CN106206072A - Corn straw prepares the method for activated carbon/Platinum Nanoparticles/polyaniline composite material - Google Patents
Corn straw prepares the method for activated carbon/Platinum Nanoparticles/polyaniline composite material Download PDFInfo
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- CN106206072A CN106206072A CN201610579322.5A CN201610579322A CN106206072A CN 106206072 A CN106206072 A CN 106206072A CN 201610579322 A CN201610579322 A CN 201610579322A CN 106206072 A CN106206072 A CN 106206072A
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- activated carbon
- platinum nanoparticles
- polyaniline
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- corn straw
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 146
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 title claims abstract description 101
- 229910052697 platinum Inorganic materials 0.000 title claims abstract description 40
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 36
- 229920000767 polyaniline Polymers 0.000 title claims abstract description 30
- 240000008042 Zea mays Species 0.000 title claims abstract description 23
- 235000002017 Zea mays subsp mays Nutrition 0.000 title claims abstract description 23
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 title claims abstract description 22
- 239000002131 composite material Substances 0.000 title claims abstract description 22
- 235000005822 corn Nutrition 0.000 title claims abstract description 22
- 239000010902 straw Substances 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 title claims abstract description 15
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims abstract description 34
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 30
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 22
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 18
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 16
- 230000004913 activation Effects 0.000 claims abstract description 14
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000002253 acid Substances 0.000 claims abstract description 12
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 11
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000011246 composite particle Substances 0.000 claims abstract description 8
- 239000007772 electrode material Substances 0.000 claims abstract description 8
- 238000002360 preparation method Methods 0.000 claims abstract description 5
- 238000012545 processing Methods 0.000 claims abstract description 5
- 239000000463 material Substances 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 239000003610 charcoal Substances 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 230000000977 initiatory effect Effects 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 238000010992 reflux Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 4
- NGNBDVOYPDDBFK-UHFFFAOYSA-N 2-[2,4-di(pentan-2-yl)phenoxy]acetyl chloride Chemical compound CCCC(C)C1=CC=C(OCC(Cl)=O)C(C(C)CCC)=C1 NGNBDVOYPDDBFK-UHFFFAOYSA-N 0.000 claims description 3
- 230000000694 effects Effects 0.000 claims description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 2
- 230000008859 change Effects 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
- 239000011734 sodium Substances 0.000 claims description 2
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- 239000001117 sulphuric acid Substances 0.000 claims description 2
- 235000011149 sulphuric acid Nutrition 0.000 claims description 2
- 239000003990 capacitor Substances 0.000 abstract description 7
- 229910052799 carbon Inorganic materials 0.000 abstract description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 abstract description 4
- 229910017604 nitric acid Inorganic materials 0.000 abstract description 4
- 235000016383 Zea mays subsp huehuetenangensis Nutrition 0.000 abstract 1
- 239000008187 granular material Substances 0.000 abstract 1
- 235000009973 maize Nutrition 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 19
- 230000015572 biosynthetic process Effects 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- 238000006116 polymerization reaction Methods 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- 238000002484 cyclic voltammetry Methods 0.000 description 3
- 238000011065 in-situ storage Methods 0.000 description 3
- 230000007935 neutral effect Effects 0.000 description 3
- 230000002194 synthesizing effect Effects 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000010306 acid treatment Methods 0.000 description 2
- 239000011157 advanced composite material Substances 0.000 description 2
- 230000001476 alcoholic effect Effects 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 235000013339 cereals Nutrition 0.000 description 2
- 229920001940 conductive polymer Polymers 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000003760 magnetic stirring Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229950000845 politef Drugs 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 239000012190 activator Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000002322 conducting polymer Substances 0.000 description 1
- 230000002079 cooperative effect Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical group Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000000840 electrochemical analysis Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 238000002847 impedance measurement Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 239000010908 plant waste Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 235000005074 zinc chloride Nutrition 0.000 description 1
- 239000011592 zinc chloride Substances 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/48—Conductive polymers
-
- 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
-
- 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
- Y02E60/13—Energy storage using capacitors
Landscapes
- Engineering & Computer Science (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
- Power Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a kind of method that corn straw prepares activated carbon/Platinum Nanoparticles/polyaniline composite material, first soak crushing maize stalk granule with phosphoric acid solution, in conjunction with microwave activation, preparation has active carbon with high specific surface area, and is used nitric acid activation processing;Then activated carbon after activation adds appropriate citric acid and the reduction chloroplatinic acid of the ethylene glycol solution containing NaOH, prepares the composite particles (C/Pt) of activated carbon/Platinum Nanoparticles;Finally C/Pt composite particles is put in the sulfuric acid solution containing finite concentration aniline, add appropriate hydrogen peroxide and cause, utilize Platinum Nanoparticles catalysed aniline to be polymerized, obtain activated carbon/platinum/polyaniline composite material (C/Pt/PAN).The present invention, by the proportionate relationship of regulation activated carbon with polyaniline, utilizes both synergism, the electrode material for super capacitor that processability is excellent.
Description
Technical field
The present invention relates to a kind of method that corn straw prepares activated carbon/Platinum Nanoparticles/polyaniline composite material, be specifically related to
A kind of Pt nano particle catalysed aniline in-situ polymerization deposited at corn straw preparing active carbon duct situ that utilizes, synthesis has high storage
The preparation method of the advanced composite material (ACM) of electrical property, belongs to composite functional material field.
Background technology
Active carbon with high specific surface area material is the positive electrode of the ultracapacitor having at present most application potential, but its cost
Account for whole condenser assembly this nearly 30%, be the main cause causing the production cost of ultracapacitor higher.Meet prepared
The requirements such as activated carbon specific surface area is big, stable performance, cost are relatively low, raw material must possess steady quality, easily obtain, with
Time the requirement such as production technology is simple, economy, environmental protection.Crop waste straw has just possessed such material characteristic, and domestic
Have been carried out more research.Wherein with corn stalk as raw material, prepare activated carbon with phosphoric acid or zinc chloride as activator, adopt
Prepare activated carbon with Muffle furnace or microwave heating to have studies have reported that and Patents.It must be noted that, at this
Even if obtaining the absorbent charcoal material of relatively high-ratio surface under the conditions of, its energy storage capacity there is also the limit, because its internal duct knot
Structure can not be utilized completely, requires further improvement.
Conductive polymer electrodes capacitor, as a kind of novel electrochemical capacitor, has electric conductivity and the electricity of excellence
Chemism, but its cycle life and thermal stability are poor, thus limit its application.Polyaniline (PAN) is typical
Conducting polymer, synthesis is simple, therefore, if with Polyaniline-modified activated carbon, it will be substantially improved active carbon electrode material
Chemical property, by cooperative effect between the two, obtains ideal electrode material for super capacitor.For polyaniline
Synthesis, general use chemical oxidization method synthesis, gained polyaniline by-product is many, and the degree of polymerization is difficult to control to.
Summary of the invention
It is an object of the invention to: provide a kind of corn straw to prepare the side of activated carbon/Platinum Nanoparticles/polyaniline composite material
Method, the active carbon with high specific surface area utilizing corn straw to prepare is matrix, by introducing Pt nano particle in situ, utilizes Pt to be catalyzed polyaniline
In-situ reaction, by the proportionate relationship of both regulations, utilizes both synergism, obtains the electrode of super capacitor of function admirable
Material;On the one hand advance the comprehensive utilization of straw, solve owing to straw is discarded and burns the wasting of resources brought and environment in violation of rules and regulations
Pollution problem;On the other hand a new thinking is provided for exploitation high-performance, low-cost super capacitor new material.
The technical solution of the present invention is the preparation method of this composite
Including step in detail below:
(1) corn stalk powder is broken to 50 mesh, after soaking under the conditions of 80 DEG C with certain density phosphoric acid solution, in microwave oven
Activation certain time, prepare the activated carbon of high-specific surface area;Wherein, the mass concentration of phosphoric acid solution is 18%, corn straw and phosphorus
The solid-to-liquid ratio of acid solution is 1:8, and soak time is 50min;Microwave activation power is 700W, and activation point is carried out, every time for 3 times
1min;
(2) activated carbon of step (1) gained is taken, in the salpeter solution of the 6mol/L being placed on its 10 ~ 20 times amount, 60 DEG C of constant temperature water baths
After heating a period of time, centrifugal, water washs to neutrality, dries, and obtains the activated carbon after activation processing;Wherein, salpeter solution is dense
Degree is 6mol/L, heated at constant temperature 4 ~ 6h;
(3) take the activated carbon after step (2) activation processing, add appropriate citric acid and the ethylene glycol solution containing 0.2M NaOH,
Inject appropriate platinum acid chloride solution, be heated to reflux 1 ~ 2h, take product and be centrifuged, wash, dry, prepare compound of activated carbon/Platinum Nanoparticles
Grain (C/Pt);Wherein the amount of activated carbon is in terms of g, the amount of chloroplatinic acid in terms of mmol, the amount ratio (g/ of activated carbon and the material of chloroplatinic acid
Mmol) it is 10:1 ~ 1:1;The amount of citric acid is in terms of g, and citric acid is 10:1 with amount ratio (g/mmol) of the material of chloroplatinic acid, hydrogen-oxygen
Change the amount (mol/mol) of material of sodium and chloroplatinic acid than being 25:1;
(4) taking activated carbon/Platinum Nanoparticles composite particles and the aniline of step (3), the sulphuric acid being placed in 100 ~ 200mL 0.6mol/L is molten
In liquid, add appropriate hydrogen peroxide initiation reaction, stirring 24 ~ 48h is stirred at room temperature on device, is centrifuged, washs, dries, prepare activity
Charcoal/Platinum Nanoparticles/polyaniline (C/Pt/PAN) combination electrode material;Wherein, the amount of activated carbon is in terms of g, and the amount of aniline, in terms of mL, is lived
The quality of property charcoal/aniline: volume ratio is (1:5 ~ 1:20), and hydrogen peroxide consumption is 0.2 ~ 0.5mL.
The invention have the advantages that 1, utilize corn straw to produce activated carbon, i.e. reduce environmental pollution, widen again the energy
Channel;2, utilize the Platinum Nanoparticles catalysed aniline polymerization of activated carbon duct situ deposition, be prevented effectively from polyaniline a large amount of by-product
The generation of thing, it is thus achieved that the polyaniline that the degree of polymerization is consistent, strengthens the electric conductivity of electrode material simultaneously, improves its storage electrical property, and this is
A kind of brand-new composite functional material not having been reported that in the past;3, the present invention utilizes phosphoric acid dip to combine microwave activation corn stalk
Stalk, prepares the activated carbon of high-ratio surface, and technique is simple, with low cost.
Accompanying drawing explanation
Fig. 1 activated carbon, activated carbon/Platinum Nanoparticles, the SEM photograph of activated carbon/Platinum Nanoparticles/polyaniline, wherein (a) is embodiment
The activated carbon C of the high-specific surface area obtained in 1, (b) is the C/Pt obtained in embodiment 1, and (c) is the C/Pt/ that embodiment 1 obtains
PAN;
Fig. 2 is the cyclic voltammetry curve of three kinds of materials of gained in embodiment 1.
Detailed description of the invention
Further illustrate the technical solution of the present invention below in conjunction with embodiment, it is right that these embodiments are not to be construed as
The restriction of technical scheme.
Embodiment 1: according to following steps synthesizing activity charcoal/Platinum Nanoparticles/polyaniline (activated carbon: aniline=1:5)
(1) the 4.0g corn straw being crushed to 50 mesh is immersed in the phosphoric acid solution of 32.0mL mass concentration 18%, at 80 DEG C of bars
After soaking 50min under part, then in the microwave oven that power is 700W, activate 3min, prepare the activated carbon (C) of high-specific surface area;
(2) activated carbon that 2.0g step (1) prepares is taken, in the nitric acid of 30.0mL 6mol/L after 60 DEG C of constant temperature water bath heating 4h,
Centrifugal, water washing, to neutral, dried, is obtained activated carbon;
(3) take the activated carbon after 0.4g step (2) acid treatment, add 0.38g citric acid and the ethylene glycol containing 0.2M NaOH is molten
Liquid 5.2mL, injects 1.0mL 0.04mol/L chloroplatinic acid, is heated to reflux 1.5h, takes product and be centrifuged, wash, dry, and prepares activity
Charcoal/Platinum Nanoparticles composite particles (C/Pt);
(4) take activated carbon/Platinum Nanoparticles composite particles, 2.0mL aniline that 0.4g step (3) prepares, be placed in 100mL 0.6mol/L
Sulfuric acid solution in, add 0.5mL mass concentration 30% hydrogen peroxide initiation reaction, on room temperature magnetic stirring apparatus stir 24h, from
The heart, wash, dry, prepare activated carbon/Platinum Nanoparticles/polyaniline (C/Pt/PAN) composite.
Embodiment 2: according to following steps synthesizing activity charcoal/Platinum Nanoparticles/polyaniline (activated carbon: aniline=1:20)
(1) the 8g corn straw being crushed to 50 mesh is immersed in the phosphoric acid solution of 64 mL mass concentrations 18%, 80 DEG C of conditions
After lower immersion 50min, then in the microwave oven that power is 700W, activate 3min, prepare the activated carbon (C) of high-specific surface area;
(2) activated carbon that 4g step (1) prepares is taken, in the nitric acid of 40mL 6mol/L after 60 DEG C of constant temperature water bath heating 4h, from
The heart, water washing, to neutral, dried, is obtained activated carbon;
(3) second two of the sodium hydroxide of the activated carbon after 0.4g step (2) processes, the citric acid of 1.9g, 26mL 0.2mol/L is taken
Alcoholic solution, 5mL 0.04mol/L platinum acid chloride solution in round-bottomed flask, be heated to reflux 2h, take product centrifuge washing dry, system
Obtain the composite of activated carbon/Platinum Nanoparticles;
(4) the prepared composite of activated carbon/Platinum Nanoparticles of 0.400g step (3), 8.0mL aniline are taken in 200mL 0.6mol/L
Sulfuric acid solution in, add 0.2mL mass concentration 30% hydrogen peroxide initiation reaction, stirring at normal temperature 36h, centrifuge washing dry,
Obtain the combination electrode material of C/Pt/PAN.
Embodiment 3: according to following steps synthesizing activity charcoal/Platinum Nanoparticles/polyaniline (activated carbon: aniline=1:10)
(1) the 4.0g corn straw being crushed to 50 mesh is immersed in the phosphoric acid solution of 32.0mL mass concentration 18%, at 80 DEG C of bars
After soaking 50min under part, then in the microwave oven that power is 700W, activate 3min, prepare the activated carbon (C) of high-specific surface area;
(2) activated carbon that 2.0g step (1) prepares is taken, in the nitric acid of 60.0mL 6mol/L after 60 DEG C of constant temperature water bath heating 4h,
Centrifugal, water washing, to neutral, dried, is obtained activated carbon;
(3) take the activated carbon after 0.4g step (2) acid treatment, add appropriate 0.76g citric acid and the second two containing 0.2M NaOH
Alcoholic solution 10.4mL, injects 2.0mL 0.04mol/L chloroplatinic acid, is heated to reflux 1.5h, takes product and be centrifuged, wash, dry, and prepares
Activated carbon/Platinum Nanoparticles composite particles (C/Pt);
(4) take activated carbon/Platinum Nanoparticles composite particles, 4.0mL aniline that 0.4g step (3) prepares, be placed in 100mL 0.6mol/L
Sulfuric acid solution in, add 0.3mL mass concentration 30% hydrogen peroxide initiation reaction, on room temperature magnetic stirring apparatus stir 48h, from
The heart, wash, dry, prepare activated carbon/Platinum Nanoparticles/polyaniline (C/Pt/PAN) composite.
Preparation mass fraction is the aqueous solution of politef of 5%, by the activated carbon/Platinum Nanoparticles of embodiment 1 gained/poly-
Aniline (C/Pt/PAN) composite, conductive black and politef mix for 85:10:5 in mass ratio, with mortar grinder extremely
Thick, it is spread upon equably one end of the 316L type rustless steel mesh sheet of long 4cm, wide 1cm, its application area be 1cm ×
1cm;After sample is dried, by the power of tablet machine 10MPa, sample is compressed, standby as working electrode.
Using CHI660B electrochemical workstation, at room temperature use three-electrode system, working electrode is for coating activated carbon
The stainless steel electrode of (activated carbon and polyaniline composite material), reference electrode is saturated calomel electrode, and auxiliary electrode is platinum electrode,
At 1mol L- 1H2SO4Solution is circulated the electro-chemical tests such as volt-ampere, time-measuring electric potential, AC impedance;In test, circulation
The potential range of volt-ampere test is 0~1V, and the electric current density of time-measuring electric potential test is 1A/g, the initial potential of ac impedance measurement
For OCP.
Fig. 1 is the scanning electron microscope (SEM) photograph of three kinds of electrode materials, and from Fig. 1 a, contrast is it can be seen that activated carbon surface has abundant
Pore structure, indication has bigger specific surface area;In Fig. 1 b, the surface of activated carbon and pore passage structure occur in that tiny receiving
Rice grain, the generation of indication Platinum Nanoparticles;And activated carbon/platinum/polyaniline occurs in that with polyaniline microscopic appearance close to vermiform
Polymer, shows the formation of polyaniline.
Fig. 2 is that 10mV/s sweeps the cyclic voltammetry curve of different materials under speed, it can be clearly seen that, C electrode not only capacity is relatively
Little, and there is not oxidoreduction peak, its cyclic voltammetry curve presents typical rectangular characteristic;And C/Pt/PAN electrode and
Pt/PAN electrode does not only have bigger ratio electric capacity, and there are obvious oxidoreduction peak, illustrates that the introducing of PAN adds method
Drawing pseudo-capacitance, the composite of C/Pt/PAN has more preferable reversibility simultaneously, has more excellent capacitor specific characteristics.
Claims (4)
1. the method that corn straw prepares activated carbon/Platinum Nanoparticles/polyaniline composite material, is characterized in that the preparation of this composite
Method includes step in detail below:
(1) corn stalk powder is broken to 50 mesh, after soaking under the conditions of 80 DEG C with certain density phosphoric acid solution, in microwave oven
Activation certain time, prepare the activated carbon of high-specific surface area;
(2) activated carbon of step (1) gained is taken, in the salpeter solution of the 6mol/L being placed on its 10 ~ 20 times amount, 60 DEG C of constant temperature water baths
After heating a period of time, centrifugal, water washs to neutrality, dries, and obtains the activated carbon after activation processing;
(3) take the activated carbon after step (2) activation processing, add appropriate citric acid and the ethylene glycol solution containing 0.2M NaOH,
Inject appropriate platinum acid chloride solution, be heated to reflux 1 ~ 2h, take product and be centrifuged, wash, dry, prepare compound of activated carbon/Platinum Nanoparticles
Grain (C/Pt);
(4) taking activated carbon/Platinum Nanoparticles composite particles and the aniline of step (3), the sulphuric acid being placed in 100 ~ 200mL 0.6mol/L is molten
In liquid, add appropriate hydrogen peroxide initiation reaction, stirring 24 ~ 48h is stirred at room temperature on device, is centrifuged, washs, dries, prepare activity
Charcoal/Platinum Nanoparticles/polyaniline (C/Pt/PAN) combination electrode material.
2. the method preparing activated carbon/Platinum Nanoparticles/polyaniline composite material according to the corn straw described in right 1, is characterized in that:
In the first step, the mass concentration of phosphoric acid solution is 18%, and corn straw is 1:8 with the solid-to-liquid ratio of phosphoric acid solution, and soak time is
50min;Microwave activation power is 700W, and activation point is carried out for 3 times, each 1min;
The method preparing activated carbon/Platinum Nanoparticles/polyaniline composite material according to the corn straw described in right 1, is characterized in that: the
In two steps, the concentration of salpeter solution is 6mol/L, and heated at constant temperature is 4 ~ 6h.
3. the method preparing activated carbon/Platinum Nanoparticles/polyaniline composite material according to the corn straw described in right 1, is characterized in that:
In 3rd step, the amount of activated carbon in terms of g, the amount of chloroplatinic acid in terms of mmol, the amount ratio (g/ of activated carbon and the material of chloroplatinic acid
Mmol) it is 10:1 ~ 1:1;The amount of citric acid is in terms of g, and citric acid is 10:1 with amount ratio (g/mmol) of the material of chloroplatinic acid, hydrogen-oxygen
Change the amount (mol/mol) of material of sodium and chloroplatinic acid than being 25:1.
4. the method preparing activated carbon/Platinum Nanoparticles/polyaniline composite material according to the corn straw described in right 1, is characterized in that:
In 4th step, the amount of activated carbon is in terms of g, and the amount of aniline is in terms of mL, and the mass volume ratio of activated carbon/aniline is (1:5 ~ 1:20),
Hydrogen peroxide consumption is 0.2 ~ 0.5mL.
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CN201610579322.5A CN106206072B (en) | 2016-07-22 | 2016-07-22 | The method that maize straw prepares activated carbon/Platinum Nanoparticles/polyaniline composite material |
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CN201610579322.5A CN106206072B (en) | 2016-07-22 | 2016-07-22 | The method that maize straw prepares activated carbon/Platinum Nanoparticles/polyaniline composite material |
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CN106206072A true CN106206072A (en) | 2016-12-07 |
CN106206072B CN106206072B (en) | 2018-01-30 |
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Cited By (3)
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CN112209356A (en) * | 2020-09-28 | 2021-01-12 | 浙江工业大学 | Class P2O5Structural material, and preparation method and application thereof |
CN113429977A (en) * | 2021-06-25 | 2021-09-24 | 阳煤丰喜肥业(集团)有限责任公司闻喜复肥分公司 | Saline-alkali soil conditioner |
CN113666389A (en) * | 2020-05-13 | 2021-11-19 | 南通新宙邦电子材料有限公司 | Preparation method of decolored potassium chloride solution |
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
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CN113666389A (en) * | 2020-05-13 | 2021-11-19 | 南通新宙邦电子材料有限公司 | Preparation method of decolored potassium chloride solution |
CN113666389B (en) * | 2020-05-13 | 2023-07-21 | 南通新宙邦电子材料有限公司 | Preparation method of decolored potassium chloride solution |
CN112209356A (en) * | 2020-09-28 | 2021-01-12 | 浙江工业大学 | Class P2O5Structural material, and preparation method and application thereof |
CN112209356B (en) * | 2020-09-28 | 2021-12-14 | 浙江工业大学 | Class P2O5Structural material, and preparation method and application thereof |
CN113429977A (en) * | 2021-06-25 | 2021-09-24 | 阳煤丰喜肥业(集团)有限责任公司闻喜复肥分公司 | Saline-alkali soil conditioner |
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