CN106602079B - A kind of preparation method of the derivative carbon nano rod supporting Pt nano particle of Cellulose nanocrystal - Google Patents
A kind of preparation method of the derivative carbon nano rod supporting Pt nano particle of Cellulose nanocrystal Download PDFInfo
- Publication number
- CN106602079B CN106602079B CN201611016661.9A CN201611016661A CN106602079B CN 106602079 B CN106602079 B CN 106602079B CN 201611016661 A CN201611016661 A CN 201611016661A CN 106602079 B CN106602079 B CN 106602079B
- Authority
- CN
- China
- Prior art keywords
- cellulose
- cellulose nanocrystal
- carbon nano
- raw material
- nano rod
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- 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
-
- 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
-
- 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
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses, as primary substrate, being handled with acid catalyzed process cellulose using cellulosic raw material, the amorphous region in cellulose and impurity component are removed, Cellulose nanocrystal powder is extracted, then by reduction of ethylene glycol method to Pt raw material H2PtCl6It is restored to prepare Pt carrying fiber element manocrystalline powders, finally after peroxidating-charing process, preparing diameter is 10-30 nm, and length is 150-350 nm, has the carbon nano rod supporting Pt material compared with big L/D ratio.The present invention is effectively utilized biological material cellulose, has the characteristics that raw material sources are wide, renewable, free of contamination；Carbon nano rod load is prepared through charing again after Cellulose nanocrystal and Pt payload, has load fastness strong, Pt nano particle good dispersion, the advantage of dimensionally stable.
Description
Technical field
This patent is related to a kind of preparation method of catalyst, especially a kind of derivative carbon nano rod load of Cellulose nanocrystal
The preparation method of Pt nano particle.
Background technique
With the consumption of the energy, demand of the whole world to the energy is further urgently changed.In order to solve the energy as topic, novel battery
The needs for being developed into a kind of development.Proton exchange membrane dye cell is that chemical energy is directly switched to electricity using hydrogen as fuel
A kind of electrochemical appliance of energy.As a kind of novel fuel cell, it has good portability, started quickly at low temperature, makes
Many advantages are extensively waited with range, thus are got more and more people's extensive concerning.Developing novel, efficient catalyst is proton exchange membrane dye
Expect one of the research emphasis of battery.Nano platinum particle is one of catalyst important in proton exchange membrane dye cell.
Selecting excellent support materials is the effective way for reducing platinum dosage and improving cell catalyst performance.Currently, research
In mostly use carbon black, carbon nano-fiber and carbon nanotube as the support materials of nano platinum particle greatly, these support materials are general
Have many characteristics, such as large specific surface area, good attack a vital point and mechanical property, stronger chemical stability.However, these carbon material tables
It is heavy that the chemical inertness in face becomes difficult surface payload nano platinum particle.Although can be in carbon nanometer using infusion process
Pipe surface supported platinum nano particle, but since platinum load capacity is less, limit the use of this method.In recent years, researcher adopts
Nano platinum particle is improved with many new technologies, new method in the load factor of carbon nano tube surface.Most common method is first will
Carbon nano tube surface carries out strong acid oxidation processes, its surface is made to generate the functionalization groups such as hydroxyl, aldehyde radical, carboxyl, uses
Different restoring method, nano platinum particle that can be controllable in the carbon nano tube surface deposition morphology of functionalization.Such as U.S. Xing
Et al. first using ultrasonic acidification carbon nanotube, directly deposit monodispersed platinum on the carbon nanotubes using ethylene glycol later 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.), add and takes
The Dodelet study group of big Montreal engineering college uses formic acid for reducing agent, directly in the carbon nanotube of carboxylic acid functional
Grow 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, carbon nanotube one-dimentional structure can be destroyed, and in it in chemical treating process
The physical properties such as optically and electrically can change.
In order to realize the payload of Pt nanoparticle on the carbon material, and the self structure and property of carbon material are not destroyed
Matter, Spain Correa-Duarte propose that non-covalent bond technology effectively can load various nanoparticles in carbon material surface, and
Do not destroy in carbon material structure and property (Grzelczak M, Correa-Duarte M,-Maceira
V,et al.Pt-Catalyzed Formation of Ni Nanoshells on Carbon Nanotubes[J]
.Angewandte Chemie International Edition,2007,46(37):7026-30.).Non-covalent modification technology
Nano platinum particle to load morphology controllable in carbon material surface indicates a new approach.Similar, the Chinese Academy of Sciences answers in Changchun
A cube Pt nanocrystal is directly loaded in by carbon nano tube surface using non-covalent modification technology with chemical Suo Yangxiurong group.
(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.) resulting compound redox reactions are shown it is good
Good catalytic effect, can be applied to the fields such as proton exchange membrane dye cell.Nevertheless, using carbon pipe as carrier, still
So there are carbon control for complex process, Pt nanoparticle payload rate is not high, electrostatic adsorption power is weak, load used
The problems such as easily-deformable in journey.
Summary of the invention
The object of the present invention is to provide a kind of systems of the derivative carbon nano rod supporting Pt nano particle of Cellulose nanocrystal
Preparation Method.The present invention is effectively utilized biological material cellulose, has the characteristics that raw material sources are wide, renewable, free of contamination；It is fine
Carbon nano rod load is prepared through charing again after the plain nanocrystalline and Pt payload of dimension, has load fastness strong, Pt nano particle
Good dispersion, the advantage of dimensionally stable.
In order to achieve the above objectives, the technical scheme is that
A kind of preparation method of the derivative carbon nano rod supporting Pt nano particle of Cellulose nanocrystal, includes the following steps: to adopt
It uses cellulosic raw material as primary substrate, cellulose is handled with acid catalyzed process, remove the amorphous region in cellulose
And impurity component, Cellulose nanocrystal powder is extracted, then by reduction of ethylene glycol method to Pt raw material H2PtCl6Restored with
Pt carrying fiber element manocrystalline powders are prepared, finally after peroxidating-charing process, preparing diameter is 10-30nm, and length is
150-350nm have the carbon nano rod supporting Pt material compared with big L/D ratio.
The extracting method of the Cellulose nanocrystal powder are as follows: cellulosic raw material is placed in hydrochloric acid solution and is configured to
Suspension is transferred to water heating kettle and reacted by the suspension of cellulose, and after reaction, reaction solution stratification is removed
Supernatant liquor obtains Cellulose nanocrystal suspension, by neutralization, filtering, freezing, dry obtained Cellulose nanocrystal powder；Its
Described in concentration of hydrochloric acid solution be 5mol/L；Solid content of the cellulosic raw material in hydrochloric acid is 0.005-0.05g/mL；It is outstanding
Reaction temperature of the supernatant liquid system in water heating kettle is 100-120 DEG C, and the reaction time is 1-5h.
The cellulosic raw material uses one of cellulose crystallite, cotton, paper scrap, sawdust, bacteria cellulose.
The reduction of ethylene glycol method prepares the nanocrystalline method of Pt carrying fiber element are as follows: takes 50~55mg cellulose nanometer
8~12mL H is added in crystalline flour end2PtCl6In aqueous solution, stirred after continuously adding 23~28mL ethylene glycol and 3~6mL KOH solution
Uniformly；It is cleaned and is filtered with acetone after reaction, Pt carrying fiber element manocrystalline powders are made after being finally dried in vacuo；Wherein institute
The H stated2PtCl6Concentration of aqueous solution is 0.007~0.01mol/L, and KOH solution concentration is 0.03~0.05mol/L, reaction temperature
It is 125~134 DEG C, 1.5~3h of reaction time.
The method that the oxidation-nanocrystalline supporting Pt of carbon fiber element prepares carbon nano rod supporting Pt material are as follows: will make
Standby obtained Pt carrying fiber element manocrystalline powders are placed directly in tube furnace under air atmosphere, carry out high temperature oxidation process, so
After be passed through protective gas, be prepared at high temperature diameter be 10-30nm, length be 150-350nm load have Pt nanometers
The carbon nano rod of particle, wherein temperature when the described high temperature oxidation process is 200-350 DEG C, by 1-3h high-temperature process；
The protective gas is warming up to after using nitrogen or argon gas, the protective gas to be passed through using gradually temperature-raising method
1000-1500 DEG C, the high temperature carbonization time is 1-3h.
The beneficial effects of the present invention are: the preparation side proposed by the invention for preparing carbon nano rod based on Cellulose nanocrystal
Method is effectively utilized biological material cellulose, has the characteristics that raw material sources are wide, renewable, free of contamination；By regulating and controlling fiber
The factors such as raw material, acid concentration, hydrolysis temperature, hydrolysis time in the nanocrystalline preparation process of element, realize Cellulose nanocrystal and
The Modulatory character of final carbon nano rod size；Since a large amount of hydroxyl is contained on Cellulose nanocrystal surface, Pt nano particle is in fibre
The load effect for tieing up plain nanocrystal surface is uniform, and load fastness is strong, dimensionally stable, the carbon nano rod prepared after oxidation-charing
Diameter is 10-30nm, and length is 150-350nm, has traditional carbon fibres, graphene, carbon nanotube in fuel cell field
Deng not available size advantage.
Specific embodiment
Embodiment 1
A kind of preparation method of the derivative carbon nano rod supporting Pt nano particle of the Cellulose nanocrystal of the present embodiment, including such as
Lower step: microcrystalline cellulose (product number 68005761, traditional Chinese medicines reagent) is placed in the hydrochloric acid solution that concentration is 5mol/L and is matched
It is made for the suspension that cellulose solid content is 0.005g/mL, suspension is transferred at 100 DEG C of water heating kettle and is reacted, instead
After answering 5h, by reaction solution stratification, supernatant liquor is removed, remaining Cellulose nanocrystal suspension is titrated with ammonium hydroxide
It neutralizes, is freeze-dried after filtering and Cellulose nanocrystal powder is made；Take 55mg Cellulose nanocrystal powder that 12mL is added
The H of 0.007mol/L2PtCl6In aqueous solution, stirred after continuously adding the KOH solution of 28mL ethylene glycol and 3mL 0.05mol/L
It is even.Reaction temperature is 134 DEG C, reaction time 1.5h, is cleaned filter with acetone after reaction, after being finally dried in vacuo to obtain the final product
Pt carrying fiber element manocrystalline powders.Then gained Pt carrying fiber element manocrystalline powders are placed directly within air gas in tube furnace
At 200 DEG C of atmosphere, high temperature oxidation process 3h is carried out, protective gas nitrogen is then passed to, is gradually warming up to 1500 DEG C, by 1h charcoal
The carbon nano rod that load has Pt nano particle is prepared after change at high temperature.
It is manufactured in the present embodiment to load the carbon nano rod average diameter for having Pt nano particle through field emission microscopy observation
For 30nm, average length 350nm.
A kind of preparation method of the derivative carbon nano rod supporting Pt nano particle of Cellulose nanocrystal that the present embodiment is proposed,
It is effectively utilized biological material cellulose, has the characteristics that raw material sources are wide, renewable, free of contamination；By regulating and controlling cellulose
The factors such as raw material, acid concentration, hydrolysis temperature, hydrolysis time in nanocrystalline preparation process realize Cellulose nanocrystal and most
The Modulatory character of whole carbon nano rod size；Since a large amount of hydroxyl is contained on Cellulose nanocrystal surface, Pt nano particle is in fiber
The load effect of plain nanocrystal surface is uniform, load fastness it is strong, dimensionally stable, fuel cell field have traditional carbon fibres,
Size advantage not available for graphene, carbon nanotube etc..
Embodiment 2
A kind of preparation method of the derivative carbon nano rod supporting Pt nano particle of the Cellulose nanocrystal of the present embodiment, including such as
Lower step: paper scrap, which is placed in, to prepare in the hydrochloric acid solution that concentration is 5mol/L becomes the suspension that cellulose solid content is 0.05g/mL
Suspension is transferred at 120 DEG C of water heating kettle and reacts by liquid, and after reacting 1h, by reaction solution stratification, it is clear to remove upper layer
Remaining Cellulose nanocrystal suspension is carried out titration neutralization with ammonium hydroxide by liquid, is freeze-dried after filtering and cellulose nanometer is made
Crystalline flour end；Take 50mg Cellulose nanocrystal powder that the H of 8mL 0.01mol/L is added2PtCl6In aqueous solution, 23mL second is continuously added
It is stirred evenly after the KOH solution of two pure and mild 6mL 0.03mol/L.Reaction temperature is 125 DEG C, and reaction time 3h, reaction terminates
It is cleaned and is filtered with acetone afterwards, up to Pt carrying fiber element manocrystalline powders after being finally dried in vacuo.By gained Pt carrying fiber element
Manocrystalline powders are placed directly in tube furnace at 350 DEG C of air atmosphere, are carried out high temperature oxidation process 1h, are then passed to protectiveness gas
Body nitrogen is gradually warming up to 1000 DEG C, and the carbon nanometer that load has Pt nano particle is prepared at high temperature after 3h is carbonized
Stick.
It is manufactured in the present embodiment to load the carbon nano rod average diameter for having Pt nano particle through field emission microscopy observation
For 10nm, average length 150nm.
A kind of preparation method of the derivative carbon nano rod supporting Pt nano particle of Cellulose nanocrystal that the present embodiment is proposed,
It is effectively utilized biological material cellulose, has the characteristics that raw material sources are wide, renewable, free of contamination；By regulating and controlling cellulose
The factors such as raw material, acid concentration, hydrolysis temperature, hydrolysis time in nanocrystalline preparation process realize Cellulose nanocrystal and most
The Modulatory character of whole carbon nano rod size；Since a large amount of hydroxyl is contained on Cellulose nanocrystal surface, Pt nano particle is in fiber
The load effect of plain nanocrystal surface is uniform, load fastness it is strong, dimensionally stable, fuel cell field have traditional carbon fibres,
Size advantage not available for graphene, carbon nanotube etc..
Embodiment 3
A kind of preparation method of the derivative carbon nano rod supporting Pt nano particle of the Cellulose nanocrystal of the present embodiment, including such as
Lower step: sawdust, which is placed in, to prepare in the hydrochloric acid solution that concentration is 5mol/L becomes the suspension that cellulose solid content is 0.01g/mL
Suspension is transferred at 110 DEG C of water heating kettle and reacts by liquid, and after reacting 3h, by reaction solution stratification, it is clear to remove upper layer
Remaining Cellulose nanocrystal suspension is carried out titration neutralization with ammonium hydroxide by liquid, is freeze-dried after filtering and cellulose nanometer is made
Crystalline flour end；Take 52mg Cellulose nanocrystal powder that the H of 10mL 0.009mol/L is added2PtCl6In aqueous solution, 25mL is continuously added
It is stirred evenly after the KOH solution of ethylene glycol and 5mL 0.04mol/L.Reaction temperature is 130 DEG C, reaction time 2h, reaction knot
It is cleaned and is filtered with acetone after beam, up to Pt carrying fiber element manocrystalline powders after being finally dried in vacuo.By gained Pt carrying fiber
Plain manocrystalline powders are placed directly in tube furnace at 250 DEG C of air atmosphere, are carried out high temperature oxidation process 2h, are then passed to protectiveness
Gases argon is gradually warming up to 1200 DEG C, and load is prepared at high temperature after 2h is carbonized has the carbon of Pt nano particle to receive
Rice stick.
It is manufactured in the present embodiment to load the carbon nano rod average diameter for having Pt nano particle through field emission microscopy observation
For 25nm, average length 210nm.
A kind of preparation method of the derivative carbon nano rod supporting Pt nano particle of Cellulose nanocrystal that the present embodiment is proposed,
It is effectively utilized biological material cellulose, has the characteristics that raw material sources are wide, renewable, free of contamination；By regulating and controlling cellulose
The factors such as raw material, acid concentration, hydrolysis temperature, hydrolysis time in nanocrystalline preparation process realize Cellulose nanocrystal and most
The Modulatory character of whole carbon nano rod size；Since a large amount of hydroxyl is contained on Cellulose nanocrystal surface, Pt nano particle is in fiber
The load effect of plain nanocrystal surface is uniform, load fastness it is strong, dimensionally stable, fuel cell field have traditional carbon fibres,
Size advantage not available for graphene, carbon nanotube etc..
A kind of preparation side of the derivative carbon nano rod supporting Pt nano particle of the Cellulose nanocrystal of 4 the present embodiment of embodiment
Method, include the following steps: for cotton to be placed in the hydrochloric acid solution that concentration is 5mol/L prepare become cellulose solid content be
Suspension is transferred at 115 DEG C of water heating kettle and reacts by the suspension of 0.02g/mL, after reacting 2h, reaction solution is stood and is divided
Layer, removes supernatant liquor, remaining Cellulose nanocrystal suspension is carried out titration neutralization with ammonium hydroxide, and system is freeze-dried after filtering
Obtain Cellulose nanocrystal powder；Take 53mg Cellulose nanocrystal powder that the H of 11mL 0.008mol/L is added2PtCl6In aqueous solution,
It is stirred evenly after continuously adding the KOH solution of 27mL ethylene glycol and 4mL 0.035mol/L.Reaction temperature is 129 DEG C, when reaction
Between be 2.5h, cleaned filter with acetone after reaction, up to Pt carrying fiber element manocrystalline powders after being finally dried in vacuo.It will
Gained Pt carrying fiber element manocrystalline powders are placed directly in tube furnace at 280 DEG C of air atmosphere, carry out high temperature oxidation process
2.5h, then passes to protective gas argon gas, is gradually warming up to 1400 DEG C, is prepared at high temperature after 1.6h is carbonized negative
It is loaded with the carbon nano rod of Pt nano particle.
It is manufactured in the present embodiment to load the carbon nano rod average diameter for having Pt nano particle through field emission microscopy observation
For 23nm, average length 310nm.
A kind of preparation method of the derivative carbon nano rod supporting Pt nano particle of Cellulose nanocrystal that the present embodiment is proposed,
It is effectively utilized biological material cellulose, has the characteristics that raw material sources are wide, renewable, free of contamination；By regulating and controlling cellulose
The factors such as raw material, acid concentration, hydrolysis temperature, hydrolysis time in nanocrystalline preparation process realize Cellulose nanocrystal and most
The Modulatory character of whole carbon nano rod size；Since a large amount of hydroxyl is contained on Cellulose nanocrystal surface, Pt nano particle is in fiber
The load effect of plain nanocrystal surface is uniform, load fastness it is strong, dimensionally stable, fuel cell field have traditional carbon fibres,
Size advantage not available for graphene, carbon nanotube etc..
Embodiment 5
A kind of preparation method of the derivative carbon nano rod supporting Pt nano particle of the Cellulose nanocrystal of the present embodiment, including such as
Lower step: bacteria cellulose (hundred million moral Food Co., Ltd of Hainan, food-grade) is placed in the hydrochloric acid solution that concentration is 5mol/L
The suspension for becoming that cellulose solid content is 0.035g/mL is prepared, suspension is transferred at 117 DEG C of water heating kettle and is reacted,
After reacting 2.5h, by reaction solution stratification, supernatant liquor is removed, remaining Cellulose nanocrystal suspension is carried out with ammonium hydroxide
Titration neutralizes, and is freeze-dried after filtering and Cellulose nanocrystal powder is made；54mg Cellulose nanocrystal powder is taken to be added
9mL0.0085mol/L H2PtCl6In aqueous solution, the KOH solution of 24mL ethylene glycol and 4.5mL 0.045mol/L is continuously added
After stir evenly.Reaction temperature is 133 DEG C, reaction time 2.5h, is cleaned filter with acetone after reaction, and last vacuum is dry
Up to Pt carrying fiber element manocrystalline powders after dry.It is hollow that gained Pt carrying fiber element manocrystalline powders are placed directly within tube furnace
At 240 DEG C of gas atmosphere, high temperature oxidation process 1.5h is carried out, protective gas argon gas is then passed to, is gradually warming up to 1300 DEG C, warp
The carbon nano rod that load has Pt nano particle is prepared at high temperature after crossing 1.5h charing.
Through field emission microscopy observation, the carbon nano rod diameter manufactured in the present embodiment that have Pt nano particle that loads is
15nm, length 240nm.
A kind of preparation method of the derivative carbon nano rod supporting Pt nano particle of Cellulose nanocrystal that the present embodiment is proposed,
It is effectively utilized biological material cellulose, has the characteristics that raw material sources are wide, renewable, free of contamination；By regulating and controlling cellulose
The factors such as raw material, acid concentration, hydrolysis temperature, hydrolysis time in nanocrystalline preparation process realize Cellulose nanocrystal and most
The Modulatory character of whole carbon nano rod size；Since a large amount of hydroxyl is contained on Cellulose nanocrystal surface, Pt nano particle is in fiber
The load effect of plain nanocrystal surface is uniform, load fastness it is strong, dimensionally stable, fuel cell field have traditional carbon fibres,
Size advantage not available for graphene, carbon nanotube etc..
Claims (3)
1. a kind of preparation method of the derivative carbon nano rod supporting Pt nano particle of Cellulose nanocrystal, which is characterized in that including such as
Lower step: using cellulosic raw material as primary substrate, being handled cellulose with acid catalyzed process, is removed in cellulose
Amorphous region and impurity component extract Cellulose nanocrystal powder, then by reduction of ethylene glycol method to Pt raw material H2PtCl6Into
Row reduction is to prepare Pt carrying fiber element manocrystalline powders, and finally after peroxidating-charing process, preparing diameter is 10-
30nm, length are 150-350nm, have the carbon nano rod supporting Pt material compared with big L/D ratio；The Cellulose nanocrystal powder
The extracting method at end are as follows: cellulosic raw material is placed in hydrochloric acid solution to the suspension for being configured to cellulose, suspension is shifted
It is reacted to water heating kettle, after reaction, by reaction solution stratification, removes supernatant liquor and obtain Cellulose nanocrystal suspension
Liquid, by neutralization, filtering, freezing, dry obtained Cellulose nanocrystal powder；Wherein the concentration of hydrochloric acid solution is 5mol/
L；Solid content of the cellulosic raw material in hydrochloric acid is 0.005-0.05g/mL；Suspension liquid ties up to the reaction temperature in water heating kettle
Degree is 100-120 DEG C, and the reaction time is 1-5h；The reduction of ethylene glycol method prepares the nanocrystalline method of Pt carrying fiber element
Are as follows: take 50~55mg Cellulose nanocrystal powder that 8~12mL H is added2PtCl6In aqueous solution, 23~28mL second two is continuously added
It is stirred evenly after pure and mild 3~6mL KOH solution；It is cleaned and is filtered with acetone after reaction, it is negative that Pt is made after being finally dried in vacuo
Carry Cellulose nanocrystal powder；The wherein H2PtCl6Concentration of aqueous solution is 0.007~0.01mol/L, and KOH solution concentration is
0.03~0.05mol/L, reaction temperature are 125~134 DEG C, 1.5~3h of reaction time.
2. a kind of preparation method of the derivative carbon nano rod supporting Pt nano particle of Cellulose nanocrystal as described in claim 1,
It is characterized in that, the cellulosic raw material is using one in cellulose crystallite, cotton, paper scrap, sawdust, bacteria cellulose
Kind.
3. a kind of preparation method of the derivative carbon nano rod supporting Pt nano particle of Cellulose nanocrystal as described in claim 1,
It is characterized in that, the method that the oxidation-nanocrystalline supporting Pt of carbon fiber element prepares carbon nano rod supporting Pt material are as follows: will
The Pt carrying fiber element manocrystalline powders being prepared are placed directly in tube furnace under air atmosphere, carry out high temperature oxidation process,
Protective gas is then passed to, it is 10-30nm that diameter is prepared at high temperature, and length is that 150-350nm load has Pt to receive
The carbon nano rod of rice grain, wherein temperature when the described high temperature oxidation process is 200-350 DEG C, at 1-3h high temperature
Reason；The protective gas is warming up to after using nitrogen or argon gas, the protective gas to be passed through using gradually temperature-raising method
1000-1500 DEG C, the high temperature carbonization time is 1-3h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611016661.9A CN106602079B (en) | 2016-11-18 | 2016-11-18 | A kind of preparation method of the derivative carbon nano rod supporting Pt nano particle of Cellulose nanocrystal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611016661.9A CN106602079B (en) | 2016-11-18 | 2016-11-18 | A kind of preparation method of the derivative carbon nano rod supporting Pt nano particle of Cellulose nanocrystal |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106602079A CN106602079A (en) | 2017-04-26 |
| CN106602079B true CN106602079B (en) | 2019-06-28 |
Family
ID=58592221
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611016661.9A Active CN106602079B (en) | 2016-11-18 | 2016-11-18 | A kind of preparation method of the derivative carbon nano rod supporting Pt nano particle of Cellulose nanocrystal |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106602079B (en) |
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 |
-
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 |
|---|
| Carbon nanorods derived from natural based nanocrystalline cellulose for highly efficient capacitive deionization;Yong Liu 等;《Journal of Materials Chemistry A》;20141028;第2卷;第20966-20972页 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106602079A (en) | 2017-04-26 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104941674B (en) | Catalyst of phosphatization cobalt and its preparation method and application is loaded on a kind of activated carbon | |
| Jiang et al. | Recent advances in carbon-based electrocatalysts for vanadium redox flow battery: Mechanisms, properties, and perspectives | |
| CN104009242B (en) | The porous carbon network structure material preparation method of the N doping of a kind of fuel battery cathod catalyst metal/metal oxide load | |
| CN107099880B (en) | Cobalt nickel oxide/tin dioxide composite nanotube and preparation method and application thereof | |
| Liang et al. | Enhanced dye photocatalysis and recycling abilities of semi-wrapped TiO2@ carbon nanofibers formed via foaming agent driving | |
| CN112844476B (en) | Biomass-based carbon material loaded nano nickel catalyst and preparation method and application thereof | |
| CN112265981B (en) | Method for preparing carbon nano tube by lignin nano micelle | |
| CN106298269B (en) | Cobalt sulfide nickel/nitrogen-doped carbon nano-fiber composite material, preparation method and application | |
| CN112345611A (en) | Preparation method of electrochemical sensor based on loofah sponge biomass charcoal composite material and preparation method of composite material | |
| CN108940285A (en) | A kind of preparation method and application of flexibility electrolysis water catalysis material | |
| CN109704307A (en) | A kind of preparation and its application of the sulfur doping porous carbon based on sterculia seed slag | |
| CN109046423B (en) | Three-dimensional grading composite material and preparation method and application thereof | |
| Wang et al. | Biomass derived the V-doped carbon/Bi2O3 composite for efficient photocatalysts | |
| CN108847492A (en) | A kind of N doping metals cobalt carbon nano-fiber composite material and its preparation method and application | |
| CN110732338B (en) | Carbon nanowire/g-C 3 N 4 Composite visible light catalyst and preparation method thereof | |
| Gao et al. | 3D heterogeneous CTF@ TiO 2/Bi 2 WO 6/Au hybrid supported by hollow carbon tubes and its efficient photocatalytic performance in the UV-vis range | |
| CN102600667B (en) | Air filter material based on carbon nano tube and preparation method thereof | |
| Gopiraman et al. | Preparation, characterization, and applications of electrospun carbon Nanofibers and its composites | |
| Ma et al. | Lignin-derived hierarchical porous flower-like carbon nanosheets decorated with biomass carbon quantum dots for efficient oxygen reduction | |
| CN111285368B (en) | Preparation method of nitrogen-boron double-doped porous hollow carbon nano-capsule material | |
| Zhai et al. | Biomass-derived carbon materials for vanadium redox flow battery: from structure to property | |
| CN112736234B (en) | Novel lithium ion battery anode material based on biomass/carbon nanotube composite modified lithium titanate and application thereof | |
| CN106587006A (en) | Method for preparing carbon nano bar based on cellulose nanocrystals | |
| CN106602079B (en) | A kind of preparation method of the derivative carbon nano rod supporting Pt nano particle of Cellulose nanocrystal | |
| TWI323747B (en) | Method and apparatus for surface modification of film component by carbon dioxide supercritical fluid |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |