CN109092297A - Carbon quantum dot load type palladium nanocomposite and its preparation method and application - Google Patents
Carbon quantum dot load type palladium nanocomposite and its preparation method and application Download PDFInfo
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- CN109092297A CN109092297A CN201811071985.1A CN201811071985A CN109092297A CN 109092297 A CN109092297 A CN 109092297A CN 201811071985 A CN201811071985 A CN 201811071985A CN 109092297 A CN109092297 A CN 109092297A
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- palladium
- quantum dot
- carbon quantum
- load type
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- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 title claims abstract description 102
- 229910052763 palladium Inorganic materials 0.000 title claims abstract description 47
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 27
- 229920001661 Chitosan Polymers 0.000 claims abstract description 14
- 239000007864 aqueous solution Substances 0.000 claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 230000003647 oxidation Effects 0.000 claims abstract description 7
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 7
- 239000000243 solution Substances 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000012696 Pd precursors Substances 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims abstract description 3
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 claims description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- YJVFFLUZDVXJQI-UHFFFAOYSA-L palladium(ii) acetate Chemical compound [Pd+2].CC([O-])=O.CC([O-])=O YJVFFLUZDVXJQI-UHFFFAOYSA-L 0.000 claims description 2
- GPNDARIEYHPYAY-UHFFFAOYSA-N palladium(ii) nitrate Chemical compound [Pd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O GPNDARIEYHPYAY-UHFFFAOYSA-N 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000002105 nanoparticle Substances 0.000 abstract description 5
- 239000002086 nanomaterial Substances 0.000 abstract description 4
- 239000002131 composite material Substances 0.000 abstract description 3
- 150000001875 compounds Chemical class 0.000 abstract description 3
- 230000003197 catalytic effect Effects 0.000 abstract description 2
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 10
- 239000003054 catalyst Substances 0.000 description 9
- 230000015572 biosynthetic process Effects 0.000 description 5
- UKVIEHSSVKSQBA-UHFFFAOYSA-N methane;palladium Chemical compound C.[Pd] UKVIEHSSVKSQBA-UHFFFAOYSA-N 0.000 description 5
- 238000003786 synthesis reaction Methods 0.000 description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- 238000002484 cyclic voltammetry Methods 0.000 description 3
- 239000003610 charcoal Substances 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 239000011943 nanocatalyst Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- 235000013162 Cocos nucifera Nutrition 0.000 description 1
- 244000060011 Cocos nucifera Species 0.000 description 1
- 241000143432 Daldinia concentrica Species 0.000 description 1
- 229910002666 PdCl2 Inorganic materials 0.000 description 1
- 229910021607 Silver chloride Inorganic materials 0.000 description 1
- 238000006161 Suzuki-Miyaura coupling reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000001548 drop coating Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 229910021397 glassy carbon Inorganic materials 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000010903 husk Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910021392 nanocarbon Inorganic materials 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- SDLBJIZEEMKQKY-UHFFFAOYSA-M silver chlorate Chemical compound [Ag+].[O-]Cl(=O)=O SDLBJIZEEMKQKY-UHFFFAOYSA-M 0.000 description 1
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
- B01J23/44—Palladium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/33—Electric or magnetic properties
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
- C25B11/091—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B3/00—Electrolytic production of organic compounds
- C25B3/20—Processes
- C25B3/23—Oxidation
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Electrochemistry (AREA)
- Metallurgy (AREA)
- Catalysts (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a kind of carbon quantum dot load type palladium nanocomposites and its preparation method and application.The preparation step of the composite material: the palladium precursor water solution of compound concentration 0.02-0.5mg/mL and the chitosan aqueous solution of concentration 2-5mg/mL, palladium presoma and chitosan 1:100-1:10 in mass ratio are added in reaction kettle, are reacted 0.5-10 hours under the conditions of 100-200 DEG C.The present invention uses one-step hydrothermal synthesis of carbon quantum dot load type palladium nanocomposite, and method is simple, and condition is controllable, is easy quantitatively to control the content and distribution of palladium in nano material.And prepared nano material, palladium nano-particles are uniform, performance is stable, have electro catalytic activity, can be applied in anodic oxidation of methanol reaction.
Description
Technical field
The present invention relates to nanocomposite technical fields, and in particular to a kind of nano combined material of carbon quantum dot load type palladium
The high efficiency preparation method of material.
Technical background
Palladium-carbon catalyst is that Metal Palladium is loaded to in carbon material a kind of catalyst for forming support type, being widely used in
Industrial and commercial bank's industry.The carrier some of supported palladium may be coconut husk, and some may be coal quality charcoal, also have plenty of staple fibre charcoal, more having can
It can be a nanometer carbon carrier.The palladium on surface is the real activated centre of catalyst, but carrier also plays very big effect, and palladium can be more
Big being utilized for degree must see whether the carrier of palladium carbon may advantageously facilitate reactant and contact well with activated centre, therefore,
The type of carrier carbon, influence of the physico-chemical property to palladium-carbon catalyst are extremely important；And in terms of the service performance of palladium charcoal, palladium and load
Interaction force between body determines the load fastness of catalyst, durability and the rate of recovery.Used palladium currently on the market
In C catalyst, the mode of loading of palladium on the carbon carrier is mainly physical attachment, and the loss of palladium is larger ([1] in use
Lv Meiying, Dong Guang, Chen Huirong wait the preparation of palladium/Nano carbon balls composite material and the Shandong electrocatalytic oxidation [J] the work to formic acid
Industry college journal, 2016,30 (6): 12-16；[2]García-Suárez E J,Lara P,García A B,et
al.Efficient and recyclable carbon-supported Pd nanocatalysts for the Suzuki–
Miyaura reaction in aqueous-based media:Microwave vs conventional heating[J]
.Applied Catalysis A General,2013,468(13):59-67；[3] Jiao Jianli, Huanglong river, Teng great Wei are inorganic
Progress [J] chemistry and bioengineering of object load type palladium catalyst, 2010,27 (3): 4-8.).
Summary of the invention
The purpose of the present invention is current palladium-carbon catalyst there are aiming at the problem that, a kind of carbon quantum dot load type palladium is provided and is received
Nano composite material and its preparation method and application.
A kind of preparation method of carbon quantum dot load type palladium nanocomposite provided by the invention, includes the following steps:
The palladium precursor water solution of compound concentration 0.02-0.5mg/mL and the chitosan aqueous solution of concentration 2-5mg/mL, palladium presoma and
Chitosan 1:100-1:10 in mass ratio is added in reaction kettle, is reacted 0.5-10 hours under the conditions of 100-200 DEG C and is obtained carbon
Quantum dot load type palladium nanocomposite.
The chitosan has low viscosity, medium viscosity and high viscosity, the preferred low viscosity chitosan of the present invention.
The palladium presoma is palladium nitrate, palladium acetate or palladium chloride, preferably cheap palladium chloride.
The reaction temperature is preferably 180 DEG C.
The reaction time is preferably 3 hours.
Carbon quantum dot load type palladium nanocomposite made above has electro catalytic activity, can be applied to methanol electricity and urges
In oxidation.
Beneficial effects of the present invention compared with prior art: the present invention uses one-step hydrothermal synthesis of carbon quantum dot support type
Palladium nanocomposite, method is simple, and condition is controllable, is easy quantitatively to control the content and distribution of palladium in nano material.Moreover,
In prepared nano material, palladium nano-particles are uniform, performance is stable, are a kind of excellent palladium carbon nano-composite catalyst materials
Material can be used in anodic oxidation of methanol reaction.
Detailed description of the invention
Fig. 1 is the transmission electron microscope picture of the carbon quantum dot without palladium chloride aqueous solution
Fig. 2 is that the carbon quantum dot of embodiment 1 loads the transmission electron microscope picture of nanometer Pd material
Fig. 3 is that the carbon quantum dot of embodiment 1 loads the EDX characterization of nanometer Pd material
Fig. 4 is electrocatalytic oxidation cyclic voltammogram of the carbon quantum dot supported palladium nanocatalyst to methanol of embodiment 1
Specific embodiment
The present invention will be further described with attached drawing combined with specific embodiments below, and following embodiment is intended to illustrate invention
Rather than limitation of the invention further.
Embodiment 1
By 10mL concentration be 2mg/mL chitosan aqueous solution and 10mL concentration be 0.2mg/mL palladium chloride aqueous solution, add
Enter into reaction kettle, 3 hours, i.e. synthesis carbon quantum dot load type palladium nanocomposite are reacted under the conditions of 180 DEG C.
Fig. 2 is that carbon quantum dot loads nanometer Pd material transmission electron microscope picture, and carbon quantum dot has lesser ruler as seen from the figure
It is very little, carbon quantum dot and PdCl2After reaction, the dispersibility of carbon dots load Pd nano particle is reduced compared with carbon quantum dot, and size is also sent out
Significant change is given birth to.Fig. 3 is that carbon quantum dot loads nanometer Pd material EDX phenogram, as can be seen from the figure contains C element and Pd
Element illustrates that we have synthesized the composite material of carbon quantum dot supported palladium.
Embodiment 2
By 25mL concentration be 3mg/mL chitosan aqueous solution and 3mL concentration be 0.5mg/mL palladium chloride aqueous solution, add
Enter into reaction kettle, 6 hours, i.e. synthesis carbon quantum dot load type palladium nanocomposite are reacted under the conditions of 180 DEG C.
Embodiment 3
By 10mL concentration be 2mg/mL chitosan aqueous solution and 10mL concentration be 0.2mg/mL palladium chloride aqueous solution, add
Enter into reaction kettle, 3 hours, i.e. synthesis carbon quantum dot load type palladium nanocomposite are reacted under the conditions of 200 DEG C.
Embodiment 4
By the chitosan aqueous solution that 10mL concentration is 4mg/mL and the palladium chloride aqueous solution that 5mL concentration is 0.4mg/mL, add
Enter into reaction kettle, 3 hours, i.e. synthesis carbon quantum dot load type palladium nanocomposite are reacted under the conditions of 180 DEG C.
Embodiment 5
By the chitosan aqueous solution that 10mL concentration is 4mg/mL and the palladium chloride aqueous solution that 5mL concentration is 0.4mg/mL, add
Enter into reaction kettle, 8 hours, i.e. synthesis carbon quantum dot load type palladium nanocomposite are reacted under the conditions of 150 DEG C.
Embodiment 6
Carbon quantum dot load type palladium nanocomposite applications prepared by embodiment 1 are reacted in anodic oxidation of methanol
In.0.1mg compound material ultrasound 1 minute is scattered in 10mL deionized water, by 10 microlitres of drop coatings of the solution in 3mm diameter
Glassy carbon electrode surface, it is 30 minutes dry at 60 DEG C, obtain carbon quantum dot load type palladium Nanoparticle Modified Electrode.Modified electrode is adopted
It is that methanol solution detects to concentration in 5mL 1.0M NaOH electrolyte solution with cyclic voltammetry, platinum electrode is pair
Electrode, silver/silver chlorate (Ag/AgCl) electrode are reference electrode, and carbon quantum dot load type palladium Nanoparticle Modified Electrode is working electrode.
Electrochemical operation potential range is-0.8-0.4V, and cyclic voltammetry scan rate is 0.02v/s, the body containing methanol in electrolyte
Product is 0 (see a curve in Fig. 4) or the volume containing methanol is 20 microlitres of electrochemistry cyclic voltammetrics obtained (see b curve in Fig. 4)
Curve.
Claims (7)
1. a kind of preparation method of carbon quantum dot load type palladium nanocomposite, it is characterised in that include the following steps: to prepare
The palladium precursor water solution of concentration 0.02-0.5mg/mL and the chitosan aqueous solution of concentration 2-5mg/mL, palladium presoma and shell are poly-
Sugar 1:100-1:10 in mass ratio is added in reaction kettle, is reacted 0.5-10 hours under the conditions of 100-200 DEG C and is obtained carbon quantum
Point load type palladium nanocomposite.
2. a kind of preparation method of carbon quantum dot load type palladium nanocomposite as described in claim 1, it is characterised in that
The chitosan is low viscosity chitosan.
3. a kind of preparation method of carbon quantum dot load type palladium nanocomposite as described in claim 1, it is characterised in that
The palladium presoma is palladium nitrate, palladium acetate or palladium chloride.
4. a kind of preparation method of carbon quantum dot load type palladium nanocomposite as described in claim 1, it is characterised in that
The reaction temperature is 180 DEG C.
5. a kind of preparation method of carbon quantum dot load type palladium nanocomposite as described in claim 1, it is characterised in that
The reaction time is 3 hours.
6. such as the carbon quantum dot load type palladium nanocomposite of claim 1-5 the method preparation.
7. carbon quantum dot load type palladium nanocomposite as claimed in claim 6 answering in anodic oxidation of methanol reaction
With.
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| CN201811071985.1A CN109092297A (en) | 2018-09-14 | 2018-09-14 | Carbon quantum dot load type palladium nanocomposite and its preparation method and application |
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|---|---|---|---|
| CN201811071985.1A CN109092297A (en) | 2018-09-14 | 2018-09-14 | Carbon quantum dot load type palladium nanocomposite and its preparation method and application |
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| CN109092297A true CN109092297A (en) | 2018-12-28 |
Family
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| CN201811071985.1A Pending CN109092297A (en) | 2018-09-14 | 2018-09-14 | Carbon quantum dot load type palladium nanocomposite and its preparation method and application |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110261465A (en) * | 2019-06-14 | 2019-09-20 | 上海大学 | A kind of method of one-step synthesis method carried noble metal solid carbon quantum dot sensor |
| CN115025773A (en) * | 2022-07-19 | 2022-09-09 | 湖南师范大学 | Method for preparing carbon/palladium composite material for efficiently degrading p-nitrophenol by using carbon dots as reducing agent |
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2018
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110261465A (en) * | 2019-06-14 | 2019-09-20 | 上海大学 | A kind of method of one-step synthesis method carried noble metal solid carbon quantum dot sensor |
| CN115025773A (en) * | 2022-07-19 | 2022-09-09 | 湖南师范大学 | Method for preparing carbon/palladium composite material for efficiently degrading p-nitrophenol by using carbon dots as reducing agent |
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