CN103922301B - A kind of preparation method of multi-functional doped carbon nano-fiber aerogel - Google Patents
A kind of preparation method of multi-functional doped carbon nano-fiber aerogel Download PDFInfo
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- CN103922301B CN103922301B CN201410093405.4A CN201410093405A CN103922301B CN 103922301 B CN103922301 B CN 103922301B CN 201410093405 A CN201410093405 A CN 201410093405A CN 103922301 B CN103922301 B CN 103922301B
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Abstract
The invention discloses a kind of preparation method of multi-functional doped carbon nano-fiber aerogel, it is characterized in that: be immersed in organic dye solution after bacterial fibers is deacidified, absorb to saturated, then after lyophilize, again through high temperature pyrolysis, obtain multi-functional doped carbon nano-fiber aerogel.The present invention utilizes dye molecule and bacteria cellulose as the multi-functional doped carbon nano-fiber aerogel of precursor power, and method is simple, and cheaper starting materials is easy to get, and is easy to scale operation; The multi-functional doped carbon nano-fiber aerogel obtained can be used as the fuel cell redox reactions catalyzer of stability and high efficiency, also can be used as electrode material for super capacitor.
Description
Technical field
The invention belongs to technical field of nano material, particularly relate to a kind of preparation method of multi-functional doped carbon nano-fiber aerogel.
Background technology
High-performance, low price, eco-friendly heteroatoms (nitrogen, boron, phosphorus, sulphur etc.) doping carbon nano material store and conversion art, as having huge application prospect in fuel cell, dye-sensitized cell, solar cell, lithium ion battery, ultracapacitor at electrochemical energy.Such as, the carbon nanomaterial of doping can overcome traditional platinum or palladium-based catalyst high cost as redox reactions eelctro-catalyst in fuel cell, supplies limited, some intrinsic disadvantages such as intersection inactivation and poor durability etc.On the other hand, when using as electrode material for super capacitor, doping carbon nano material is by the compound of electric double layer capacitance and fake capacitance, show excellent capacitive property (as, large electrochemical capacitor, high power density energy density, and long circulating stability etc.).
Prior art discloses the multiple method for the preparation of Heteroatom doping carbon nanomaterial, mainly can be divided into two types: direct synthesis technique, aftertreatment synthesis method.Direct synthesis technique comprises chemical Vapor deposition process, Component seperation growth method, solvent-thermal method and arc discharge method etc.These methods all need to adopt special equipment and exacting terms, and output is very low, limits their large-scale application.Post treatment method is mainly included in heteroatoms atmosphere or with containing heteroatomic compound and carries out common heat treating process and plasma method.Among most method all inevitably relate to and adopt expensive and poisonous precursor, make it be difficult to practical application.
Organic dye, is widely used in many industries, and as weaving, papermaking, printing, plastics, medicine, foam, makeup, food, therefore the waste water of these industries is often containing excessive dye molecule.Some dyestuff and degraded derivative thereof have potential carinogenicity and toxicity, and their existence in water can cause and cause serious threat to hydrobiont and the mankind.Consider and be rich in heteroatoms in various organic dye, they can be used as precursor to prepare doping carbon nano material.Bacteria cellulose is a typical biological material; the production of industrial scale can be carried out by fermentation process; be that manufacture is ultralight, the excellent precursor of the carbon nanofiber aerogel of flexibility and high conductivity, has higher adsorptive power to organic dye molecule.
Summary of the invention
The present invention is for avoiding the weak point existing for above-mentioned prior art, there is provided a kind of dye molecule in trade effluent and bacteria cellulose of utilizing as the method for precursor power doped carbon nano-fiber aerogel, namely there is versatility, preparation technology can be simplified again, reduce preparation cost, environmental protection simultaneously.
Technical solution problem of the present invention, adopts following technical scheme:
The preparation method of the multi-functional doped carbon nano-fiber aerogel of the present invention, its feature is to carry out as follows:
A, by bacteria cellulose soak deacidify in deionized water, obtain bacteria cellulose for subsequent use;
B, described bacteria cellulose for subsequent use is immersed in organic dye solution, absorbs to saturated, obtain dyestuff/bacteria cellulose; In order to make immersion more thorough, bacteria cellulose for subsequent use can be cut into pane and the cubic block small pieces of suitable size; For ensureing that bacteria cellulose is absorbed with organic dye to saturated, soak time is provided with 3-7 days;
Dyestuff/bacteria cellulose described in c, use liquid nitrogen freezing, then carries out freezing rear dyestuff/bacteria cellulose the aerogel that drying obtains dyestuff/bacteria cellulose hydridization in freeze drier;
D, the aerogel of described dyestuff/bacteria cellulose hydridization is placed in tube furnace carries out high temperature pyrolysis, obtain multi-functional doped carbon nano-fiber aerogel.
Preferably, soaking the condition deacidified in deionized water described in step a is: soak time 3-7 days, and changes deionized water every day.
Preferably, organic dye solution described in step b is for solute with one or more the arbitrary combination in methylene blue (nitrogenous, sulphur), Congo red (nitrogenous, sulphur), C.I. 42685 (nitrogenous, sulphur), tropeolin-D (nitrogenous, sulphur), Viola crystallina (nitrogenous) and rhodamine B (nitrogenous), be that solvent is prepared with deionized water, described organic dye solution concentration is 0.1-3g/L.In addition, the malachite green dyestuff containing nitrogen element also can as solute.
Preferably, freezing described in the step c time is 20-30min.For avoiding dyestuff/bacteria cellulose bursting by freezing time freezing, first a beaker can be put into liquid nitrogen (-196 DEG C), take out after freezing 3-5min, then beaker is put into by adherent for dyestuff/bacteria cellulose, finally beaker is put into the freezing 20-30min of liquid nitrogen again, until dyestuff/bacteria cellulose can, easily from abate walls of beaker, avoid dyestuff/bacteria cellulose directly to contact with liquid nitrogen time freezing.
Preferably, the time dry described in step c is 3-5 days, and drying temperature is-50 DEG C, and pressure is 0.04mbar.
Preferably, described in steps d, the aerogel of described dyestuff/bacteria cellulose hydridization being placed in the method that tube furnace carries out high temperature pyrolysis is: the aerogel of described dyestuff/bacteria cellulose hydridization is placed in ceramic boat, then puts into tube furnace; In tube furnace, pass into argon gas or nitrogen as protection gas, first by tube furnace with the ramp to 500 DEG C of 1-3 DEG C/min, keep 1-3h, then with the ramp to 600 of 4-6 DEG C/min DEG C-1400 DEG C, keep 2-4h; Be cooled to 500 DEG C with the speed of 4-6 DEG C/min again, be finally naturally down to room temperature again; Normal pressure is kept in tube furnace.
Compared with the prior art, beneficial effect of the present invention is embodied in:
1, the present invention utilizes dye molecule and bacteria cellulose as the multi-functional doped carbon nano-fiber aerogel of precursor power, and method is simple, and cheaper starting materials is easy to get, and is easy to scale operation; The multi-functional doped carbon nano-fiber aerogel obtained can be used as the fuel cell redox reactions catalyzer of stability and high efficiency, also can be used as electrode material for super capacitor;
2, organic dye solution used in the present invention can obtain from industrial production wastewater, reduces environmental pollution, reduces costs simultaneously.
Accompanying drawing explanation
The stereoscan photograph of the multi-functional doped carbon nano-fiber aerogel that Fig. 1 obtains for the embodiment of the present invention 1;
The x-ray photoelectron power spectrum comparison diagram of non-doped carbon nano-fiber aerogel under the multi-functional doped carbon nano-fiber aerogel that Fig. 2 obtains for the embodiment of the present invention 1 and equal conditions;
Cyclic voltammetry curve in the 0.1M potassium hydroxide solution that multi-functional doped carbon nano-fiber aerogel is saturated at nitrogen and oxygen is saturated that Fig. 3 obtains for the embodiment of the present invention 1;
The chronoa mperometric plot of the multi-functional doped carbon nano-fiber aerogel that Fig. 4 obtains for the embodiment of the present invention 1 and commercial platinum C catalyst;
The multi-functional doped carbon nano-fiber aerogel that Fig. 5 obtains for the embodiment of the present invention 1 and commercial platinum C catalyst respond chronoa mperometric plot to methyl alcohol;
The cyclic voltammetry curve of multi-functional doped carbon nano-fiber aerogel in Water-Electrolyte under different charge-discharge velocity that Fig. 6 obtains for the embodiment of the present invention 2;
The constant current charge-discharge curve of multi-functional doped carbon nano-fiber aerogel under different current density that Fig. 7 obtains for the embodiment of the present invention 2;
The x-ray photoelectron energy spectrogram of the multi-functional doped carbon nano-fiber aerogel that Fig. 8 obtains for the embodiment of the present invention 3;
Embodiment
Embodiment 1
The preparation method of the multi-functional doped carbon nano-fiber aerogel of the present embodiment carries out as follows:
A, get 320 × 240 × 12mm that one piece of business buys
3bacteria cellulose is large stretch of, soaks 5 days disacidifies in deionized water, and changes deionized water every day, obtain bacteria cellulose for subsequent use;
B, the bacteria cellulose sheet after disacidify is cut into 50 × 20 × 12mm
3fritter, then in concentration be in the methylene blue solution of 1g/L soak 3 days, obtain dyestuff/bacteria cellulose;
C, use liquid nitrogen freezing dyestuff/bacteria cellulose 25min, then by freezing rear dyestuff/bacteria cellulose dry 4 days (drying temperature is-50 DEG C, and pressure is 0.04mbar) in freeze drier, obtain the aerogel of dyestuff/bacteria cellulose hydridization;
D, the aerogel of dyestuff/bacteria cellulose hydridization is placed in ceramic boat, then transfers to tube furnace; Pass in tube furnace nitrogen as protection gas, first from room temperature by tube furnace with the ramp to 500 DEG C of 1 DEG C/min, keep 1h, then with the ramp to 800 DEG C of 4 DEG C/min, keep 2h come abundant pyrolysis; Be cooled to 500 DEG C with the speed of 4 DEG C/min again, be finally naturally down to room temperature again, obtain the doped carbon nano-fiber aerogel of black; In reaction process, in tube furnace, keep normal pressure.
Field emission scanning electron microscope observation is carried out to the multi-functional doped carbon nano-fiber aerogel that the present embodiment obtains, result is see Fig. 1, as shown in Figure 1, the multi-functional doped carbon nano-fiber aerogel that the present embodiment obtains is the three dimensional skeletal structure that the fiber being 10-20nm by diameter is formed, and there are many crosslinked ducts centre.
Carry out x-ray photoelectron power spectrum sign to the multi-functional doped carbon nano-fiber aerogel that the present embodiment obtains, and compare with the x-ray photoelectron energy spectrogram of non-doped carbon nano-fiber aerogel, result is see Fig. 2.As shown in Figure 2, the multi-functional doping carbon nanoporous aerogel that the present embodiment obtains achieves nitrogen-atoms and sulphur atom to the doping of carbon nanofiber aerogel.
Using the carbon nanofiber aerogel of above-mentioned nitrogen, sulphur codoped as the eelctro-catalyst of redox reactions, obtain the cyclic voltammetry curve in saturated at nitrogen and that oxygen is saturated 0.1M potassium hydroxide solution respectively, result is see Fig. 3, and it is active that the multi-functional doped carbon nano-fiber aerogel that as can be seen from the figure the present embodiment obtains has significant redox reactions.
In the 0.1M potassium hydroxide solution that oxygen is saturated, utilize the stability of chronoa mperometric plot to the multi-functional doped carbon nano-fiber aerogel that the present embodiment obtains to characterize, and contrast with the chronoa mperometric plot of commercial platinum C catalyst, result is see Fig. 4, as can be seen from the figure in the 20000s test duration, the multi-functional doped carbon nano-fiber aerogel activity that the present embodiment obtains only has 6% loss, and under equal conditions, commercial platinum C catalyst loss 31% is active.
Methanol tolerance active testing is carried out to the multi-functional doped carbon nano-fiber aerogel that the present embodiment obtains, and with commercial platinum C catalyst, chronoa mperometric plot is responded to methyl alcohol and contrast, result is see Fig. 5, the doped carbon nano-fiber aerogel that the present embodiment obtains as we know from the figure effectively to the cross action of methanol tolerance, can have significant reaction preference.
From above-mentioned experiment, doped carbon nano-fiber aerogel provided by the invention can be applied to redox reactions catalyzer, has the advantages such as high reactivity, high stability, methanol tolerance cross action.
Embodiment 2
The preparation method of the multi-functional doped carbon nano-fiber aerogel of the present embodiment carries out as follows:
A, get 320 × 240 × 12mm that one piece of business buys
3bacteria cellulose is large stretch of, soaks 5 days disacidifies in deionized water, and changes deionized water every day, obtain bacteria cellulose for subsequent use;
B, the bacteria cellulose sheet after disacidify is cut into 50 × 20 × 12mm
3fritter, then in concentration be in the methylene blue solution of 1g/L soak 7 days, obtain dyestuff/bacteria cellulose;
C, use liquid nitrogen freezing dyestuff/bacteria cellulose 25min, then by freezing rear dyestuff/bacteria cellulose dry 5 days (drying temperature is-50 DEG C, and pressure is 0.04mbar) in freeze drier, obtain the aerogel of dyestuff/bacteria cellulose hydridization;
D, the aerogel of dyestuff/bacteria cellulose hydridization is placed in ceramic boat, then transfers to tube furnace; Pass in tube furnace nitrogen as protection gas, first from room temperature by tube furnace with the ramp to 500 DEG C of 3 DEG C/min, keep 1h, then with the ramp to 700 DEG C of 6 DEG C/min, keep 4h come abundant pyrolysis; Be cooled to 500 DEG C with the speed of 6 DEG C/min again, be finally naturally down to room temperature again, obtain the doped carbon nano-fiber aerogel of black; In reaction process, in tube furnace, keep normal pressure.
By the application of doped carbon nano-fiber aerogel and electrode material for super capacitor.Utilize cyclic voltammetry curve to characterize it, obtain the cyclic voltammetry curve of doped carbon nano-fiber aerogel in Water-Electrolyte under different charge-discharge velocity, result is see Fig. 6.As can be seen from the figure, at different rates, cyclic voltammetry curve shape maintains substantially, and the doped carbon nano-fiber aerogel that the present embodiment obtains shows good high rate performance.Utilize constant current charge-discharge to test the capacitive property of the doped carbon nano-fiber aerogel described in characterizing, obtain the constant current charge-discharge curve under different current density, result is see Fig. 7.As we know from the figure, be close to symmetrical charging and discharging curve and show that the doped carbon nano-fiber aerogel that the present embodiment obtains has electric double layer capacitance and fake capacitance simultaneously.
From above-mentioned experiment, doped carbon nano-fiber aerogel provided by the invention can be applied to electrode material for super capacitor, shows good high rate performance, and has electric double layer capacitance and fake capacitance simultaneously.
Experiment shows, prepared by the present invention, employing methylene blue is presoma, when 800 DEG C of pyrolysis gained doped carbon nano-fiber aerogels are as redox reactions eelctro-catalyst, has that take-off potential is high, limiting current is large, the advantage such as good stability and methanol tolerance cross action.Employing methylene blue is presoma, when the doped carbon nano-fiber aerogel of 700 DEG C of pyrolysis gained is as electrode material for super capacitor, has excellent high rate performance, and power density is large, cyclical stability is high.
Embodiment 3
The preparation method of the multi-functional doped carbon nano-fiber aerogel of the present embodiment carries out as follows:
A, get 320 × 240 × 12mm that one piece of business buys
3bacteria cellulose is large stretch of, soaks 5 days disacidifies in deionized water, and changes deionized water every day, obtain bacteria cellulose for subsequent use;
B, the bacteria cellulose sheet after disacidify is cut into 50 × 20 × 12mm
3fritter, then in concentration be in the rhodamine B solution of 3g/L soak 5 days, obtain dyestuff/bacteria cellulose;
C, use liquid nitrogen freezing dyestuff/bacteria cellulose 25min, then will the drying 5 days in freeze drier of freezing rear dyestuff/bacteria cellulose, obtain the aerogel of dyestuff/bacteria cellulose hydridization;
D, the aerogel of dyestuff/bacteria cellulose hydridization is placed in ceramic boat, then transfers to tube furnace; Pass in tube furnace nitrogen as protection gas, first from room temperature by tube furnace with the ramp to 500 DEG C of 1 DEG C/min, keep 1h, then with the ramp to 800 DEG C of 4 DEG C/min, keep 2h come abundant pyrolysis; Be cooled to 500 DEG C with the speed of 4 DEG C/min again, be finally naturally down to room temperature again, obtain the doped carbon nano-fiber aerogel of black; In reaction process, in tube furnace, keep normal pressure.
Carry out x-ray photoelectron power spectrum sign to the multi-functional doped carbon nano-fiber aerogel that the present embodiment obtains, and compare with the x-ray photoelectron energy spectrogram of non-doped carbon nano-fiber aerogel, result is see Fig. 8.As shown in Figure 8, the multi-functional doping carbon nanoporous aerogel that the present embodiment obtains achieves the doping of nitrogen-atoms to carbon nanofiber aerogel.
Claims (5)
1. a preparation method for multi-functional doped carbon nano-fiber aerogel, is characterized in that carrying out as follows:
A, by bacteria cellulose soak deacidify in deionized water, obtain bacteria cellulose for subsequent use;
B, described bacteria cellulose for subsequent use is immersed in organic dye solution, absorbs to saturated, obtain dyestuff/bacteria cellulose;
Dyestuff/bacteria cellulose described in c, use liquid nitrogen freezing, then carries out freezing rear dyestuff/bacteria cellulose the aerogel that drying obtains dyestuff/bacteria cellulose hydridization in freeze drier;
D, the aerogel of described dyestuff/bacteria cellulose hydridization is placed in tube furnace carries out high temperature pyrolysis, obtain multi-functional doped carbon nano-fiber aerogel, concrete grammar is: the aerogel of described dyestuff/bacteria cellulose hydridization is placed in ceramic boat, then puts into tube furnace; In tube furnace, pass into argon gas or nitrogen as protection gas, first by tube furnace with the ramp to 500 DEG C of 1-3 DEG C/min, keep 1-3h, then with the ramp to 600 of 4-6 DEG C/min DEG C-1400 DEG C, keep 2-4h; Be cooled to 500 DEG C with the speed of 4-6 DEG C/min again, be finally naturally down to room temperature again; Normal pressure is kept in tube furnace.
2. preparation method according to claim 1, is characterized in that: soaking the condition deacidified in deionized water described in step a is: soak time 3-7 days, and changes deionized water every day.
3. preparation method according to claim 1, it is characterized in that: organic dye solution described in step b is solute with one or more the arbitrary combination in methylene blue, Congo red, C.I. 42685, tropeolin-D, Viola crystallina and rhodamine B, is that solvent is prepared with deionized water, and described organic dye solution concentration is 0.1-3g/L.
4. preparation method according to claim 1, is characterized in that: the time of liquid nitrogen freezing described in step c is 20-30min.
5. preparation method according to claim 1, is characterized in that: the time dry described in step c is 3-5 days, and drying temperature is-50 DEG C, and pressure is 0.04mbar.
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| CN105060861B (en) * | 2015-08-06 | 2017-03-01 | 河南工程学院 | There is the porous ceramicss class catalyst carrier in two-dimensional nano duct and preparation method thereof |
| CN105036131A (en) * | 2015-09-08 | 2015-11-11 | 哈尔滨工业大学 | Preparing method of nanometer active carbon fiber |
| CN105174253A (en) * | 2015-09-08 | 2015-12-23 | 哈尔滨工业大学 | Method for preparing nano active carbon fiber in one step |
| CN105413729B (en) * | 2015-11-09 | 2018-05-01 | 中国科学技术大学 | A kind of preparation method of the nitrogen-doped carbon nano-fiber aeroge of molybdenum carbide particles insertion |
| CN105363435B (en) * | 2015-12-09 | 2018-03-27 | 广东南海普锐斯科技有限公司 | A kind of preparation method of oxygen reduction electro-catalyst Pt/N carbon nanocoils |
| CN105884356A (en) * | 2016-04-15 | 2016-08-24 | 华东师范大学 | Preparation method of carbon nanorod aerogel based on nanocellulose |
| CN106245375B (en) * | 2016-09-21 | 2018-06-01 | 佛山市南海德耀翔胜纺织有限公司 | A kind of dyestuff and its preparation and colouring method based on cellulose base aeroge |
| CN107159122A (en) * | 2017-06-30 | 2017-09-15 | 东北林业大学 | A kind of Heteroatom doping type charcoal-aero gel and preparation method thereof |
| CN108083253A (en) * | 2017-12-29 | 2018-05-29 | 中国林业科学研究院木材工业研究所 | Compound carbon aerogels of a kind of inorganic-cellulose and preparation method thereof |
| CN114853126A (en) * | 2022-04-29 | 2022-08-05 | 青岛科技大学 | Carbon fiber aerogel protected bismuth nanocluster and preparation method thereof |
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