CN106334801A - Method for preparing porous carbon loaded nano-metal through microwave assistance - Google Patents
Method for preparing porous carbon loaded nano-metal through microwave assistance Download PDFInfo
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- CN106334801A CN106334801A CN201610811205.7A CN201610811205A CN106334801A CN 106334801 A CN106334801 A CN 106334801A CN 201610811205 A CN201610811205 A CN 201610811205A CN 106334801 A CN106334801 A CN 106334801A
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- 229910052751 metal Inorganic materials 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 42
- 239000002184 metal Substances 0.000 title claims abstract description 34
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title abstract description 24
- 229910052799 carbon Inorganic materials 0.000 title abstract description 24
- 238000010438 heat treatment Methods 0.000 claims abstract description 30
- 150000001720 carbohydrates Chemical class 0.000 claims abstract description 16
- 239000007769 metal material Substances 0.000 claims abstract description 10
- 238000003763 carbonization Methods 0.000 claims abstract description 6
- 230000018044 dehydration Effects 0.000 claims abstract description 4
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 4
- 150000003839 salts Chemical class 0.000 claims abstract description 4
- 239000003610 charcoal Substances 0.000 claims description 51
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 40
- 229910052737 gold Inorganic materials 0.000 claims description 26
- 239000010931 gold Substances 0.000 claims description 26
- 239000000463 material Substances 0.000 claims description 26
- 239000004202 carbamide Substances 0.000 claims description 20
- 235000013877 carbamide Nutrition 0.000 claims description 20
- 239000007787 solid Substances 0.000 claims description 16
- 238000002360 preparation method Methods 0.000 claims description 12
- 229910044991 metal oxide Inorganic materials 0.000 claims description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- 150000004706 metal oxides Chemical class 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 6
- GUBGYTABKSRVRQ-QKKXKWKRSA-N Lactose Natural products OC[C@H]1O[C@@H](O[C@H]2[C@H](O)[C@@H](O)C(O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@H]1O GUBGYTABKSRVRQ-QKKXKWKRSA-N 0.000 claims description 6
- 239000008103 glucose Substances 0.000 claims description 6
- 239000008101 lactose Substances 0.000 claims description 6
- 239000012298 atmosphere Substances 0.000 claims description 5
- GUBGYTABKSRVRQ-XLOQQCSPSA-N Alpha-Lactose Chemical compound O[C@@H]1[C@@H](O)[C@@H](O)[C@@H](CO)O[C@H]1O[C@@H]1[C@@H](CO)O[C@H](O)[C@H](O)[C@H]1O GUBGYTABKSRVRQ-XLOQQCSPSA-N 0.000 claims description 4
- 229930091371 Fructose Natural products 0.000 claims description 4
- 239000005715 Fructose Substances 0.000 claims description 4
- RFSUNEUAIZKAJO-ARQDHWQXSA-N Fructose Chemical compound OC[C@H]1O[C@](O)(CO)[C@@H](O)[C@@H]1O RFSUNEUAIZKAJO-ARQDHWQXSA-N 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 4
- WQYVRQLZKVEZGA-UHFFFAOYSA-N hypochlorite Chemical compound Cl[O-] WQYVRQLZKVEZGA-UHFFFAOYSA-N 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 239000002905 metal composite material Substances 0.000 claims description 3
- OWEGMIWEEQEYGQ-UHFFFAOYSA-N 100676-05-9 Natural products OC1C(O)C(O)C(CO)OC1OCC1C(O)C(O)C(O)C(OC2C(OC(O)C(O)C2O)CO)O1 OWEGMIWEEQEYGQ-UHFFFAOYSA-N 0.000 claims description 2
- 229910000952 Be alloy Inorganic materials 0.000 claims description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 2
- 239000004375 Dextrin Substances 0.000 claims description 2
- 229920001353 Dextrin Polymers 0.000 claims description 2
- GUBGYTABKSRVRQ-PICCSMPSSA-N Maltose Natural products O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@@H]1O[C@@H]1[C@@H](CO)OC(O)[C@H](O)[C@H]1O GUBGYTABKSRVRQ-PICCSMPSSA-N 0.000 claims description 2
- 229910019142 PO4 Inorganic materials 0.000 claims description 2
- 229920002472 Starch Polymers 0.000 claims description 2
- 229930006000 Sucrose Natural products 0.000 claims description 2
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 2
- 239000000956 alloy Substances 0.000 claims description 2
- GUBGYTABKSRVRQ-QUYVBRFLSA-N beta-maltose Chemical compound OC[C@H]1O[C@H](O[C@H]2[C@H](O)[C@@H](O)[C@H](O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@@H]1O GUBGYTABKSRVRQ-QUYVBRFLSA-N 0.000 claims description 2
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 2
- 235000019425 dextrin Nutrition 0.000 claims description 2
- 239000008246 gaseous mixture Substances 0.000 claims description 2
- 239000001307 helium Substances 0.000 claims description 2
- 229910052734 helium Inorganic materials 0.000 claims description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 229910000765 intermetallic Inorganic materials 0.000 claims description 2
- 239000000155 melt Substances 0.000 claims description 2
- 229910001960 metal nitrate Inorganic materials 0.000 claims description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 2
- 150000003891 oxalate salts Chemical class 0.000 claims description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 2
- 239000010452 phosphate Substances 0.000 claims description 2
- 230000001681 protective effect Effects 0.000 claims description 2
- 239000008107 starch Substances 0.000 claims description 2
- 235000019698 starch Nutrition 0.000 claims description 2
- 239000005720 sucrose Substances 0.000 claims description 2
- 229910052715 tantalum Inorganic materials 0.000 claims description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims 1
- 125000002791 glucosyl group Chemical group C1([C@H](O)[C@@H](O)[C@H](O)[C@H](O1)CO)* 0.000 claims 1
- 229910052741 iridium Inorganic materials 0.000 claims 1
- 229920000609 methyl cellulose Polymers 0.000 claims 1
- 239000001923 methylcellulose Substances 0.000 claims 1
- 229910052702 rhenium Inorganic materials 0.000 claims 1
- 239000000126 substance Substances 0.000 claims 1
- 230000015572 biosynthetic process Effects 0.000 abstract description 16
- 238000003786 synthesis reaction Methods 0.000 abstract description 15
- 239000002086 nanomaterial Substances 0.000 abstract description 12
- 239000002245 particle Substances 0.000 abstract description 9
- 239000013078 crystal Substances 0.000 abstract description 6
- 238000011068 loading method Methods 0.000 abstract description 5
- 239000000203 mixture Substances 0.000 abstract description 5
- 238000006555 catalytic reaction Methods 0.000 abstract description 4
- 230000005518 electrochemistry Effects 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 3
- 238000011065 in-situ storage Methods 0.000 abstract description 2
- 235000014633 carbohydrates Nutrition 0.000 abstract 1
- 239000011259 mixed solution Substances 0.000 abstract 1
- 238000003760 magnetic stirring Methods 0.000 description 11
- 235000001727 glucose Nutrition 0.000 description 9
- 239000007788 liquid Substances 0.000 description 8
- 239000003814 drug Substances 0.000 description 7
- 239000004570 mortar (masonry) Substances 0.000 description 6
- 239000002105 nanoparticle Substances 0.000 description 6
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 5
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- 150000002304 glucoses Chemical class 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 239000011148 porous material Substances 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 238000007334 copolymerization reaction Methods 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 230000002194 synthesizing effect Effects 0.000 description 3
- 238000010189 synthetic method Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 2
- 238000007598 dipping method Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000010408 film Substances 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 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 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 239000012266 salt solution Substances 0.000 description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 229910002676 Pd(NO3)2·2H2O Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000012876 carrier material Substances 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 238000001802 infusion Methods 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000007144 microwave assisted synthesis reaction Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000005610 quantum mechanics Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
- B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/06—Ferric oxide [Fe2O3]
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Crystallography & Structural Chemistry (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Composite Materials (AREA)
- Materials Engineering (AREA)
- Carbon And Carbon Compounds (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a method for preparing porous carbon loaded nano-metal through microwave assistance and belongs to the technical field of nano material preparing. The method comprises the steps that porous carbon is formed through microwave heating, dehydration and carbonization in situ by utilizing the characteristic that ureal derivatives, carbohydrates and metal salt can form a uniform mixed solution at a certain temperature, and then the porous carbon is subjected to high-temperature heat treatment, so that the porous carbon loaded nano-metal material is prepared. According to the method, the loading type nano material which is controllable over loading amount, particle size, crystal phase and composition at the same time by changing the proportion of raw materials, the microwave duration, the power and other synthesis conditions. The whole process has the advantages of being easy to operate, environmentally friendly, low in cost and the like. The obtained porous carbon loaded nano-metal material has wide application prospects in industrial catalysis, water treatment, electrochemistry and other many aspects.
Description
Technical field
The invention provides a kind of method that porous charcoal supported nano-gold belongs to oxide or nano metal material, belong to nanometer
Technical field of material.
Background technology
Nano material refers to be made up of superfine crystal grain, characteristic dimension size nanometer scale (~ 100nm) solid material
Material.Nano material has the performance not available for many conventional materials, including optical property, electromagnetic property, thermodynamic property,
Quantum mechanics performance etc., due to these performances, nano material is widely used in the fields such as lubrication, photoelectricity, magnetic recording, catalysis.So
And, due to its high surface energy, the easily spontaneous reunion of nano-particle, greatly limit the nano effect of nano material, reduce it
Application and effect.Therefore nano material generally requires carrier, and porous material is a kind of by the cavity being mutually communicated or close
Constitute the material of network structure, porous charcoal is ideal catalyst carrier, can hinder the reunion of loaded granule, provide
The transfer passage of reaction solution, promotes the diffusion generating material again, and big specific surface area contributes to catalyst and reactant
Contact, is one of indispensable important materials in modern industry.The preparation of porous charcoal is generally by hard template method and soft mode
The synthesis of plate method is it is considered to be synthesizing porous charcoal most successful and most efficient method.The nano metal of porous charcoal load or oxide
Material all has broad application prospects in all many-sides such as Industrial Catalysis, water process and electrochemistry.
In terms of porous charcoal supports the preparation method of nano material, commonly used is direct dipping process and copolymerization process.
Direct dipping process is by porous carbon materials direct impregnation in metal salt solution, and then drying is born with being thermally treated resulting in porous charcoal
The nano material carrying.Ryoo etc. [joo s h, choi s j, oh i, et al. (2001). nature 412
(6843): 169-172.] by impregnating method of reducing, Pt nanoparticle is incorporated in ordered mesoporous carbon, obtains high degree of dispersion
Particle diameter be only 3 nm platinum grain so as to be expected to there is application prospect in fuel cell field.Infusion process is widely used, but right
Lack effectively to regulate and control in the particle diameter of nanoparticle, component and distribution in the carrier.Copolymerization process refers to slaine and carbon
Source is filled in foraminous die plate, by carbonization and removing template thus obtaining porous carbon composite material.[ding j, the chan such as ding
K y, ren j, et al. (2005) .electrochimica acta 50 (15): 3131-3141.] with sba-15 as mould
Plate, methanol are carbon source, pt (nh3)4(no3)2For slaine, prepare ordered mesoporous carbon/platinum composite, and have studied
Its electrocatalysis characteristic to oxygen reduction reaction.However, the preparation method complexity of copolymerization process is loaded down with trivial details, need repeatedly to irrigate carbon source
With slaine and remove removing template, cycle length, high cost, this undoubtedly hinders the scale application of the method.
Microwave process for synthesizing is to utilize high frequency microwave energy, produces substantial amounts of heat within a very short time, thus promoting all kinds of chemistry
The carrying out of reaction, is more effective energy utilization and mode of heating.The fortune of reaction molecular can be significantly accelerated in microwave heating synthesis
Move and impact velocity, be conducive to a large amount of formation of nucleus, the increase of crystal particle diameter can be limited, ratio conventional method institute can be synthesized
The particle diameter preparing crystal is less, nano material evenly.At present, microwave-assisted synthesis are widely used to the system of nano material
Standby..Peiro etc. prepares tio in two steps2Thin film: the first step, immerse the substrate in the tio through microwave radiation2In colloid solution, find
Tio crystal deposition is had on substrate；Second step, the substrate immersion of above-mentioned process is contained ti4+Aqueous solution in, and use microwave radiation.
Experiment finds, the tio that second step is made2Film growth speed is faster than the first step, and crystal structure is complete, and particle size distribution is 50
[peiro ana m, elena vigil, et a1.titanium () oxide thin films between ~ 100nm
Obtained by a two-step-solution method.thin solid films, 2002,411:185].Wang etc.
With Schweinfurt green and sodium hydroxide as raw material, in alcohol solvent, by microwave radiation, successfully synthesis mean diameter is the cuo of 4nm
Granule.Granule-morphology is spherical in shape, purity height [wang hui, xu jinzhong, the et a1.preparation of of product
cuo nanopar-ticles by microwave irradiation.j cryst growth,2002,244:88].
Sum it up, traditional porous charcoal loads synthetic method long, the masterplate that often there is synthetic route of nano material
Agent high cost, the problems such as the later stage processes seriously polluted, thus is difficult to large-scale production.The pore passage structure of carbon carrier, and
The parameter such as the metal supporting or the size of metal-oxide, component, crystalline phase and loading is difficult to be controlled simultaneously.Additionally, passing
System synthetic method can not be widely used in the preparation of various nano metals or oxide due to the restriction of preparation method.Therefore,
A kind of simply pervasive porous charcoal supported nano-gold genus of exploitation or the preparation method of metal oxide composite, and can close
Control the parameter such as the pore passage structure of carbon carrier and the size of nanoparticle, component, crystalline phase and loading, for this during one-tenth
The extensive application of class material will produce great impetus.
Content of the invention
It is an object of the invention to developing a kind of simply pervasive porous charcoal supported nano-gold to belong to oxide or nano metal
The preparation method of material, the method can be widely suitable for the synthesis that numerous charcoals carry metal-oxide or metal.
The present invention forms molten homogeneous liquid so that slaine is equal at a certain temperature using saccharide, carbamide and slaine
Even it is distributed in mixing liquid.Afterwards, saccharide carbonization is made to obtain porous charcoal using microwave heating, metal active constituent is equal simultaneously
Even be distributed in porous charcoal, subsequently after high-temperature heat treatment under shielding gas or reducing atmosphere, obtain porous charcoal supported nano-gold
Belong to oxide or nano metal material.
The specific implementation step of the present invention is: microwave method preparation porous charcoal supported nano-gold belongs to oxide or nano metal material
Material, is carried out as steps described below:
A) will be placed in the vessel for the mixing of saccharide, carbamide and slaine, at 100 ~ 220 DEG C, stirring 5 ~ 60 min are so that mixing is solid
Body melts completely, forms uniform solution；
B) by the solution obtaining in step a) microwave treatment 1 ~ 60min, the power of microwave heating is 100 ~ 1200w so that saccharide
Dehydration carbonization obtains dark brown solid；
C) by the dark brown solid being obtained in step b) under protective gas atmosphere, at 200-1100 DEG C, heat treatment 2-24h, obtains
The nano metal oxide materials of porous charcoal load；
D) by the dark brown solid being obtained in step b) under reproducibility atmosphere, at 200 ~ 1100 DEG C, heat treatment 2 ~ 24 h, obtains
Nano metal/alloy material to porous charcoal load.
Slaine wherein described in step (a) be metal nitrate, halogenide, hypochlorite, acetate, oxalates,
One of phosphate or sulfate or the salt of more than one different metal elements, the species of metallic element has: mg, al, pb,
in、sn、sb、zr、nb、la、ce、ta、mo、w、re、ti、v、cr、mn、fe、co、ni、cu、zn、ag、pt、pd、ir、ru、rh、
Y, ba, sr, la and os.Wherein in step (a), saccharide is in glucose, Fructose, sucrose, maltose, Lactose, starch and dextrin
A kind of；
Wherein in step (a), saccharide and the mass ratio of carbamide are 20:1 ~ 1:60；The mass ratio of saccharide and slaine in step (a)
For 100:1 ~ 1:10；
Shielding gas wherein described in step (c) is one of nitrogen, argon, helium；Reproducibility gas described in step (d)
Body is hydrogen or carbon monoxide volume fraction is 5% ~ 10% gaseous mixture, and Balance Air is nitrogen or argon.
The porous carbon supported nano-gold that wherein said step (c) obtains belongs to oxide, can be single metallic elements oxide
Can be metal composite oxide, wherein single metal oxides include one of oxide of following elements, and composition metal
Oxide then include the oxide of two or more different metal element: mg, al, pb, in, sn, sb, zr, nb, la, ce,
Ta, mo, w, re, ti, v, cr, mn, fe, co, ni, cu, zn, ag, pt, pd, ir, ru, rh, y, ba, sr, la and os.
The porous carbon supported nano-gold that wherein said step (d) obtains belongs to material, can be a kind of list of metallic element
Matter can also be alloy or the intermetallic compound of two kinds and above different metal element, wherein metallic element include mg, al,
sc、ti、v、cr、mn、fe、co、ni、cu、zn、nb、mo、pt、pd、ru、os、rh、ir、au、ag、pb、in、sn、sb、zr、nb、
La, ce, ta, mo, w and re.
The present invention forms molten homogeneous liquid so that slaine is equal at a certain temperature using saccharide, carbamide and slaine
Even it is distributed in mixing liquid.Afterwards, using the method for fabricated in situ, saccharide dehydration carbonization, metal simultaneously are made at high temperature
Component is evenly distributed in carbon carrier, obtains charcoal supported nano-gold finally by high-temperature heat treatment and belongs to.The present invention can be used for bearing
Carry numerous nano metal materials, its a size of 5 ~ 1000 nm and monodispersity are high, by adjusting synthesis condition, can control and receive
The composition of rice metal, crystalline phase and loading etc..Additionally, the pore size of carbon carrier can also pass through proportioning raw materials, reaction pressure
The condition such as power and temperature, time is controlled, and pore-size distribution is from 0.1 nm ~ 10 μm.This synthetic method belongs to anhydrous system,
The synthesis that prior synthesizing method causes because metal salt solution hydrolyzes can be avoided difficult.Additionally, the present invention also has synthesis
The advantage such as route is simple and with low cost, therefore all many-sides such as Industrial Catalysis, water process and electrochemistry have huge should
Use prospect.
Brief description
Fig. 1 be embodiment 1 be obtained xrd figure.
Fig. 2 is the xrd figure of the porous charcoal carried metal ni that embodiment 2 is obtained.
Fig. 3 is the xrd figure of the porous charcoal carried metal ni that embodiment 3 is obtained.
Fig. 4 is the xrd figure of the porous charcoal carried metal ag that embodiment 4 is obtained.
Fig. 5 is the xrd figure of the porous charcoal carried metal cu that embodiment 5 is obtained.
Fig. 6 is the tem figure of the porous charcoal carried metal ni that embodiment 1 is obtained.
Fig. 7 is the tem figure of the porous charcoal carried metal ni that embodiment 2 is obtained.
Fig. 8 is the tem figure of the porous charcoal carried metal ni that embodiment 3 is obtained.
Specific embodiment
With reference to specific embodiment, the present invention will be further described, but protection scope of the present invention not limited to this.
Embodiment 1: porous charcoal load nanometer ni
Synthesis material: glucose, carbamide, ni (no3)2`6h2O(nickel nitrate)
(1) 1.5 g glucoses, 2.5 g carbamide and 0.9 g ni (no are weighed3)2·9h2O in 100 ml beakers, afterwards
Beaker is placed in heatable magnetic stirring apparatuss.The temperature of magnetic stirring apparatuss rises to 120 DEG C, and continuously stirred 10min is straight
To beaker, medicine forms molten condition.
(2) melt liquid described in (1) is taken out, put into heating in microwave, heating power is 300w, heating 15min obtains
To pitchy bulk solids.
(3) with mortar by the sample obtaining in (2) grind, and put with crucible in, at 500 DEG C, 5%h2/n2Under the conditions of heat
Process 5 h, obtain porous charcoal load nanometer ni, xrd test display ni size is 35 nm.
Fig. 1 belongs to the xrd figure of ni for porous charcoal supported nano-gold, and in figure visible nano metal ni is evenly distributed on carbon carrier
In, the tem that Fig. 6 belongs to ni for carbon supported nano-gold schemes it was demonstrated that nano metal ni is consistent with xrd result.
Embodiment 2: porous charcoal load nanometer ni
Synthesis material: glucose, carbamide, ni (no3)2`6h2O(nickel nitrate)
(1) 1.5 g glucoses, 2.5 g carbamide and 0.9 g ni (no are weighed3)2·9h2O in 100 ml beakers, afterwards
Beaker is placed in heatable magnetic stirring apparatuss.The temperature of magnetic stirring apparatuss rises to 120 DEG C, and continuously stirred 10min is straight
To beaker, medicine forms molten condition.
(2) melt liquid described in (1) is taken out, put into heating in microwave, heating power is 500w, heating 10min obtains
To pitchy bulk solids.
(3) with mortar by the sample obtaining in (2) grind, and put with crucible in, at 500 DEG C, 5%h2/n2Under the conditions of heat
Process 5 h, obtain porous charcoal load nanometer ni, xrd test display ni size is 22 nm.
Fig. 2 belongs to the xrd figure of ni for porous charcoal supported nano-gold, and in figure visible nano metal ni is evenly distributed on carbon carrier
In, the tem that Fig. 7 belongs to ni for carbon supported nano-gold schemes it was demonstrated that nano metal ni particle diameter about 20nm, is consistent with xrd result.
Embodiment 3: porous charcoal load nanometer ni
Synthesis material: glucose, carbamide, ni (no3)2`6h2O(nickel nitrate)
(1) 1.5 g glucoses, 2.5 g carbamide and 0.9 g ni (no are weighed3)2·9h2O in 100 ml beakers, afterwards
Beaker is placed in heatable magnetic stirring apparatuss.The temperature of magnetic stirring apparatuss rises to 120 DEG C, and continuously stirred 10min is straight
To beaker, medicine forms molten condition.
(2) melt liquid described in (1) is taken out, put into heating in microwave, heating power is 700w, heating 5min obtains
Pitchy bulk solids.
(3) with mortar by the sample obtaining in (2) grind, and put with crucible in, at 500 DEG C, 5%h2/n2Under the conditions of heat
Process 5 h, obtain porous charcoal load nanometer ni, xrd test display ni size is 8 nm.
Fig. 3 belongs to the xrd figure of ni for porous charcoal supported nano-gold, and in figure visible nano metal ni is evenly distributed on carbon carrier
In.The tem that Fig. 8 belongs to ni for carbon supported nano-gold schemes it was demonstrated that the metal particle diameter that this method obtains is about 6nm.
Experimental example 4: porous charcoal load nanometer ag
Synthesis material: Fructose, carbamide, ag (no3)2(silver nitrate)
(1) 1 g Fructose, 5g carbamide, ag (no are weighed3)2In 100 ml beakers, afterwards beaker is placed on heatable
In magnetic stirring apparatuss.The temperature of magnetic stirring apparatuss rises to 120 DEG C, and continuously stirred 15 min form melting up to medicine in beaker
State.
(2) 15min will be heated in beaker microwave after, heating power is 800w, obtains pitchy bulk solids.
(3) with mortar, the product obtaining in (2) is ground, and be put in crucible.The product obtaining will be reacted at 200 DEG C,
h2Under the conditions of heat treatment 2 hours, obtain porous charcoal load nanometer ag.
The xrd that Fig. 4 belongs to ag for carbon supported nano-gold schemes it was demonstrated that the metal that this method obtains has higher degree of crystallinity.
Experimental example 5: porous charcoal load nanometer pd
Synthesis material: glucose, carbamide, pd (no3)2·2h2O(Palladous nitrate .)
(1) weigh 20 g glucoses and 1 g carbamide in 100 ml beakers, afterwards beaker is placed on heatable magnetic force
In agitator.The temperature of magnetic stirring apparatuss rises to 120 DEG C, and continuously stirred 10 min form molten up to medicine in beaker
State.
(3) 10min will be heated in beaker microwave after, heating power is 500w, obtains pitchy bulk solids.300
At DEG C, 5%h2/n2Under the conditions of heat treatment 3 hours, obtain porous charcoal supported nano-gold and belong to pd particle.
Experimental example 6: porous charcoal load nano-cu
Synthesis material: Lactose, carbamide, cu (no3)2·3h2O(copper nitrate)
(1) weigh 1 g Lactose and 60g carbamide in 100 ml beakers, afterwards beaker is placed on heatable magnetic force and stirs
Mix in device.The temperature of magnetic stirring apparatuss rises to 130 DEG C, and continuously stirred 15min forms molten condition up to medicine in beaker.
(2) weigh 1 g cu (no3)2·3h2O adds in melt liquid described in (1), continuously stirred 20min, to melting
State.15min will be heated afterwards, heating power is 700w, obtains pitchy bulk solids in beaker microwave.
(3) with mortar, the product obtaining in (2) is ground, and be put in crucible.At 500 DEG C, 5%h2/n2Under the conditions of heat
Process 4 hours, obtain porous charcoal supported nano-gold and belong to cu particle, xrd display cu size is 30 nm.
The xrd that Fig. 5 belongs to cu for carbon supported nano-gold schemes it was demonstrated that the metal that this method obtains has higher degree of crystallinity.
Experimental example 7: porous charcoal load nanometer fe2o3
Synthesis material: Lactose, carbamide, fe (no3)2·9h2O(ferric nitrate)
(1) weigh 1g Lactose and 10g carbamide in 100 ml beakers, afterwards beaker is placed on heatable magnetic force and stirs
Mix in device.The temperature of magnetic stirring apparatuss rises to 130 DEG C, and continuously stirred 25min forms molten condition up to medicine in beaker.
(2) 15min will be heated in beaker microwave after, heating power is 500w, obtains pitchy bulk solids.
(3) with mortar, the product obtaining in (2) is ground, and be put in crucible.The product obtaining will be reacted in n2Protection
Under under conditions of 650 DEG C heat treatment 4 hours, obtain porous charcoal load fe2o3Nanoparticle.
Claims (7)
1. a kind of microwave-assisted prepare porous charcoal supported nano-gold belong to oxide or nano metal material method it is characterised in that
Carry out as steps described below:
A) saccharide and carbamide are pressed the mass ratio of 20:1 ~ 1:60, saccharide is mixed according to the mass ratio of 100:1 ~ 1:10 with slaine
Placed in the vessel, at 100 ~ 220 DEG C, 5 ~ 60 min are so that hybrid solid melts completely for stirring, form uniform solution；
B) 0.5min ~ 60min will be processed under the solution obtaining in step a) microwave heating, the power of microwave heating is 100 ~
30kw is so that saccharide dehydration carbonization obtains dark brown solid；
C) by the dark brown solid being obtained in step b) under protective gas atmosphere, at 250-1100 DEG C, heat treatment 2-24h, obtains
The nano metal oxide materials of porous charcoal load；
D) by dark brown solid obtained by step b) under reproducibility atmosphere, at 200 ~ 1100 DEG C, heat treatment 2 ~ 24 h, obtains
Nano metal/the alloy material of porous charcoal load.
2. a kind of microwave-assisted preparation porous charcoal supported nano-gold according to claim 1 belongs to oxide or nano metal material
The method of material is it is characterised in that the slaine wherein described in step (a) is metal nitrate, halogenide, hypochlorite, acetic acid
One of salt, oxalates, phosphate or sulfate or the salt of more than one different metal elements, the species of metallic element has:
mg、al、pb、in、sn、sb、zr、nb、la、ce、ta、mo、w、re、ti、v、cr、mn、fe、co、ni、cu、zn、ag、pt、pd、
Ir, ru, rh, y, ba, sr, la and os.
3. a kind of microwave-assisted according to claim 1 prepares the method that porous charcoal supported nano-gold belongs to material, its feature
It is that wherein in step (a), saccharide is glucose, Fructose, sucrose, maltose, Lactose, starch, in methylcellulose and dextrin
A kind of.
4. a kind of microwave-assisted according to claim 1 prepares the method that porous charcoal supported nano-gold belongs to material, its feature
It is that in wherein step (a), saccharide and the mass ratio of carbamide are 20:1 ~ 1:60；The mass ratio of saccharide and slaine in step (b)
For 100:1 ~ 1:10.
5. a kind of microwave-assisted according to claim 1 prepares the method that porous charcoal supported nano-gold belongs to material, its
It is characterised by that the shielding gas wherein described in step (c) is one of nitrogen, argon, helium；Reduction described in step (d)
Property gas be the gaseous mixture that hydrogen or carbon monoxide volume fraction are 5% ~ 10%, Balance Air is nitrogen or argon.
6. a kind of microwave-assisted preparation porous charcoal supported nano-gold according to claim 1 belongs to oxide or nano metal material
Material method it is characterised in that wherein said step (c) obtain nano-metal-oxide be single metallic elements oxide or
Metal composite oxide, wherein single metal oxides are one of oxide of following elements, and metal composite oxide is then
Oxide including two or more different metal element: mg, al, pb, in, sn, sb, zr, nb, la, ce, ta, mo, w,
Re, ti, v, cr, mn, fe, co, ni, cu, zn, ag, pt, pd, ir, ru, rh, y, ba, sr, la and os.
7. a kind of microwave-assisted preparation porous charcoal supported nano-gold according to claim 1 belongs to oxide or nano metal material
The method of material is it is characterised in that the nano metal that wherein said step (d) obtains can be a kind of simple substance of metallic element
Can be alloy or the intermetallic compound of two kinds and above different metal element, wherein metallic element include mg, al, sc, ti,
v、cr、mn、fe、co、ni、cu、zn、nb、mo、pt、pd、ru、os、rh、ir、au、ag、pb、in、sn、sb、zr、nb、la、ce、
Ta, mo, w or re.
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| CN108546962B (en) * | 2018-03-29 | 2020-01-17 | 上海大学 | Preparation method of high-specific-surface-area porous carbon iridium-doped electrolyzed water oxygen evolution catalyst |
| CN113443622A (en) * | 2020-08-19 | 2021-09-28 | 李潮云 | Method for loading nano metal oxide or nano metal material on porous carbon |
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