CN105800587A - Method for preparing porous carbon-loaded nano-material - Google Patents
Method for preparing porous carbon-loaded nano-material Download PDFInfo
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- CN105800587A CN105800587A CN201610129204.4A CN201610129204A CN105800587A CN 105800587 A CN105800587 A CN 105800587A CN 201610129204 A CN201610129204 A CN 201610129204A CN 105800587 A CN105800587 A CN 105800587A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
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- 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
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- 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The invention discloses a method for preparing a porous carbon-loaded nano-material, belongs to the technical field of porous material preparation, and particularly relates to a porous carbon-loaded nano-metal oxide or nano-metal material prepared by utilizing organic amine as a template by one-step in situ formation through high-temperature melting, charring and roasting treatment. According to the method, the pore size of porous carbon is regulated and controlled by different types of organic amine templates, the whole process has the advantage of simple one-step operation, low preparation cost and the like, and the prepared porous carbon-loaded nano-metal oxide or nano-metal material has a wide application prospect in industrial catalysis, water treatment, electrochemistry and other aspects.
Description
Technical field
The invention provides the preparation method of a kind of novel porous charcoal load nano material, belong to porous material preparing technical field.
Background technology
Porous carbon material has higher specific surface area, flourishing pore structure, surface has more functional group and the strongest absorbability, also have high temperature resistant, acid and alkali-resistance, conduct electricity and a series of advantage such as heat transfer, regulatable aperture and surface property, make porous carbon material be widely used in fields such as catalyst carrier, ultracapacitor, catalyst, adsorbents.Preparing the method that porous carbon materials the most generally uses is template, furfuryl alcohol, ethylene, acrylonitrile, phenolic resin, resorcinol formaldehyde resin, acetonitrile, polypyrrole, pitch prill also have other aromatic compound etc. for carbon source, introduce porogen to match with template, synthesize through carbonization, template is removed after completing pore, form hole, thus prepare porous carbon materials.Ryoo et al. (Angew. Chem. Int. Ed., 2003,
42 (19): 2182-2185) prove that the mesoporous of silicon dioxide can be filled by the presoma (such as sucrose) of charcoal, thus from silica template, generate the copy of a carbon.Can be obtained by meso-porous carbon material by after silicon template etch, the structure of this material is to be determined by the pattern of silica template.The method preparation technology is relative complex, and cost is high.The porous carbon materials of synthesis is the anti-phase copy of its template, can introduce some impurity in building-up process unavoidably.
In recent years, people have carried out another method: soft template method.Soft template method is that one presoma reacts with surfactant, through polymerization, carbonization and the method for self assembly porous carbon materials.Moriguchi et al. is at first time in 1999 report Micellar Gel synthesizing ordered mesoporous carbon material.Being inspired by synthesis MCM-41, they are with surfactant CTAB (cetyltrimethylammonium bromide, the CTAB) phenolic resin that as template and successfully assembles mesoporous phase and surfactant.Although soft template method can synthesize the mesoporous carbon of high-sequential, but the price limit of its costliness its scale business application.
Often there is synthetic route for the synthetic method of traditional porous charcoal load nano material long, template agent cost is high, and the later stage processes the problems such as seriously polluted, thus is difficult to large-scale production.Therefore this method use cheap organic amine be template, glucose be that carbon source one-step synthesis porous charcoal supported nano-gold belongs to or metal oxide composite, utilize and control different types of Organic amine template regulation and control porous charcoal pore size, it is achieved the adjustable control of porous charcoal pore structure is standby.
Summary of the invention
It is an object of the invention to develop a kind of simple and quick novel porous charcoal supported nano-gold belong to or the preparation method of metal oxide composite, the method can be widely suitable for numerous charcoal and carry metal and the synthesis of oxide.
The present invention utilizes saccharide to be carbon source, organic amine forms molten homogeneous liquid at a certain temperature for template agent and slaine so that slaine is evenly distributed in mixing liquid.Afterwards, heating makes saccharide carbonization obtain porous charcoal, during metal active constituent is evenly distributed on porous charcoal simultaneously, subsequently under protection gas or reducing atmosphere after high-temperature heat treatment, obtains porous charcoal supported nano-gold genus/metal oxide composite.
The step that is embodied as of the present invention is: a kind of method that porous charcoal supported nano-gold belongs to oxide or nano metal material, carries out as steps described below:
A) saccharide and organic amine are pressed the mass ratio of 100:1 ~ 1:10, and saccharide mixes placed in the vessel with slaine according to the mass ratio of 100:1 ~ 1:10, at 50-220
At DEG C, stir 10-60
Min so that hybrid solid melts completely, forms uniform solution；
B) by the solution that obtains in step a) at 100-250
Heat treatment 8-48 at a temperature of DEG C
H so that saccharide dehydration carbonization obtains dark brown solid；This heat treatment process can be carried out in normal pressure or airtight reactor；
C) by the dark brown solid for preparing in step b) under protective gas atmosphere, in 250-1100
Heat treatment 2-24 h at DEG C, obtains the nano metal oxide materials of porous charcoal load；
D) nano-metal-oxide loaded by the charcoal obtained by step c) is under reproducibility atmosphere, in 250-1100
Heat treatment 1-24 h at DEG C, obtains the nano metal/nano metal oxide materials of porous charcoal load.
Wherein in step (a), saccharide is the one in glucose, fructose, sucrose, maltose, lactose, starch and dextrin.
Wherein the organic amine described in step (a) is fatty amines (ethylenediamine, triethylamine), alcamines (monoethanolamine, diethanolamine, triethanolamine, monoisopropanolamine), amide-type (Methanamide, diethylenetriamines), polymine.
Wherein the protection gas described in step (c) is the one in nitrogen, argon, helium.
Wherein the reducibility gas described in step (d) is hydrogen or carbon monoxide volume fraction is the gaseous mixture of 5% ~ 10%, and Balance Air is nitrogen or argon.
It is single metallic elements oxide or metal composite oxide that wherein said step (c) obtains nano-metal-oxide, one during wherein single metal oxides is the oxide of following elements, metal composite oxide then includes the oxide of two or more different metal element: Mg, Al, Pb, Sn, Sb, Zr, Nb, La, Ce, Mo, W, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ag, Pt, Pd, Ir, Ru, Rh, Y, Ba, Sr.
The nano metal that wherein said step (d) obtains can be the simple substance of a kind of metallic element can also be two kinds and the alloy of above different metal element or intermetallic compound, wherein metallic element includes Mg, Al, Pb, Sn, Sb, Zr, Nb, La, Ce, Mo, W, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ag, Pt, Pd, Ir, Ru, Rh, Y, Ba, Sr.
The present invention utilize organic amine for template, through and saccharide, slaine high-temperature fusion, carbonization and calcination process, obtain the nano-metal-oxide of porous charcoal load or the nano metal material being formed in situ with organic amine for template one-step method.The present invention may be used for loading numerous nano metal or oxide material, its a size of 10-1000
Nm and monodispersity are high, by regulation synthesis condition, can control nano metal or the composition of oxide, crystalline phase and loading etc..Additionally, the pore size of high-area carbon can also be controlled by the kind of organic amine, pore-size distribution is from 0.1
nm-10 μm.This synthetic method belongs to anhydrous system, can avoid the synthesis difficulty that prior synthesizing method causes due to metal salt solution hydrolysis.Additionally, the present invention also has the advantages such as synthetic route is simple and with low cost, therefore have huge application prospect in all many-sides such as Industrial Catalysis, water process and electrochemistry.
Accompanying drawing explanation
Fig. 1 is the XRD figure of the porous charcoal loaded Cu that embodiment 1 prepares.
Fig. 2 is the TEM figure of the porous charcoal loaded Cu that embodiment 1 prepares.
Fig. 3 is the XRD figure of the porous charcoal load Ni alloy that embodiment 2 prepares.
Fig. 4 is the nitrogen adsorption-desorption test curve of the porous charcoal load Ni alloy that embodiment 2 prepares.
Fig. 5 is the graph of pore diameter distribution of the porous charcoal load Ni alloy that embodiment 2 prepares.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention will be further described, but protection scope of the present invention is not limited to this.
Embodiment 1: porous charcoal load nanometer Cu
Synthesis material: glucose, ethylenediamine, Cu (NO3)2·3H2O(copper nitrate)
(1) 1 g glucose and 0.1 g Cu (NO are weighed3)2·3H2Beaker, in 100 mL beakers, is placed in heatable magnetic stirring apparatus after slowly dripping the ethylenediamine of 10 g by O.The temperature of magnetic stirring apparatus rises to 100 DEG C, and continuously stirred 60 min until in beaker medicine formed molten condition.
(2) by melt liquid described in (1), take out a part of solution to put in 120 DEG C of baking ovens and be designated as sample A, another part solution addition pyroreaction still is put in 120 DEG C of baking ovens and is designated as sample B, reacting 48 h sample A and obtain pitchy bulk solids, sample B obtains pitchy compact solid.
(3) with mortar, the sample A obtained in (2) and sample B is ground respectively, and point be put in two crucibles, then at N2Protect lower 550 DEG C of heat treatments 7 hours, obtain porous charcoal load nanometer CuO.
(4) by the sample A that obtains in (3) at 500 DEG C, 5% H2/N2Under the conditions of heat treatment 6 h, obtain porous charcoal load nanometer Cu, XRD test display Cu size be 50 nm.
Experimental example 2: porous charcoal load Ni nanoparticle alloy
Synthesis material: glucose, polymine (PEI), Ni (NO3)2·6H2O
(1) 10 g glucoses, 0.1 g PEI, 0.1 g Ni (NO are weighed3)2·6H2Beaker, in 100 mL beakers, is placed in heatable magnetic stirring apparatus by O afterwards.The temperature of magnetic stirring apparatus rises to 220 DEG C, and continuously stirred 60 min until in beaker medicine formed molten condition.
(2) after, beaker is put in 250 DEG C of baking ovens, react 1 hour, obtain pitchy bulk solids.
(3) with mortar, the product obtained in (2) is ground, and be put in crucible.The product that reaction is obtained at 250 DEG C, 5% H2/N2Under the conditions of heat treatment 24 hours, obtain porous charcoal load Ni nanoparticle granule.
Experimental example 3: porous charcoal load nano-TiO2
Synthesis material: sucrose, ethanolamine, TiOSO4(titanyl sulfate)
(1) weigh 1 g sucrose and 5 g ethanolamine in 100 mL beakers, afterwards beaker is placed in heatable magnetic stirring apparatus.The temperature of magnetic stirring apparatus rises to 100 DEG C, and is stirred continuously until medicine formation molten condition in beaker.
(2) 10 g TiOSO are weighed4Adding described in (1) in melt liquid, continuously stirred 15 min, to molten condition.Afterwards beaker is put in 160 DEG C of baking ovens, react 40 hours, obtain pitchy bulk solids.
(3) with mortar, the product obtained in (2) is ground, and be put in crucible.Product reaction obtained is at N2Under protection under conditions of 250 DEG C heat treatment 24 hours, obtain porous charcoal load TiO2Nanoparticle, XRD shows TiO2Size is 20 nm, and crystal formation is anatase.
Claims (8)
1. the preparation method that a novel porous charcoal supported nano-gold belongs to, it is characterised in that carry out as steps described below:
A) saccharide and organic amine are pressed the mass ratio of 100:1 ~ 1:10, and saccharide mixes placed in the vessel with slaine according to the mass ratio of 100:1 ~ 1:10, at 50-220 DEG C, stirs 10-60 min so that hybrid solid melts completely, forms uniform solution；
B) the solution heat treatment 8-48 h at a temperature of 100-250 DEG C that will obtain in step a) so that saccharide dehydration carbonization obtains dark brown solid；This heat treatment process can be carried out in normal pressure or airtight reactor；
C) by the dark brown solid for preparing in step b) under protective gas atmosphere, heat treatment 2-24 h at 250-1100 DEG C, obtain the nano metal oxide materials of porous charcoal load；
D) nano-metal-oxide loaded by the charcoal obtained by step c) is under reproducibility atmosphere, and heat treatment 1-24 h at 250-1100 DEG C obtains the nano metal/nano metal oxide materials of porous charcoal load.
The method that a kind of porous charcoal supported nano-gold the most according to claim 1 belongs to oxide or nano metal material, it is characterised in that wherein the slaine described in step (a) is the salt of one or more different metal elements in metal nitrate, halogenide, hypochlorite, acetate, oxalates, phosphate or sulfate.
The method that a kind of porous charcoal supported nano-gold the most according to claim 1 belongs to oxide or nano metal material, it is characterised in that wherein in step (a), saccharide is the one in glucose, fructose, sucrose, maltose, lactose, starch and dextrin.
The method that a kind of porous charcoal supported nano-gold the most according to claim 1 belongs to oxide or nano metal material, it is characterised in that wherein the organic amine described in step (a) is fatty amines, alcamines, amide-type, alicyclic ring amine, aromatic amine, naphthalene system amine, other amine.
The method that a kind of porous charcoal supported nano-gold the most according to claim 1 belongs to oxide or nano metal material, it is characterised in that wherein in step (a), the mass ratio of saccharide and organic amine is 100:1 ~ 1:10；In step (b), saccharide is 100:1 ~ 1:10 with the mass ratio of slaine.
The method that a kind of porous charcoal supported nano-gold the most according to claim 1 belongs to oxide or nano metal material, it is characterised in that wherein the protection gas described in step (c) is the one in nitrogen, argon, helium；Reducibility gas described in step (d) is hydrogen or carbon monoxide volume fraction is the gaseous mixture of 5% ~ 10%, and Balance Air is nitrogen or argon.
A kind of porous charcoal supported nano-gold the most according to claim 1 belongs to the preparation method of oxide or metal material, it is characterized in that wherein said step (c) obtains nano-metal-oxide is single metallic elements oxide or metal composite oxide, one during wherein single metal oxides is the oxide of following elements, metal composite oxide then includes the oxide of two or more different metal element: Mg, Al, Pb, Sn, Sb, Zr, Nb, La, Ce, Mo, W, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ag, Pt, Pd, Ir, Ru, Rh, Y, Ba, Sr.
A kind of porous carbon supported nano-gold the most according to claim 1 belongs to the preparation method of oxide or metal material, it is characterized in that the nano metal that wherein said step (d) obtains can be the simple substance of a kind of metallic element can also be two kinds and the alloy of above different metal element or intermetallic compound, wherein metallic element includes Mg, Al, Pb, Sn, Sb, Zr, Nb, La, Ce, Mo, W, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ag, Pt, Pd, Ir, Ru, Rh, Y, Ba, Sr.
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Cited By (4)
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| CN108179301A (en) * | 2017-12-27 | 2018-06-19 | 武汉工程大学 | A kind of preparation method of carbon containing composite carrier load nano metal material |
| CN111217743A (en) * | 2020-03-20 | 2020-06-02 | 中国科学院兰州化学物理研究所 | Method for synthesizing amide compound from non-metallic porous carbon catalytic heterocyclic compound |
| CN111940721A (en) * | 2020-08-19 | 2020-11-17 | 李潮云 | Method for loading nano metal oxide or nano metal material on porous carbon |
| WO2021018268A1 (en) * | 2019-08-01 | 2021-02-04 | 厦门大学 | Preparation method for carbon-supported nano-silver catalyst |
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| CN111940721A (en) * | 2020-08-19 | 2020-11-17 | 李潮云 | Method for loading nano metal oxide or nano metal material on porous carbon |
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