CN107265438A - Carbon nano-fiber aeroge and preparation method thereof derived from a kind of bacteria cellulose - Google Patents
Carbon nano-fiber aeroge and preparation method thereof derived from a kind of bacteria cellulose Download PDFInfo
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- CN107265438A CN107265438A CN201710447486.7A CN201710447486A CN107265438A CN 107265438 A CN107265438 A CN 107265438A CN 201710447486 A CN201710447486 A CN 201710447486A CN 107265438 A CN107265438 A CN 107265438A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0091—Preparation of aerogels, e.g. xerogels
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/10—Solid density
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
Abstract
The invention provides a kind of preparation method of carbon nano-fiber aeroge derived from bacteria cellulose, including：S1) bacteria cellulose is soaked in the solution containing inorganic ammonium salt, is then freeze-dried, bacteria cellulose aeroge is obtained；S2 carbon nano-fiber aeroge is obtained after the bacteria cellulose aeroge) is carried out into high temperature pyrolysis.Compared with prior art, the present invention is by adding inorganic ammonium salt as the catalyst to changing the route that bacteria cellulose fibre is pyrolyzed, effectively facilitate dehydration, decline carbon-to-oxygen ratio in the gaseous state and liquid product of loss, and then more carbon is remained among solid product, the carbon residue surplus after bacteria cellulose pyrolysis is improved, finally makes the output increased of carbon nano-fiber aeroge, product also has relatively low density, larger specific surface area, good electric conductivity and mechanical performance；And different densities and the carbon nano-fiber aeroge of mechanical performance can be prepared by adjusting the solution concentration of inorganic ammonium salt.
Description
Technical field
The invention belongs to carbon nano-fiber airsetting derived from technical field of nano material, more particularly to a kind of bacteria cellulose
Glue and preparation method thereof.
Background technology
Carbon aerogels have noticeable special performance, including low bulk density, bigger serface, abundant hole knot
Structure, high conductivity, good mechanical performance, stable chemical property and Environmental compatibility, therefore by the wide of researcher
General research.Carbon aerogels have in environmental protection, electrochemical energy storage and conversion, polymer science and advanced sensors field
Great application potential.
Carbon aerogels material is prepared at present, there is following several method：1st, prepared by carbonization organic matter gel, such as
Pekala etc. has invented the carbon aerogels (US patent 1989,4873218) of phenolic resin, passes through organic point in the aqueous solution
Son sol-gel process polymer precursor has been made, by pyrolysis, highly cross-linked organic aerogel be converted into it is porous,
Conductive three-dimensional aeroge (J.Mater.Sci.1989,24,3221), this method can prepare carbon aerogels on a large scale, but
Need to use poisonous reactant resorcinol and formaldehyde；2nd, prepared by chemical vapor deposition (CVD) method, current carbon nanometer
Pipe (CNT) sponge, grapheme foam, carbon nano tube/graphene mixing aeroge are all the focus materials of research, and chemical gaseous phase
Sedimentation is a kind of common method for synthesizing these carbon aerogels, and such as Cao Anyuan is prepared for CNT sponges using CVD
CNT skeletons including self assembly in (Adv.Mater.2010,22,617), this aeroge, being cross-linked with each other, porosity is more than
99%, high mechanical elasticity, using widely, but CVD processes need expensive predecessor, complicated equipment and technology, limit
Make it to mass produce, it is difficult to practical application；3rd, prepared by assembling primitive, the assembling primitive such as CNT and graphene is led to
Cross self assembling process and be changed into macroscopic material, to construct the carbon aerogels of one-component or miscellaneous ingredients, such as Worsley leads to
Cross mixing graphene oxide, resorcinol and formaldehyde and be prepared for a kind of high conductivity, the graphene aerogel of bigger serface
(J.Am.Chem.Soc.2010,132,14067), the high superfine mixed solution by CNT and graphene is freeze-dried, chemistry is gone back
Original, prepares a kind of extremely-low density, cycle performance is outstanding for compression, the pressure-dependent mixing aeroge of electrical conductivity
(Adv.Mater.2013,25,2554), but the assembling primitive of costliness has been used in these methods, equally limit theirs
Large-scale application.
Bacteria cellulose is formed by several special bacterial fermentations, and its composition is pure cellulose, cellulose Nanowire
Dimension forms the Nanofiber Network of three-dimension interaction crosslinking.It is cellulose nano-fibrous to be converted into carbon nano-fiber after pyrolysis, also protect
Original three-dimensional crosslinked network structure is held.Carbon nano-fiber aeroge has wide practical use derived from bacteria cellulose,
Already function as oils sorbing material (Chinese patent, ZL 201210562508.1), elastic conductor (NPG Asia
Mater.2012,4, e19), catalyst carrier (Chinese patent, ZL 201410093405.4), the electrode of ultracapacitor
(Adv.Mater.2013,25,4746) etc..Meanwhile, bacteria cellulose or a kind of typical biological material can be in works
Prepared in the fermentation process of industry, the material of carbon aerogels prepared compared to other, with it is cheap, originate it is wide, environmentally friendly,
It the advantage such as can prepare on a large scale, therefore be that one kind preferably prepares carbon by the converting carbon nano-fiber aeroge of bacteria cellulose
The method of aeroge.
But, usually prepare in carbon nano-fiber aeroge, pyrolytic process mass loss using bacterial fibers at present serious,
So that the carbon nano-fiber aeroge yield obtained is very low, and carbon nano-fiber aeroge volume contraction is serious, limits it and enters
One step application.
The content of the invention
In view of this, the technical problem to be solved in the present invention is to provide carbon nano-fiber derived from a kind of bacteria cellulose
Aeroge and preparation method thereof, the preparation method yield is higher.
The invention provides a kind of preparation method of carbon nano-fiber aeroge derived from bacteria cellulose, including：
S1) bacteria cellulose is soaked in the solution containing inorganic ammonium salt, is then freeze-dried, bacterium is obtained fine
The plain aeroge of dimension；
S2 carbon nano-fiber aeroge is obtained after the bacteria cellulose aeroge) is carried out into high temperature pyrolysis.
It is preferred that, the bacteria cellulose is first passed through except acid treatment, is then soaked in again in the solution containing inorganic ammonium salt.
It is preferred that, it is described except acid treatment is specially immersion deacidification；The time of the immersion deacidification is 5~10 days.
It is preferred that, the one or more in ammonium salt of the inorganic ammonium salt selected from phosphoric acid, sulfuric acid and hydrochloric acid.
It is preferred that, the concentration of inorganic ammonium salt is 0.1~1000mmol/L in the solution containing inorganic ammonium salt；The leaching
The time of bubble is 5~10 days.
It is preferred that, the step S1) be specially：
Bacteria cellulose will be soaked in the solution containing inorganic ammonium salt, then with after liquid nitrogen frozen, then freezed
Dry, obtain bacteria cellulose aeroge.
It is preferred that, the time of the liquid nitrogen frozen is 15~25min；The time of the freeze-drying is 3~5 days.
It is preferred that, the heating rate of high temperature pyrolysis is 2~10 DEG C/min；The temperature of the high temperature pyrolysis be 600 DEG C~
1400℃；The time of the high temperature pyrolysis is 1~3h.
It is preferred that, 400 DEG C~600 DEG C are cooled to 4~6 DEG C/min speed after the high temperature pyrolysis, then be down to room naturally
Temperature, obtains carbon nano-fiber aeroge.
Present invention also offers carbon nano-fiber aeroge prepared by a kind of above method, the carbon nano-fiber aeroge
It is interior doped with hetero atom.
The invention provides a kind of preparation method of carbon nano-fiber aeroge derived from bacteria cellulose, including：S1) will
Bacteria cellulose is soaked in the solution containing inorganic ammonium salt, is then freeze-dried, and obtains bacteria cellulose aeroge；
S2 carbon nano-fiber aeroge is obtained after the bacteria cellulose aeroge) is carried out into high temperature pyrolysis.Compared with prior art, originally
Invention effectively facilitates dehydration, made by adding inorganic ammonium salt as the catalyst to changing the route that bacteria cellulose fibre is pyrolyzed
Carbon-to-oxygen ratio declines in the gaseous state and liquid product of loss, and then more carbon is remained among solid product, makes bacterial fibers
Carbon residue surplus after element pyrolysis is improved, and finally makes the output increased of carbon nano-fiber aeroge, obtained carbon nanoporous aerogel
With relatively low density, larger specific surface area, good electric conductivity and mechanical performance；And the present invention utilizes bacteria cellulose
Carbon nano-fiber aeroge is prepared as presoma with inorganic ammonium salt, method is simple, and raw material is cheap and easy to get, it is easy to extensive raw
Production, the carbon nanoporous aerogel output increased obtained improves raw material availability, effectively reduces cost；The present invention is obtained simultaneously
Carbon nano-fiber aeroge shape remain intact, be conducive to various follow-up processing and application；Furthermore, due to the mistake in synthesis
Introduce in inorganic ammonium salt, pyrolytic process that Heteroatom doping is into carbon nano-fiber in journey, the carbon for obtaining Heteroatom doping is received
Rice fiber aeroge, can be used as fuel cell redox reactions catalyst, it is also possible to make electrode material for super capacitor, and
The properties such as density, conductance and the space of carbon nano-fiber aeroge can be controlled by adjusting the solution concentration of inorganic ammonium salt,
Prepare different densities and the carbon nano-fiber aeroge of mechanical performance.
Brief description of the drawings
Fig. 1 is the stereoscan photograph of the carbon nano-fiber aeroge obtained in the embodiment of the present invention 1；
Fig. 2 is the mechanical test figure of the carbon nano-fiber aeroge obtained in the embodiment of the present invention 1；
Fig. 3 is the stereoscan photograph of the carbon nano-fiber aeroge obtained in the embodiment of the present invention 2；
Fig. 4 is the mechanical test figure of the carbon nano-fiber aeroge obtained in the embodiment of the present invention 2；
Fig. 5 is the stereoscan photograph of the carbon nano-fiber aeroge obtained in the embodiment of the present invention 3；
Fig. 6 is the mechanical test figure of the carbon nano-fiber aeroge obtained in the embodiment of the present invention 3.
Embodiment
Below in conjunction with the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described,
Obviously, described embodiment is only a part of embodiment of the invention, rather than whole embodiments.Based in the present invention
Embodiment, the every other embodiment that those of ordinary skill in the art are obtained under the premise of creative work is not made, all
Belong to the scope of protection of the invention.
The invention provides a kind of preparation method of carbon nano-fiber aeroge derived from bacteria cellulose, including：S1) will
Bacteria cellulose is soaked in the solution containing inorganic ammonium salt, is then freeze-dried, and obtains bacteria cellulose aeroge；
S2 carbon nano-fiber aeroge is obtained after the bacteria cellulose aeroge) is carried out into high temperature pyrolysis.
Wherein, the present invention is not particularly limited to the source of all raw materials, is commercially available.
According to the present invention, preferably bacteria cellulose is first passed through except acid treatment；It is described except acid treatment be preferably immersion deacidification,
More preferably bacteria cellulose is soaked in deionized water and deacidified；The time of the immersion deacidification is preferably 5~10 days,
And need to change deionized water daily.
After acid treatment, bacteria cellulose is preferably cut into suitable size, be preferably (10~50) × (10~50) ×
(10~50) mm3, more preferably (15~40) × (10~40) × (10~40) mm3, it is further preferably (20~30) × (10~20)
× (10~20) mm3, most preferably 25 × 15 × 12mm3, then it is soaked in the solution containing inorganic ammonium salt；The Inorganic Ammonium
Salt is inorganic ammonium salt well known to those skilled in the art, has no special limitation, is preferably the ammonium of inorganic acid in the present invention
One or more in the ammonium salt of salt, more preferably phosphoric acid, sulfuric acid and hydrochloric acid；Inorganic Ammonium in the solution containing inorganic ammonium salt
The concentration of salt is preferably 0.1~1000mmol/L, more preferably 0.5~500mmol/L, is further preferably 0.5~200mmol/L,
Most preferably 0.5~100mmol/L；In some embodiments that the present invention is provided, nothing in the solution containing inorganic ammonium salt
The concentration of machine ammonium salt is preferably 100mmol/L；In some embodiments that the present invention is provided, the solution containing inorganic ammonium salt
The concentration of middle inorganic ammonium salt is preferably 10mmol/L；It is described to contain inorganic ammonium salt in other embodiments that the present invention is provided
Solution in the concentration of inorganic ammonium salt be preferably 0.5mmol/L；The time of the immersion is preferably 5~10 days, is made containing inorganic
Inside of the solution of ammonium salt well into bacteria cellulose.
After immersion, preferably first with after liquid nitrogen frozen, then it is freeze-dried, obtains bacterial cellulose gel.The liquid nitrogen
The time of freezing is preferably 15~25min, more preferably 20~25min.To avoid bacteria cellulose from rupturing during freezing, preferably will
It is firstly placed in solution cools down after 2~3min in liquid nitrogen, and bacteria cellulose touch to the side wall cryofixation of container, then by its
It is put into 15~25min of freezing in liquid nitrogen；Bacteria cellulose is avoided directly to be contacted with liquid nitrogen during freezing；The freeze-drying preferably exists
Carried out in freeze drier；The temperature of cold-trap is preferably -80 DEG C~-40 DEG C during the freeze-drying, more preferably -60 DEG C~-
50 DEG C, be further preferably -55 DEG C；The pressure during freeze-drying is preferably 0.01~0.06mbar, more preferably 0.03~
0.05mbar, is further preferably 0.04mbar；The time of the freeze-drying is preferably 3~5 days.
The bacteria cellulose aeroge is subjected to high temperature pyrolysis；The high temperature pyrolysis is carried out preferably in protective atmosphere；
The protective atmosphere be protective atmosphere well known to those skilled in the art, the present invention in be preferably nitrogen and/or argon gas；Institute
State bacterial cellulose gel and be preferably disposed in ceramic boat and carry out high temperature pyrolysis；The high temperature pyrolysis is carried out preferably in tube furnace；
The heating rate of the high temperature pyrolysis is preferably 2~10 DEG C/min, more preferably 3~8 DEG C/min, further preferably for 4~6 DEG C/
Min, most preferably 5 DEG C/min；The temperature of the high temperature pyrolysis is preferably 600 DEG C~1400 DEG C, more preferably 600 DEG C~1200
DEG C, it is further preferably 600 DEG C~1000 DEG C, is further preferably 800 DEG C~1000 DEG C, most preferably 800 DEG C；The high temperature pyrolysis when
Between be preferably 1~3h, that is, be warming up to after the temperature of high temperature pyrolysis insulation 1~3h, more preferably 2h.
After high temperature pyrolysis, 400 DEG C~600 DEG C are preferably cooled to, 450 DEG C~550 DEG C is more preferably cooled to, further preferably drops
Temperature is to 500 DEG C, then is down to room temperature naturally, obtains carbon nano-fiber aeroge；The speed of the cooling is preferably 4~6 DEG C/min,
More preferably 5 DEG C/min.In the present invention, the high temperature pyrolysis is with temperature-fall period, keeping normal pressure in tube furnace.
The present invention is effectively promoted by adding inorganic ammonium salt as the catalyst to changing the route that bacteria cellulose fibre is pyrolyzed
Enter dehydration, decline carbon-to-oxygen ratio in the gaseous state and liquid product of loss, and then more carbon is remained among solid product, make
Carbon residue surplus after bacteria cellulose pyrolysis is improved, and finally makes the output increased of carbon nano-fiber aeroge, obtained carbon nanometer
Aeroge also has relatively low density, larger specific surface area, good electric conductivity and mechanical performance；And the present invention is using carefully
Fungin and inorganic ammonium salt prepare carbon nano-fiber aeroge as presoma, and method is simple, and raw material is cheap and easy to get, it is easy to big
Large-scale production, the carbon nanoporous aerogel output increased obtained, improves raw material availability, effectively reduces cost；While this hair
Bright obtained carbon nano-fiber aeroge shape is remained intact, and is conducive to various follow-up processing and application；Furthermore, due to closing
Heteroatom doping in inorganic ammonium salt, pyrolytic process is introduced during and, into carbon nano-fiber, obtains Heteroatom doping
Carbon nano-fiber aeroge, can be used as fuel cell redox reactions catalyst, it is also possible to make electrode of super capacitor material
Material, and density, conductance and the space of carbon nano-fiber aeroge can be controlled by adjusting the solution concentration of inorganic ammonium salt
Etc. property, different densities and the carbon nano-fiber aeroge of mechanical performance are prepared.
Present invention also offers carbon nano-fiber aeroge prepared by a kind of above method, the carbon nano-fiber aeroge
It is interior doped with hetero atom；Carbon nano-fiber aeroge yield prepared by the present invention is high, and shape is remained intact, and can be used for adsorption material
Material, sensor material, catalyst backbone, electrode material and polymer composites.
In order to further illustrate the present invention, derived from a kind of bacteria cellulose provided with reference to embodiments the present invention
Carbon nano-fiber aeroge and preparation method thereof is described in detail.
Reagent used is commercially available in following examples.
Embodiment 1
1.1 take one piece of 320 × 240 commercially available × 12mm3Bacteria cellulose is large stretch of, and 10 are soaked in deionized water
My god, and deionized water is changed daily.The bacteria cellulose sheet after acid will be gone to be cut into 25 × 15 × 12mm3Fritter it is stand-by.
1.2 configuration 100mmol/L ammonium dihydrogen phosphates, fritter bacteria cellulose is soaked 5 days wherein.
1.3 by the fritter bacteria cellulose liquid nitrogen frozen 25min after immersion, is then transferred into freeze drier and dries
3 days, condenser temperature was -55 DEG C, and pressure is 0.04mbar.
1.4 are placed in the mixing aeroge for being freeze-dried obtained bacteria cellulose/ammonium dihydrogen phosphate in ceramic boat, then
It is put into tube furnace；Argon gas or nitrogen are passed through into tube furnace as protection gas, tube furnace first is warming up to 5 DEG C/min speed
800 DEG C, keep 2h；500 DEG C are cooled to 5 DEG C/min speed again, finally room temperature is down to naturally, the carbon Nanowire of black is obtained
Tie up aeroge.
The carbon nano-fiber aeroge quality obtained accounts for the 47.3% of bacteria cellulose aeroge quality, and density is
19.4mg/cm3, electrical conductivity is 0.0055S/cm.
The carbon nano-fiber aeroge obtained in embodiment 1 is observed using field emission scanning electron microscope, tied
Fruit is referring to Fig. 1, and the carbon nano-fiber aeroge that the present embodiment is obtained is made up of 30~70nm of diameter carbon nano-fiber, and centre has
Many cross-linked structures.
Mechanical test is carried out to the carbon nano-fiber aeroge obtained in embodiment 1, as a result referring to Fig. 2, Fig. 2 is this implementation
The carbon nano-fiber aeroge that example is provided compresses 30%, 50% and 80% mechanical test figure.Obtained as shown in Figure 2 in embodiment 1
The carbon nano-fiber Mechanical Properties of Aerogels arrived is good, and compression 80% still can be replied completely.
Embodiment 2
2.1 take one piece of 320 × 240 commercially available × 12mm3Bacteria cellulose is large stretch of, and 10 are soaked in deionized water
My god, and deionized water is changed daily.The bacteria cellulose sheet after acid will be gone to be cut into 25 × 15 × 12mm3Fritter it is stand-by.
2.2 configuration 10mmol/L ammonium dihydrogen phosphates, fritter bacteria cellulose is soaked 5 days wherein.
2.3, by the fritter bacteria cellulose after immersion, use liquid nitrogen frozen 25min, are then transferred into freeze drier and do
Dry 3 days, condenser temperature was -55 DEG C, and pressure is 0.04mbar.
2.4 are placed in the mixing aeroge for being freeze-dried obtained bacteria cellulose/ammonium dihydrogen phosphate in ceramic boat, then
It is put into tube furnace；Argon gas or nitrogen are passed through into tube furnace as protection gas, tube furnace first is warming up to 5 DEG C/min speed
800 DEG C, keep 2h；500 DEG C are cooled to 5 DEG C/min speed again, finally room temperature is down to naturally, the carbon Nanowire of black is obtained
Tie up aeroge.
Carbon nano-fiber aeroge quality obtained in embodiment 2 accounts for the 33.2% of bacteria cellulose aeroge quality,
Density is 6.2mg/cm3, electrical conductivity is 0.021S/cm.
The carbon nano-fiber aeroge obtained in embodiment 2 is observed using field emission scanning electron microscope, tied
Fruit is referring to Fig. 3.The carbon nano-fiber aeroge that the present embodiment is obtained as shown in Figure 3 by 15~30nm of diameter carbon nano-fiber structure
Into there are many cross-linked structures centre.
Mechanical test is carried out to the carbon nano-fiber aeroge obtained in embodiment 2, as a result referring to Fig. 4, Fig. 4 is this implementation
The carbon nano-fiber aeroge that example is provided compresses 30%, 50% and 80% mechanical test figure.As shown in Figure 4, carbon nano-fiber
Mechanical Properties of Aerogels is good, and compression 80% still can be replied completely.
Embodiment 3
3.1 take one piece of 320 × 240 commercially available × 12mm3Bacteria cellulose is large stretch of, and 10 are soaked in deionized water
My god, and deionized water is changed daily.The bacteria cellulose sheet after acid will be gone to be cut into 25 × 15 × 12mm3Fritter it is stand-by.
3.2 configuration 0.5mmol/L ammonium dihydrogen phosphates, fritter bacteria cellulose is soaked 5 days wherein.
3.3, by the fritter bacteria cellulose after immersion, use liquid nitrogen frozen 25min, are then transferred into freeze drier and do
Dry 3 days, condenser temperature was -55 DEG C, and pressure is 0.04mbar.
3.4 are placed in the mixing aeroge for being freeze-dried obtained bacteria cellulose/ammonium dihydrogen phosphate in ceramic boat, then
It is put into tube furnace；Argon gas or nitrogen are passed through into tube furnace as protection gas, tube furnace first is warming up to 5 DEG C/min speed
800 DEG C, keep 2h；500 DEG C are cooled to 5 DEG C/min speed again, finally room temperature is down to naturally, the carbon Nanowire of black is obtained
Tie up aeroge.
Carbon nano-fiber aeroge quality obtained in embodiment 3 accounts for the 15.0% of bacteria cellulose aeroge quality,
Density is 4.4mg/cm3, electrical conductivity is 0.038S/cm.
The carbon nano-fiber aeroge obtained in embodiment 3 is observed using field emission scanning electron microscope, tied
Fruit is referring to Fig. 5.The carbon nano-fiber aeroge that the present embodiment is obtained as shown in Figure 5 by 15~30nm of diameter carbon nano-fiber structure
Into there are many cross-linked structures centre.
Mechanical test is carried out to the carbon nano-fiber aeroge obtained in embodiment 3, as a result referring to Fig. 6, Fig. 6 is this implementation
The carbon nano-fiber aeroge that example is provided compresses 30%, 50% and 80% mechanical test figure.Carbon nano-fiber gas as shown in Figure 6
Gel good mechanical properties, compression 80% still can be replied completely.
Claims (10)
1. the preparation method of carbon nano-fiber aeroge derived from a kind of bacteria cellulose, it is characterised in that including：
S1) bacteria cellulose is soaked in the solution containing inorganic ammonium salt, is then freeze-dried, bacteria cellulose is obtained
Aeroge；
S2 carbon nano-fiber aeroge is obtained after the bacteria cellulose aeroge) is carried out into high temperature pyrolysis.
2. preparation method according to claim 1, it is characterised in that the bacteria cellulose is first passed through except acid treatment, so
It is soaked in again in the solution containing inorganic ammonium salt afterwards.
3. preparation method according to claim 2, it is characterised in that described except acid treatment is specially immersion deacidification；It is described
The time of immersion deacidification is 5~10 days.
4. preparation method according to claim 1, it is characterised in that the inorganic ammonium salt is selected from phosphoric acid, sulfuric acid and hydrochloric acid
Ammonium salt in one or more.
5. preparation method according to claim 1, it is characterised in that inorganic ammonium salt in the solution containing inorganic ammonium salt
Concentration be 0.1~1000mmol/L；The time of the immersion is 5~10 days.
6. preparation method according to claim 1, it is characterised in that the step S1) be specially：
Bacteria cellulose will be soaked in the solution containing inorganic ammonium salt, then with after liquid nitrogen frozen, then is freeze-dried,
Obtain bacteria cellulose aeroge.
7. preparation method according to claim 6, it is characterised in that the time of the liquid nitrogen frozen is 15~25min；Institute
The time for stating freeze-drying is 3~5 days.
8. preparation method according to claim 1, it is characterised in that the heating rate of high temperature pyrolysis is 2~10 DEG C/min；
The temperature of the high temperature pyrolysis is 600 DEG C~1400 DEG C；The time of the high temperature pyrolysis is 1~3h.
9. preparation method according to claim 1, it is characterised in that dropped after the high temperature pyrolysis with 4~6 DEG C/min speed
Temperature is to 400 DEG C~600 DEG C, then is down to room temperature naturally, obtains carbon nano-fiber aeroge.
10. a kind of carbon nano-fiber aeroge prepared by claim 1~9 any one, it is characterised in that the carbon nanometer
Doped with hetero atom in fiber aeroge.
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| CN110117000A (en) * | 2019-06-14 | 2019-08-13 | 中国科学技术大学 | A kind of bulk carbon nano-fiber aeroge and preparation method thereof |
| CN110589826A (en) * | 2019-10-15 | 2019-12-20 | 东北林业大学 | N, P co-doped carbon aerogel and preparation method and application thereof |
| CN111003799A (en) * | 2019-12-31 | 2020-04-14 | 丽水学院 | Biological carrier for sewage treatment and preparation method thereof |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103011864A (en) * | 2012-12-21 | 2013-04-03 | 中国科学技术大学 | Carbon nanofiber aerogel as well as preparation method and application thereof |
| CN105413729A (en) * | 2015-11-09 | 2016-03-23 | 中国科学技术大学 | Preparation method of nitrogen-doped carbon nanofiber aerogel with inlaid molybdenum carbide particles |
-
2017
- 2017-06-14 CN CN201710447486.7A patent/CN107265438A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103011864A (en) * | 2012-12-21 | 2013-04-03 | 中国科学技术大学 | Carbon nanofiber aerogel as well as preparation method and application thereof |
| CN105413729A (en) * | 2015-11-09 | 2016-03-23 | 中国科学技术大学 | Preparation method of nitrogen-doped carbon nanofiber aerogel with inlaid molybdenum carbide particles |
Non-Patent Citations (2)
| Title |
|---|
| LI-FENG CHEN ET AL.: "Three-Dimensional Heteroatom-Doped Carbon Nanofi ber Networks Derived from Bacterial Cellulose for Supercapacitors", 《ADVANCED FUNCTIONAL MATERIALS》 * |
| 吴振禹: "功能化碳纳米纤维材料的宏量制备及其性能研究", 《博士论文》 * |
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