CN109704308A - A kind of preparation method of biomass-based carbon electrode material - Google Patents
A kind of preparation method of biomass-based carbon electrode material Download PDFInfo
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- CN109704308A CN109704308A CN201910116106.0A CN201910116106A CN109704308A CN 109704308 A CN109704308 A CN 109704308A CN 201910116106 A CN201910116106 A CN 201910116106A CN 109704308 A CN109704308 A CN 109704308A
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Abstract
The present invention provides a kind of preparation methods of biomass-based carbon electrode material characterized by comprising step 1: pomelo peel being cut into bulk, supersound washing is dry, grind into powder；Ground pomelo peel powder metallurgy is carbonized in advance；Step 2: dispersing the pomelo peel powder being carbonized in advance in deionized water, iron chloride is added and is uniformly mixed；Step 3: the solution that step 2 is obtained is placed in a vacuum drying oven be dried in vacuo after, high-temperature calcination handles to obtain biomass-based carbon electrode material.Preparation process of the present invention avoids the use of strong acid and strong base, have the characteristics that environmentally friendly, prepared biomass-based carbon electrode material size is more uniform, it is simple to operate, economic and practical is strong, and raw material is relatively inexpensive to be easy to get, and production cost is low, preparation efficiency is high, has broad application prospects and market potential.
Description
Technical field
Present invention relates particularly to field of material technology, more particularly to a kind of preparation side of biomass-based carbon electrode material
Method.
Background technique
Biomass resource is early widely used to the preparation of traditional carbon material.Biomass-based carbon material refers to rich in carbon
Biomass material under conditions of anaerobic or anoxic, through under certain temperature decompose obtained by a kind of porosu solid powder.But
Its pore distribution and pore size mainly based on microcellular structure, there are the arrangement of complicated duct, pore size distribution compared with
Wide and not ideal enough chemical functionalities problem, limits its potential application value.But since it is with good conduction
Property is easy to the excellent performances such as functionalization, high chemical inertness and mechanical stability, in absorption, catalysis, gas storage, energy storage and conversion etc.
Field shows wide application prospect, to get more and more people's extensive concerning.
Carbon source for synthesizing carbon material is from a wealth of sources, mainly with the chemical industry such as phenolic resin, furfuryl alcohol, ethylene or synthesis material
Based on.However, these expensive raw material prices, and contain certain toxicity, cause the production of carbon material and Environmental costs higher,
It is set to be difficult to large scale preparation and application.Therefore, searching can recycle, is cheap, green carbon source becomes mesoporous carbon
One important directions of Materials.Biomass is abundance, cheap as a kind of natural renewable resource, and contains
Carbon amounts is higher, is a kind of environmentally friendly material for complying fully with Green Chemistry requirement.In recent years, it is made using biomass as carbon source
Standby carbon material is increasingly becoming research hotspot.Currently, the preparation method of biomass-based carbon material mainly include template, carbonizatin method and
Hydro-thermal method.It is different according to the synthesis path of carbon material and action principle, and template can be divided into hard template method and soft template
Method.The present invention is prepared for the excellent gauze bio base carbon material of pattern, and preparation process avoids the use of strong acid and strong base, has ring
Border friendly feature, simple to operate, economic and practical is strong, and raw material is relatively inexpensive to be easy to get, and production cost is low, can be applied to big
Technical scale metaplasia produces.
Summary of the invention
Present invention mainly solves the technologies such as the preparation process complexity of existing biomass-based carbon electrode material, severe reaction conditions
Problem, to provide a kind of preparation method of the biomass-based carbon electrode material of simple possible.
The technical scheme of the present invention is realized as follows:
A kind of preparation method of biomass-based carbon electrode material characterized by comprising
Step 1: pomelo peel being cut into bulk, ultrasound is washed, dry, grind into powder；By ground pomelo peel powder
High temperature is carbonized in advance；
Step 2: dispersing the pomelo peel powder being carbonized in advance in deionized water, iron chloride is added and is uniformly mixed；
Step 3: the solution that step 2 is obtained is placed in a vacuum drying oven be dried in vacuo after, high-temperature calcination is handled
To biomass-based carbon electrode material.
Preferably, the preparation method of the biomass-based carbon electrode material further include:
Step 4: after the grinding of obtained biomass-based carbon electrode material, being mixed with acetylene black and PTFE emulsion, ultrasound point
It dissipates, obtains electrode material.
Preferably, the pomelo peel powder in the step 1 and the amount ratio of the deionized water in step 2 are 1~2g:5
~20ml.
Preferably, the pre- carburizing temperature in the step 1 is 400~800 DEG C, and pre- carbonization time is 2~4h.
Preferably, the pomelo peel powder and FeCl in the step 23Amount ratio is 2:1~1:4.
Preferably, the drying temperature in the step 3 be 60~100 DEG C, drying time be 12~for 24 hours.
Preferably, the calcination temperature in the step 4 is 400~800 DEG C, and calcination time is 2~4h.
Preferably, the ratio of biomass-based carbon electrode material, acetylene black and PTFE emulsion is 8mg in the step 4:
1mg:100 μ l, the solid content of PTFE emulsion are 5%-20%.
The biomass-based carbon electrode material that the present invention obtains is with KOH solution or H2SO4Solution selects three electricity as electrolyte
Its chemical property of pole system of determination, three-electrode system reference electrode can be Ag/AgCl reference electrode, saturation HgCl2Reference
Electrode.
Compared with existing scheme, the beneficial effects of the present invention are:
Biomass-based carbon electrode material size prepared by the present invention is more uniform, simple to operate, economic and practical
By force, raw material is relatively inexpensive is easy to get, and production cost is low, and preparation efficiency is high, has broad application prospects and market potential.
Detailed description of the invention
Fig. 1 is the SEM figure of biomass-based carbon electrode material prepared by embodiment 1.
Fig. 2 is the SEM figure of biomass-based carbon electrode material prepared by embodiment 2.
Specific embodiment
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, those skilled in the art
Member can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Range.
Embodiment 1
A kind of preparation method of biomass-based carbon electrode material, specifically includes the following steps:
(1) pomelo peel is cut into bulk, is 40KHz with frequency, power is 300W ultrasound 30min, is washed with deionized
And dry, grind into powder；
(2) 1g ground pomelo peel powder is carbonized 2h in advance in 500 DEG C of high temperature；
(3) it disperses the pomelo peel powder being carbonized in advance in 5ml deionized water, by pomelo peel powder and FeCl3Quality
Than FeCl is added for 2:13And it is uniformly mixed；
(4) resulting solution is placed in a vacuum drying oven, is dried in vacuo 12h at 60 DEG C；
(5) dried sample is finally transferred to tube furnace, under nitrogen atmosphere, with 2 degrees Celsius of heating per minute
Rate is warming up to 600 DEG C of high-temperature calcination 2h, obtains biomass-based carbon electrode material.
(6) after obtained biomass-based carbon electrode material being ground to 100 mesh, electronic balance precise sample is used
8mg is added in the centrifuge tube of 2ml, and 1mg acetylene black and 100 μ l solid contents are added and mix for 10% PTFE emulsion, then put
Enter and carry out ultrasonic disperse in ultrasonic cleaning machine, obtains required electrode material.By electrode material preparation coated in nickel foam, apply
It applies with a thickness of 0.1~0.5 μm.
(7) it can be seen that the biomass-based carbon electrode material is at uniform reticular structure, directly from scanning electron microscope (SEM) photograph
Diameter is about 50nm.
(8) biomass-based carbon electrode material electrochemical property test: using electrochemical workstation, right in three-electrode system
The biomass-based carbon electrode of preparation carries out electrochemical property test.Using the KOH solution of 6M as electrolyte, working electrode is biomass
Base carbon electrode, auxiliary electrode are platinized platinum, and reference electrode is Ag/AgCl electrode.When current density is 0.5A/g, the ratio electricity of material
Holding is 303F/g.
Embodiment 2
A kind of preparation method of biomass-based carbon electrode material, specifically includes the following steps:
(1) pomelo peel is cut into bulk, is 40KHz with frequency, power is 300W ultrasound 30min, is washed with deionized
And dry, grind into powder；
(2) 2g ground pomelo peel powder is carbonized 2h in advance in 600 DEG C of high temperature；
(3) it disperses the pomelo peel powder being carbonized in advance in 10ml deionized water, is in mass ratio 1:1 addition
FeCl3And it is uniformly mixed；
(4) solution is placed in a vacuum drying oven, is dried in vacuo 12h at 70 DEG C；
(5) dried sample is finally transferred to tube furnace, under nitrogen atmosphere, with 2 degrees Celsius of heating per minute
Rate is warming up to 700 DEG C of high-temperature calcination 2h, obtains biomass-based carbon electrode material.
(6) after obtained biomass-based carbon electrode material being ground to 100 mesh, electronic balance precise sample is used
8mg is added in the centrifuge tube of 2ml, and 1mg acetylene black and 100 μ l solid contents are added and mix for 5% PTFE emulsion, then put
Enter and carry out ultrasonic disperse in ultrasonic cleaning machine, obtains required electrode material.Electrode material is applied in nickel foam, applied thickness
It is 0.1~0.5 μm.
(7) it can be seen that material is at uniform reticular structure from scanning electron microscope (SEM) photograph, diameter is about 50nm.
(8) biomass-based carbon electrode material electrochemical property test: using electrochemical workstation, right in three-electrode system
The biomass-based carbon electrode of preparation carries out electrochemical property test.With the H of 1M2SO4Solution is electrolyte, and working electrode is biology
Matter base carbon electrode, auxiliary electrode are platinized platinum, and reference electrode is Ag/AgCl electrode.When current density is 0.5A/g, the ratio of material
Capacitor is 295F/g.
Embodiment 3
A kind of preparation method of biomass-based carbon electrode material, specifically includes the following steps:
(1) pomelo peel is cut into bulk, is 40KHz with frequency, power is 300W ultrasound 30min, is washed with deionized
And dry, grind into powder；
(2) 1.5g ground pomelo peel powder is carbonized 4h in advance in 700 DEG C of high temperature；
(3) it disperses the pomelo peel powder being carbonized in advance in 15ml deionized water, is in mass ratio 1:2 addition
FeCl3And it is uniformly mixed；
(4) solution is placed in a vacuum drying oven, is dried in vacuo for 24 hours at 80 DEG C；
(5) dried sample is finally transferred to tube furnace, under nitrogen atmosphere, with 2 degrees Celsius of heating per minute
Rate is warming up to 700 DEG C of high-temperature calcination 4h, obtains biomass-based carbon electrode material.
(6) after obtained biomass-based carbon electrode material being ground to 100 mesh, electronic balance precise sample is used
8mg is added in the centrifuge tube of 2ml, and 1mg acetylene black and 100 μ l solid contents are added and mix for 15% PTFE emulsion, then put
Enter and carry out ultrasonic disperse in ultrasonic cleaning machine, obtains required electrode material.By electrode material coated in nickel foam, coating is thick
Degree is 0.1~0.5 μm.
(7) it can be seen that material is at uniform reticular structure from scanning electron microscope (SEM) photograph, diameter is about 50nm.
(8) biomass-based carbon electrode material electrochemical property test: using electrochemical workstation, right in three-electrode system
The biomass-based carbon electrode of preparation carries out electrochemical property test.Using 6M KOH solution as electrolyte, working electrode is biomass
Base carbon electrode, auxiliary electrode are platinized platinum, and reference electrode is Ag/AgCl electrode.When current density is 0.5A/g, the ratio electricity of material
Holding is 278F/g.
Embodiment 4
A kind of preparation method of biomass-based carbon electrode material, specifically includes the following steps:
(1) pomelo peel is cut into bulk, is 40KHz with frequency, power is 300W ultrasound 30min, is washed with deionized
And dry, grind into powder；
(2) 2g ground pomelo peel powder is carbonized 4h in advance in 700 DEG C of high temperature；
(3) it disperses the pomelo peel powder calcined in 20ml deionized water, FeCl is added for 1:4 in mass ratio3And
It is uniformly mixed；
(4) solution is placed in a vacuum drying oven, is dried in vacuo for 24 hours at 100 DEG C；
(5) dried sample is finally transferred to tube furnace, under nitrogen atmosphere, with 2 degrees Celsius of heating per minute
Rate is warming up to 800 DEG C of high-temperature calcination 4h, obtains biomass-based carbon electrode material.
(6) after obtained biomass-based carbon electrode material being ground to 100 mesh, electronic balance precise sample is used
8mg is added in the centrifuge tube of 2ml, and 1mg acetylene black and 100 μ l solid contents are added and mix for 20% PTFE emulsion, then put
Enter and carry out ultrasonic disperse in ultrasonic cleaning machine, obtains required electrode material.By electrode material coated in nickel foam, coating is thick
Degree is 0.1~0.5 μm.
(7) it can be seen that material is at uniform reticular structure from scanning electron microscope (SEM) photograph, diameter is about 50nm.
(8) biomass-based carbon electrode material electrochemical property test: using electrochemical workstation, right in three-electrode system
The biomass-based carbon electrode of preparation carries out electrochemical property test.With the H of 1M2SO4Solution is electrolyte, and working electrode is biology
Matter base carbon electrode, auxiliary electrode are platinized platinum, and reference electrode is Ag/AgCl electrode.When current density is 0.5A/g, the ratio of material
Capacitor is 316F/g.
Comparing with traditional biomass base carbon electrode material has more regular structure, and pattern can from SEM figure
Out.Biomass-based carbon electrode material size is more uniform, and simple to operate, economic and practical is strong, and raw material is relatively inexpensive to be easy to get,
Production cost is low, has broad application prospects and market potential.
Above content is only the basic explanation under present inventive concept, and that technical solution according to the present invention is done is any etc.
Effect transformation, is within the scope of protection of the invention.
Claims (9)
1. a kind of preparation method of biomass-based carbon electrode material characterized by comprising
Step 1: pomelo peel being cut into bulk, ultrasound is washed, dry, grind into powder；By ground pomelo peel powder metallurgy
Pre- carbonization；
Step 2: dispersing the pomelo peel powder being carbonized in advance in deionized water, iron chloride is added and is uniformly mixed；
Step 3: the solution that step 2 is obtained is placed in a vacuum drying oven be dried in vacuo after, high-temperature calcination, which is handled, is given birth to
Substance base carbon electrode material.
2. the preparation method of biomass-based carbon electrode material as described in claim 1, which is characterized in that further include: step 4:
After the grinding of obtained biomass-based carbon electrode material, is mixed with acetylene black and PTFE emulsion, ultrasonic disperse, obtain electrode material
Material.
3. the preparation method of biomass-based carbon electrode material as claimed in claim 2, which is characterized in that further include: it is described
Calcination temperature in step 4 is 400~800 DEG C, and calcination time is 2~4h.
4. the preparation method of biomass-based carbon electrode material as claimed in claim 2, which is characterized in that further include: it is described
The ratio of biomass-based carbon electrode material, acetylene black and PTFE emulsion is 8mg:1mg:100 μ l in step 4, and PTFE emulsion is consolidated
Content is 5%-20%.
5. the preparation method of biomass-based carbon electrode material as described in claim 1, which is characterized in that in the step 1
Pomelo peel powder and step 2 in deionized water amount ratio be 1~2g:5~20ml.
6. the preparation method of biomass-based carbon electrode material as described in claim 1, which is characterized in that the pre- carbonization temperature
Degree is 400~800 DEG C, and pre- carbonization time is 2~4h.
7. the preparation method of biomass-based carbon electrode material as described in claim 1, which is characterized in that the shaddock peel powder
End and FeCl3Amount ratio is 2:1~1:4.
8. the preparation method of biomass-based carbon electrode material as described in claim 1, which is characterized in that the drying temperature
Be 60~100 DEG C, drying time be 12~for 24 hours.
9. the preparation method of biomass-based carbon electrode material as described in claim 1, which is characterized in that the calcination temperature
It is 400~800 DEG C, calcination time is 2~4h.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111204734A (en) * | 2020-01-20 | 2020-05-29 | 上海应用技术大学 | Flaky biomass carbon material and preparation method thereof |
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| CN111204734A (en) * | 2020-01-20 | 2020-05-29 | 上海应用技术大学 | Flaky biomass carbon material and preparation method thereof |
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