtration, washing,
40 DEG C of vacuum drying, that is, obtain mesoporous carbon and FeS2Combination electrode material.
The thiocarbamide quality added in the present embodiment is 3.74g.
At the uniform velocity stir in the present embodiment, i.e., rotating speed is 200r/min.
The mesoporous carbon obtained by the present embodiment and FeS2Combination electrode material carries out pore-size distribution test, obtains pore-size distribution
As shown in figure 3, the aperture of mesoporous carbon is in macropore range.
Claims (6)
1. one kind prepares mesoporous carbon and FeS with waste mushroom leftover2The method of combination electrode material, it is characterised in that:Described preparation side
Method comprises the steps:
(One), carbon source pretreatment:Waste mushroom leftover is taken for carbon source, is crushed, addition 1.0mol/L hydrochloric acid, 40~60 min of ultrasound,
Suction filtration distilled water is cleaned, and 50 DEG C of dryings are then placed in 0.5 mol/LCoCl2In solution, after at the uniform velocity 60~90min of stirring, 40 DEG C
Vacuum drying, control waste mushroom leftover and CoCl2Mass ratio be 10:1;
(Two), prepare mesoporous carbon:By step(One)Gained sample is put into tube furnace, under nitrogen atmosphere, gradient increased temperature roasting 3~4
Hour, room temperature being cooled to, is added in 1~2mol/L hydrochloric acid solutions, stirring at low speed 3 hours, after filtration under diminished pressure, first uses distilled water
Washing, then washed with ethanol, then 40 DEG C of 70~100 min of vacuum drying, had both been obtained mesoporous carbon;
(Three), prepare mesoporous carbon and iron hydroxide mixed solution:By step(Two)Gained mesoporous carbon is added to volume fraction for 20
In~40% glycol water, iron chloride is subsequently added, the mass ratio for controlling the mesoporous carbon and iron chloride for adding is 1:2~1:
4,20~40 min are stirred at the uniform velocity, NH is simultaneously added dropwise3˙H2O sets up pH, and mesoporous carbon and iron hydroxide mixed solution is obtained;
(Four), prepare mesoporous carbon and FeS2With combination electrode material:By step(Three)Gained mesoporous carbon and iron hydroxide mixed solution
Middle addition reducing agent thiocarbamide, under certain frequency after 10~40 min of ultrasound, 120~160 DEG C of temperature control back flow reaction 15 hours is taken out
Filter, washing, 40 DEG C of vacuum drying, the ratio for controlling the amount of the material of the thiocarbamide and iron chloride for adding are 2:1, that is, obtain mesoporous carbon with
FeS2Combination electrode material.
2. a kind of waste mushroom leftover according to claim 1 prepares mesoporous carbon and FeS2The method of combination electrode material, its are special
Levy and be:The step(One)In 50 g waste mushroom leftovers add hydrochloric acid amount be 80~100 mL, supersonic frequency be 30~
50kHz.
3. a kind of waste mushroom leftover according to claim 1 prepares mesoporous carbon and FeS2The method of combination electrode material, its are special
Levy and be:The step(Two)Gradient increased temperature is first to be warmed up to 300~400 DEG C of constant temperature 1 hour, then is warmed up to 800~900 DEG C of perseverances
Temperature 2~3 hours, stirring at low speed speed are 50 ~ 100r/min.
4. a kind of waste mushroom leftover according to claim 1 prepares mesoporous carbon and FeS2The method of combination electrode material, its are special
Levy and be:The step(Three)At the uniform velocity mixing speed be 150 ~ 200r/min, wherein be added dropwise NH3˙H2O adjusts pH=8~10.
5. a kind of waste mushroom leftover according to claim 1 prepares mesoporous carbon and FeS2The method of combination electrode material, its are special
Levy and be:The step(Four)Supersonic frequency is 30~50kHz, and vacuum drying vacuum is met less than or equal to 50Pa.
6. a kind of waste mushroom leftover according to claim 1 prepares mesoporous carbon and FeS2The method of combination electrode material, its are special
Levy and be:The waste mushroom leftover is mushroom mushroom bran, asparagus mushroom bran, HUAZIGU mushroom bran, auricuralia auricular bran, glossy ganoderma mushroom bran, white fungus
In mushroom bran one or more.
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CN109192942A (en) * | 2018-08-15 | 2019-01-11 | 中原工学院 | A kind of sodium ion battery electrode material and preparation method thereof |
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CN105098183A (en) * | 2014-05-21 | 2015-11-25 | 长春市朗欢科技有限公司 | Preparation for carbon anode material of lithium ion battery by using rice hull as raw material |
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