CN106602079A - Method for preparing cellulose nanocrystalline-based derived carbon nanorod loaded with Pt nanoparticles - Google Patents
Method for preparing cellulose nanocrystalline-based derived carbon nanorod loaded with Pt nanoparticles Download PDFInfo
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- CN106602079A CN106602079A CN201611016661.9A CN201611016661A CN106602079A CN 106602079 A CN106602079 A CN 106602079A CN 201611016661 A CN201611016661 A CN 201611016661A CN 106602079 A CN106602079 A CN 106602079A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/88—Processes of manufacture
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/92—Metals of platinum group
- H01M4/925—Metals of platinum group supported on carriers, e.g. powder carriers
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention discloses a method for preparing a cellulose nanocrystalline-based derived carbon nanorod loaded with Pt nanoparticles. The method comprises the steps of adopting a cellulose raw material as an original base material, processing the cellulose by an acid catalysis method, removing an amorphous region and impurity content from the cellulose, and extracting cellulose nanocrystalline powder; next, performing reduction on H<2>PtCl6> of the Pt raw material through an ethanediol reduction method to prepare Pt-loaded cellulose nanocrystalline powder; and finally performing oxidization-carbonization processing to prepare the carbon nanorod loaded with the Pt material, wherein the carbon nanorod is relatively high in length-diameter ratio and has the diameter of 10-30nm and the length of 150-350nm. By effectively utilizing the biomass material namely the cellulose, the method has the characteristics of wide raw material resource, renewable property and no pollution; and the carbon nanorod load body is prepared by effective loading of the cellulose nanocrystalline with the Pt and then carbonization, so that the advantages of high loading firmness, high dispersity of the Pt nanoparticles, and stable dimensions are achieved.
Description
Technical field
This patent is related to a kind of preparation method of catalyst, the derivative carbon nano rod load of particularly a kind of Cellulose nanocrystal
The method of Pt nano-particle.
Background technology
With the consumption of the energy, the whole world is further urgently changed to the demand of the energy.In order to solve the energy for topic, novel battery
Be developed into a kind of needs of development.PEM dye cell is, with hydrogen as fuel, chemical energy directly to be switched to electricity
A kind of electrochemical appliance of energy.Used as a kind of new fuel cell, it has good portability, started quickly at low temperature, makes
Many advantages are extensively waited with scope, thus is got more and more people's extensive concerning.New, the efficient catalyst of exploitation is PEM dye
One of research emphasis of material battery.Nano platinum particle is one of catalyst important in PEM dye cell.
It is the effective way for reducing platinum consumption and improving cell catalyst performance from excellent support materials.At present, study
In mostly using white carbon black, carbon nano-fiber and CNT as nano platinum particle support materials, these support materials are general
Attack a vital point and the feature such as mechanical property, stronger chemical stability with specific surface area is big, good.However, these material with carbon element tables
The chemical inertness in face causes surface payload nano platinum particle to become difficult.Although can be in carbon nanometer using infusion process
Pipe surface supported platinum nano particle, but because platinum load capacity is less, limit the use of the method.In recent years, research worker is adopted
Load factor of the nano platinum particle in carbon nano tube surface is improved with many new techniques, new method.Most common method is first will
Carbon nano tube surface carries out strong acid oxidation processes so as to which surface produces the functionalization groups such as hydroxyl, aldehyde radical, carboxyl, adopts
Different method of reducing, can be in the controllable nano platinum particle of the carbon nano tube surface deposition morphology of functionalization.Such as U.S. Xing
Et al. first using ultrasonic acidification CNT, directly deposit monodispersed platinum on the carbon nanotubes using ethylene glycol afterwards and receive
Rice corpuscles（Xing Y. Synthesis and Electrochemical Characterization of Uniformly-
Dispersed High Loading Pt Nanoparticles on Sonochemically-Treated Carbon
Nanotubes[J]. Journal of Physical Chemistry B, 2004, 108(50):19255-19259.）, plus
The put on airs Dodelet seminar of Montreal engineering college adopts formic acid for reducing agent, directly in the CNT of carboxylic acid functional
Upper growth platinum nanometer rods（Sun S, Yang D, Zhang G, et al. Synthesis and Characterization
of Platinum Nanowire–Carbon Nanotube Heterostructures[J]. Chemistry of
Materials, 2007, 19(26):6376-6378.）.However, in chemical treating process, CNT one-dimentional structure meeting
It is destroyed, and in it the physical property such as optically and electrically can change.
In order to realize Pt nanoparticle payload on the carbon material, and the self structure and property of material with carbon element are not destroyed
Matter, Spain Correa-Duarte proposes that non-covalent bond technology effectively can load various nanoparticles in carbon material surface, and
Do not destroy in material with carbon element structure and property（Grzelczak M, Correa‐Duarte M, Salgueiriño‐
Maceira V, et al. Pt‐Catalyzed Formation of Ni Nanoshells on Carbon Nanotubes
[J]. Angewandte Chemie International Edition, 2007, 46(37):7026-30.）.It is non-covalent to repair
Decorations technology is that the nano platinum particle for loading morphology controllable in carbon material surface indicates a new approach.Similar, the Chinese Academy of Sciences
A cube Pt nanocrystal is directly loaded in CNT table by Changchun applied chemistry Suo Yangxiurong group using non-covalent modification technology
Face.（Yang W, Wang X, Yang F, et al. Carbon Nanotubes Decorated with Pt
Nanocubes by a Noncovalent Functionalization Method and Their Role in Oxygen
Reduction[J]. Advanced Materials, 2008, 20(13):2579-2587.）The complex of gained is to oxygen
Reduction reaction shows good catalytic effect, can apply to the fields such as PEM dye cell.Even so, using
Carbon pipe is used as carrier, however it remains carbon pipe complicated process of preparation, Pt nanoparticle payload rate be not high, electrostatic adsorption power
The problems such as yielding during weak, load use.
The content of the invention
Object of the present invention is to provide a kind of side of the derivative carbon nano rod supporting Pt nano-particle of Cellulose nanocrystal
Method.The present invention is effectively utilized biological material cellulose, with raw material sources are wide, renewable, free of contamination feature；Cellulose
Again Jing carbonizations prepare carbon nano rod load after nanocrystalline and Pt payload, strong with load fastness, the dispersion of Pt nano-particle
Good, the advantage of dimensionally stable of property.
To reach above-mentioned purpose, the technical scheme is that：
A kind of method of the derivative carbon nano rod supporting Pt nano-particle of Cellulose nanocrystal, comprises the steps：Using cellulose
Raw material is processed cellulose as primary substrate with acid catalyzed process, remove cellulose in amorphous region and impurity into
Point, Cellulose nanocrystal powder is extracted, then by reduction of ethylene glycol method to Pt raw material H2PtCl6Reduced and born with preparing Pt
Cellulose nanocrystal powder is carried, after eventually passing oxidation-charing process, a diameter of 10-30 nm is prepared, length is 150-350
Nm, with the carbon nano rod supporting Pt material compared with big L/D ratio.
The extracting method of described Cellulose nanocrystal powder is：Cellulose is placed in hydrochloric acid solution and is configured to cellulose
Suspension, suspension is transferred to into water heating kettle and is reacted, reaction terminate after, by reactant liquor stratification, remove upper strata clear
Liquid obtains Cellulose nanocrystal suspension, through neutralization, filters, freezes, being dried prepared Cellulose nanocrystal powder；It is wherein described
Concentration of hydrochloric acid solution be 5 mol/L；Solid content of the cellulose in hydrochloric acid is 0.005-0.05 g/mL；Suspension liquid is tied up to
Reaction temperature in water heating kettle is 100-120 DEG C, and the response time is 1-5h.
Described cellulosic raw material is using the one kind in cellulose crystallite, Cotton Gossypii, paper scrap, wood flour, Bacterial cellulose.
Described reduction of ethylene glycol method prepares the nanocrystalline method of Pt carrying fibers element：Take 50 ~ 55 mg cellulose nanometers
Crystalline flour end adds 8 ~ 12 mL H2PtCl6In aqueous solution, continuously add and stirred after 23 ~ 28 mL ethylene glycol and 3 ~ 6 mL KOH solutions
Uniformly；Reaction is filtered after terminating with acetone cleaning, and Pt carrying fibers element manocrystalline powders are obtained after being finally vacuum dried；Wherein institute
The H for stating2PtCl6Concentration of aqueous solution be 0.007 ~ 0.01 mol/L, KOH solution concentration be 0.03 ~ 0.05 mol/L, reaction temperature
For 125 ~ 134 DEG C, the h of response time 1.5 ~ 3.
The method that the nanocrystalline supporting Pt of described oxidation-carbon fiber element prepares carbon nano rod supporting Pt material is：Will system
The standby Pt carrying fibers element manocrystalline powders for obtaining are placed directly within tube furnace under air atmosphere, carry out high temperature oxidation process, so
After be passed through protective gas, a diameter of 10-30 nm is prepared at high temperature, length is loaded with Pt and receives for 150-350 nm
The carbon nano rod of rice grain, wherein temperature during described high temperature oxidation process is 200-350 DEG C, at 1-3 h high temperature
Reason；Using nitrogen or argon, described protective gas is warming up to described protective gas after being passed through using progressively temperature-raising method
1000-1500 DEG C, the high temperature carbonization time is 1-3h.
The invention has the beneficial effects as follows：The method that carbon nano rod is prepared based on Cellulose nanocrystal proposed by the invention,
Biological material cellulose is effectively utilized, with raw material sources are wide, renewable, free of contamination feature；By regulating and controlling cellulose
The factor such as raw material, acid concentration, hydrolysis temperature, hydrolysis time in nanocrystalline preparation process, realizes Cellulose nanocrystal and most
The Modulatory character of whole carbon nano rod size；Because substantial amounts of hydroxyl is contained on Cellulose nanocrystal surface, Pt nano-particle is in fiber
The load effect of plain nanocrystal surface is uniform, and load fastness is strong, and dimensionally stable, the carbon nano rod prepared after oxidized-carbonization is straight
Footpath is 10-30 nm, and length is 150-350 nm, has traditional carbon fibres, Graphene, CNT in fuel cell field
Deng not available size advantage.
Specific embodiment
Embodiment 1
A kind of method of the derivative carbon nano rod supporting Pt nano-particle of Cellulose nanocrystal of the present embodiment, comprises the steps：
By Microcrystalline Cellulose（Production code member 68005761, traditional Chinese medicines reagent）It is placed in the hydrochloric acid solution that concentration is 5 mol/L and is configured as
Cellulose solid content is the suspension of 0.005 g/mL, suspension is transferred at 100 DEG C of water heating kettle and is reacted, and reacts 5 h
Afterwards, by reactant liquor stratification, the supernatant is removed, during remaining Cellulose nanocrystal suspension is titrated with ammonia
With lyophilization after filtration is obtained Cellulose nanocrystal powder；Take 55 mg Cellulose nanocrystals powder and add 12 mL 0.007
The H of mol/L2PtCl6In aqueous solution, continuously add and stirred after the KOH solution of 28 mL ethylene glycol and the mol/L of 3 mL 0.05
It is even.Reaction temperature is 134 DEG C, and the response time is 1.5 h, and reaction is filtered after terminating with acetone cleaning, after being finally vacuum dried i.e.
Obtain Pt carrying fibers element manocrystalline powders.Then gained Pt carrying fibers element manocrystalline powders are placed directly within into air in tube furnace
At 200 DEG C of atmosphere, the h of high temperature oxidation process 3 is carried out, then pass to protective gas nitrogen, be progressively warming up to 1500 DEG C, Jing
Cross after 1 h carbonizations and prepare the carbon nano rod for being loaded with Pt nano-particle at high temperature.
Jing field emission microscopy observations, the carbon nano rod average diameter for being loaded with Pt nano-particle manufactured in the present embodiment
For 30 nm, average length is 350 nm.
A kind of method of the derivative carbon nano rod supporting Pt nano-particle of Cellulose nanocrystal that the present embodiment is proposed, effectively
Biological material cellulose is make use of, with raw material sources are wide, renewable, free of contamination feature；By regulating and controlling cellulose nanometer
The factor such as raw material, acid concentration, hydrolysis temperature, hydrolysis time in brilliant preparation process, realizes Cellulose nanocrystal and final carbon
The Modulatory character of nanometer rods size；Because substantial amounts of hydroxyl is contained on Cellulose nanocrystal surface, Pt nano-particle is received in cellulose
The load effect on the brilliant surface of rice is uniform, and load fastness is strong, and dimensionally stable has traditional carbon fibres, graphite in fuel cell field
Size advantage not available for alkene, CNT etc..
Embodiment 2
A kind of method of the derivative carbon nano rod supporting Pt nano-particle of Cellulose nanocrystal of the present embodiment, comprises the steps：
Paper scrap is placed in the hydrochloric acid solution that concentration is 5 mol/L and is configured as the suspension that cellulose solid content is 0.05 g/mL, will
Suspension is transferred at 120 DEG C of water heating kettle and is reacted, and after 1 h of reaction, by reactant liquor stratification, removes the supernatant, will
Remaining Cellulose nanocrystal suspension carries out titration neutralization with ammonia, and lyophilization after filtration is obtained Cellulose nanocrystal powder
End；Take the H that 50 mg Cellulose nanocrystals powder add the mol/L of 8 mL 0.012PtCl6In aqueous solution, 23 mL second are continuously added
Stir after the KOH solution of glycol and the mol/L of 6 mL 0.03.Reaction temperature is 125 DEG C, and the response time is 3 h, is reacted
Filtered with acetone cleaning after end, Pt carrying fibers element manocrystalline powders are obtained final product after being finally vacuum dried.Gained Pt loads is fine
The plain manocrystalline powders of dimension are placed directly within tube furnace at 350 DEG C of air atmosphere, carry out the h of high temperature oxidation process 1, then pass to protect
Shield property gas nitrogen, is progressively warming up to 1000 DEG C, prepares at high temperature after 3 h carbonizations and is loaded with Pt nano-particle
Carbon nano rod.
Jing field emission microscopy observations, the carbon nano rod average diameter for being loaded with Pt nano-particle manufactured in the present embodiment
For 10 nm, average length is 150 nm.
A kind of method of the derivative carbon nano rod supporting Pt nano-particle of Cellulose nanocrystal that the present embodiment is proposed, effectively
Biological material cellulose is make use of, with raw material sources are wide, renewable, free of contamination feature；By regulating and controlling cellulose nanometer
The factor such as raw material, acid concentration, hydrolysis temperature, hydrolysis time in brilliant preparation process, realizes Cellulose nanocrystal and final carbon
The Modulatory character of nanometer rods size；Because substantial amounts of hydroxyl is contained on Cellulose nanocrystal surface, Pt nano-particle is received in cellulose
The load effect on the brilliant surface of rice is uniform, and load fastness is strong, and dimensionally stable has traditional carbon fibres, graphite in fuel cell field
Size advantage not available for alkene, CNT etc..
Embodiment 3
A kind of method of the derivative carbon nano rod supporting Pt nano-particle of Cellulose nanocrystal of the present embodiment, comprises the steps：
Wood flour is placed in the hydrochloric acid solution that concentration is 5 mol/L and is configured as the suspension that cellulose solid content is 0.01 g/mL, will
Suspension is transferred at 110 DEG C of water heating kettle and is reacted, and after 3 h of reaction, by reactant liquor stratification, removes the supernatant, will
Remaining Cellulose nanocrystal suspension carries out titration neutralization with ammonia, and lyophilization after filtration is obtained Cellulose nanocrystal powder
End；Take the H that 52 mg Cellulose nanocrystals powder add the mol/L of 10 mL 0.0092PtCl6In aqueous solution, 25 mL are continuously added
Stir after the KOH solution of ethylene glycol and the mol/L of 5 mL 0.04.Reaction temperature is 130 DEG C, and the response time is 2 h, instead
Filtered with acetone cleaning after should terminating, Pt carrying fibers element manocrystalline powders are obtained final product after being finally vacuum dried.By gained Pt loads
Cellulose nanocrystal powder is placed directly within tube furnace at 250 DEG C of air atmosphere, carries out the h of high temperature oxidation process 2, is then passed to
Protective gas argon, is progressively warming up to 1200 DEG C, prepares at high temperature after 2 h carbonizations and is loaded with Pt nanometers
The carbon nano rod of grain.
Jing field emission microscopy observations, the carbon nano rod average diameter for being loaded with Pt nano-particle manufactured in the present embodiment
For 25 nm, average length is 210 nm.
A kind of method of the derivative carbon nano rod supporting Pt nano-particle of Cellulose nanocrystal that the present embodiment is proposed, effectively
Biological material cellulose is make use of, with raw material sources are wide, renewable, free of contamination feature；By regulating and controlling cellulose nanometer
The factor such as raw material, acid concentration, hydrolysis temperature, hydrolysis time in brilliant preparation process, realizes Cellulose nanocrystal and final carbon
The Modulatory character of nanometer rods size；Because substantial amounts of hydroxyl is contained on Cellulose nanocrystal surface, Pt nano-particle is received in cellulose
The load effect on the brilliant surface of rice is uniform, and load fastness is strong, and dimensionally stable has traditional carbon fibres, graphite in fuel cell field
Size advantage not available for alkene, CNT etc..
A kind of method of the derivative carbon nano rod supporting Pt nano-particle of Cellulose nanocrystal of the present embodiment of embodiment 4, bag
Include following steps：Cotton Gossypii is placed in the hydrochloric acid solution that concentration is 5 mol/L and is configured as cellulose solid content for 0.02 g/mL
Suspension, suspension is transferred at 115 DEG C of water heating kettle and is reacted, reaction 2 h after, reactant liquor stratification is removed
The supernatant, titration neutralization is carried out by remaining Cellulose nanocrystal suspension with ammonia, and lyophilization after filtration is obtained fiber
Plain manocrystalline powders；Take the H that 53 mg Cellulose nanocrystals powder add 11 mL 0.008mol/L2PtCl6In aqueous solution, continue
Stir after the KOH solution for adding 27 mL ethylene glycol and the mol/L of 4 mL 0.035.Reaction temperature is 129 DEG C, during reaction
Between be 2.5 h, reaction terminate after with acetone cleaning filter, finally be vacuum dried after obtain final product Pt carrying fibers element manocrystalline powders.
Gained Pt carrying fibers element manocrystalline powders are placed directly within tube furnace at 280 DEG C of air atmosphere, high temperature oxidation process is carried out
2.5 h, then pass to protective gas argon, are progressively warming up to 1400 DEG C, are prepared at high temperature after 1.6 h carbonizations
To the carbon nano rod for being loaded with Pt nano-particle.
Jing field emission microscopy observations, the carbon nano rod average diameter for being loaded with Pt nano-particle manufactured in the present embodiment
For 23 nm, average length is 310 nm.
A kind of method of the derivative carbon nano rod supporting Pt nano-particle of Cellulose nanocrystal that the present embodiment is proposed, effectively
Biological material cellulose is make use of, with raw material sources are wide, renewable, free of contamination feature；By regulating and controlling cellulose nanometer
The factor such as raw material, acid concentration, hydrolysis temperature, hydrolysis time in brilliant preparation process, realizes Cellulose nanocrystal and final carbon
The Modulatory character of nanometer rods size；Because substantial amounts of hydroxyl is contained on Cellulose nanocrystal surface, Pt nano-particle is received in cellulose
The load effect on the brilliant surface of rice is uniform, and load fastness is strong, and dimensionally stable has traditional carbon fibres, graphite in fuel cell field
Size advantage not available for alkene, CNT etc..
Embodiment 5
A kind of method of the derivative carbon nano rod supporting Pt nano-particle of Cellulose nanocrystal of the present embodiment, comprises the steps：
By Bacterial cellulose（The moral Food Co., Ltd of Hainan hundred million, food stage）It is placed in the hydrochloric acid solution that concentration is 5 mol/L and is configured to
For the suspension that cellulose solid content is 0.035 g/mL, suspension is transferred at 117 DEG C of water heating kettle and is reacted, reacted
After 2.5 h, by reactant liquor stratification, the supernatant is removed, remaining Cellulose nanocrystal suspension is dripped with ammonia
Fixed neutralization, lyophilization after filtration is obtained Cellulose nanocrystal powder；Take 54 mg Cellulose nanocrystals powder and add 9 mL
The H of 0.0085 mol/L2PtCl6In aqueous solution, the KOH solution of 24 mL ethylene glycol and the mol/L of 4.5 mL 0.045 is continuously added
After stir.Reaction temperature is 133 DEG C, and the response time is 2.5 h, and reaction is filtered after terminating with acetone cleaning, last vacuum
Pt carrying fibers element manocrystalline powders are obtained final product after drying.Gained Pt carrying fibers element manocrystalline powders are placed directly within tube furnace
At 240 DEG C of air atmosphere, the h of high temperature oxidation process 1.5 is carried out, then pass to protective gas argon, be progressively warming up to 1300
DEG C, the carbon nano rod for being loaded with Pt nano-particle is prepared at high temperature after 1.5 h carbonizations.
Jing field emission microscopy observations, the carbon nano rod for being loaded with Pt nano-particle manufactured in the present embodiment a diameter of 15
Nm, length is 240 nm.
A kind of method of the derivative carbon nano rod supporting Pt nano-particle of Cellulose nanocrystal that the present embodiment is proposed, effectively
Biological material cellulose is make use of, with raw material sources are wide, renewable, free of contamination feature；By regulating and controlling cellulose nanometer
The factor such as raw material, acid concentration, hydrolysis temperature, hydrolysis time in brilliant preparation process, realizes Cellulose nanocrystal and final carbon
The Modulatory character of nanometer rods size；Because substantial amounts of hydroxyl is contained on Cellulose nanocrystal surface, Pt nano-particle is received in cellulose
The load effect on the brilliant surface of rice is uniform, and load fastness is strong, and dimensionally stable has traditional carbon fibres, graphite in fuel cell field
Size advantage not available for alkene, CNT etc..
Claims (5)
1. a kind of method that Cellulose nanocrystal derives carbon nano rod supporting Pt nano-particle, it is characterised in that including following step
Suddenly：Using cellulosic raw material as primary substrate, cellulose is processed with acid catalyzed process, the nothing removed in cellulose is determined
Shape area and impurity component, extract Cellulose nanocrystal powder, then by reduction of ethylene glycol method to Pt raw material H2PtCl6Carry out also
It is former after eventually passing oxidation-charing process, to prepare a diameter of 10-30 nm to prepare Pt carrying fibers element manocrystalline powders, it is long
Spend for 150-350 nm, with the carbon nano rod supporting Pt material compared with big L/D ratio.
2. the method that a kind of Cellulose nanocrystal as claimed in claim 1 derives carbon nano rod supporting Pt nano-particle, it is special
Levy and be, the extracting method of described Cellulose nanocrystal powder is：Cellulose is placed in hydrochloric acid solution and is configured to cellulose
Suspension, suspension is transferred to into water heating kettle and is reacted, reaction terminate after, by reactant liquor stratification, remove upper strata clear
Liquid obtains Cellulose nanocrystal suspension, through neutralization, filters, freezes, being dried prepared Cellulose nanocrystal powder；It is wherein described
Concentration of hydrochloric acid solution be 5 mol/L；Solid content of the cellulose in hydrochloric acid is 0.005-0.05 g/mL；Suspension liquid is tied up to
Reaction temperature in water heating kettle is 100-120 DEG C, and the response time is 1-5h.
3. the method that a kind of Cellulose nanocrystal as claimed in claim 2 derives carbon nano rod supporting Pt nano-particle, it is special
Levy and be, described cellulosic raw material is using the one kind in cellulose crystallite, Cotton Gossypii, paper scrap, wood flour, Bacterial cellulose.
4. the method that a kind of Cellulose nanocrystal as claimed in claim 1 derives carbon nano rod supporting Pt nano-particle, it is special
Levy and be, described reduction of ethylene glycol method prepares the nanocrystalline method of Pt carrying fibers element and is：Take 50 ~ 55 mg cellulose nanometers
Crystalline flour end adds 8 ~ 12 mL H2PtCl6In aqueous solution, continuously add and stirred after 23 ~ 28 mL ethylene glycol and 3 ~ 6 mL KOH solutions
Uniformly；Reaction is filtered after terminating with acetone cleaning, and Pt carrying fibers element manocrystalline powders are obtained after being finally vacuum dried；Wherein institute
The H for stating2PtCl6Concentration of aqueous solution be 0.007 ~ 0.01 mol/L, KOH solution concentration be 0.03 ~ 0.05 mol/L, reaction temperature
For 125 ~ 134 DEG C, the h of response time 1.5 ~ 3.
5. the method that a kind of Cellulose nanocrystal as claimed in claim 1 derives carbon nano rod supporting Pt nano-particle, it is special
Levy and be, the method that described oxidation-nanocrystalline supporting Pt of carbon fiber element prepares carbon nano rod supporting Pt material is：To prepare
The Pt carrying fibers element manocrystalline powders for obtaining are placed directly within tube furnace under air atmosphere, carry out high temperature oxidation process, then
Protective gas is passed through, a diameter of 10-30 nm is prepared at high temperature, length is loaded with Pt nanometers for 150-350 nm
The carbon nano rod of granule, wherein temperature during described high temperature oxidation process is 200-350 DEG C, at 1-3 h high temperature
Reason；Using nitrogen or argon, described protective gas is warming up to described protective gas after being passed through using progressively temperature-raising method
1000-1500 DEG C, the high temperature carbonization time is 1-3h.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102040663A (en) * | 2010-12-06 | 2011-05-04 | 东华大学 | Preparation method of narrow-distribution cellulose nanocrystalline |
| CN104600332A (en) * | 2013-11-04 | 2015-05-06 | 中国石油化工股份有限公司 | Membraneless fuel cell catalyst slurry and methods for preparing catalyst slurry and electrode |
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2016
- 2016-11-18 CN CN201611016661.9A patent/CN106602079B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102040663A (en) * | 2010-12-06 | 2011-05-04 | 东华大学 | Preparation method of narrow-distribution cellulose nanocrystalline |
| CN104600332A (en) * | 2013-11-04 | 2015-05-06 | 中国石油化工股份有限公司 | Membraneless fuel cell catalyst slurry and methods for preparing catalyst slurry and electrode |
Non-Patent Citations (1)
| Title |
|---|
| YONG LIU 等: "Carbon nanorods derived from natural based nanocrystalline cellulose for highly efficient capacitive deionization", 《JOURNAL OF MATERIALS CHEMISTRY A》 * |
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