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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
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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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- 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
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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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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| JP2008300639A (en) * | 2007-05-31 | 2008-12-11 | Yokohama Rubber Co Ltd:The | Electrical double layer capacitor using polyaniline/porous carbon complex |
| CN102649843A (en) * | 2012-05-16 | 2012-08-29 | 中国林业科学研究院林产化学工业研究所 | Polyaniline/active carbon composite material and preparation method thereof |
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| JP2008300639A (en) * | 2007-05-31 | 2008-12-11 | Yokohama Rubber Co Ltd:The | Electrical double layer capacitor using polyaniline/porous carbon complex |
| CN102649843A (en) * | 2012-05-16 | 2012-08-29 | 中国林业科学研究院林产化学工业研究所 | Polyaniline/active carbon composite material and preparation method thereof |
Non-Patent Citations (2)
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| ZHOU GUANG_MIN等: "The effect of carbon particle morphology on the electrochemical properties of nanocarbon/polyaniline composites in supercapacitors", 《新型碳材料》 * |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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