CN109126814A - A kind of method of micro nano structure copper molybdate growth in situ - Google Patents
A kind of method of micro nano structure copper molybdate growth in situ Download PDFInfo
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- CN109126814A CN109126814A CN201811134947.6A CN201811134947A CN109126814A CN 109126814 A CN109126814 A CN 109126814A CN 201811134947 A CN201811134947 A CN 201811134947A CN 109126814 A CN109126814 A CN 109126814A
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- 238000000034 method Methods 0.000 title claims abstract description 22
- IKUPISAYGBGQDT-UHFFFAOYSA-N copper;dioxido(dioxo)molybdenum Chemical compound [Cu+2].[O-][Mo]([O-])(=O)=O IKUPISAYGBGQDT-UHFFFAOYSA-N 0.000 title claims abstract description 11
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 11
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 9
- 239000010949 copper Substances 0.000 claims abstract description 41
- 229910052802 copper Inorganic materials 0.000 claims abstract description 22
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 21
- 230000003647 oxidation Effects 0.000 claims abstract description 11
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 11
- 239000011684 sodium molybdate Substances 0.000 claims abstract description 6
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000000463 material Substances 0.000 claims description 22
- 238000006243 chemical reaction Methods 0.000 claims description 11
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000001354 calcination Methods 0.000 claims description 7
- 239000003792 electrolyte Substances 0.000 claims description 7
- 235000015393 sodium molybdate Nutrition 0.000 claims description 5
- 235000019441 ethanol Nutrition 0.000 claims description 4
- 239000011521 glass Substances 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- 238000010792 warming Methods 0.000 claims description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims 1
- 239000001301 oxygen Substances 0.000 claims 1
- 238000003786 synthesis reaction Methods 0.000 abstract description 7
- 239000000126 substance Substances 0.000 abstract description 6
- 239000003054 catalyst Substances 0.000 abstract description 5
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 230000003197 catalytic effect Effects 0.000 abstract description 3
- 238000009776 industrial production Methods 0.000 abstract description 3
- 231100000614 poison Toxicity 0.000 abstract description 3
- 230000007096 poisonous effect Effects 0.000 abstract description 3
- 239000008187 granular material Substances 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 229910004619 Na2MoO4 Inorganic materials 0.000 abstract 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 abstract 1
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 description 4
- 239000003513 alkali Substances 0.000 description 3
- 238000012512 characterization method Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000007772 electrode material Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 230000009257 reactivity Effects 0.000 description 2
- 238000001291 vacuum drying Methods 0.000 description 2
- 238000013019 agitation Methods 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 238000007743 anodising Methods 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 239000011805 ball Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005297 material degradation process Methods 0.000 description 1
- 239000004005 microsphere Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- VLAPMBHFAWRUQP-UHFFFAOYSA-L molybdic acid Chemical compound O[Mo](O)(=O)=O VLAPMBHFAWRUQP-UHFFFAOYSA-L 0.000 description 1
- 239000011807 nanoball Substances 0.000 description 1
- 239000002077 nanosphere Substances 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 239000013535 sea water Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
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- 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
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/85—Chromium, molybdenum or tungsten
- B01J23/88—Molybdenum
- B01J23/885—Molybdenum and copper
-
- 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
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
-
- 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
- B01J35/20—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state
- B01J35/23—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state in a colloidal state
-
- 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
- B01J35/391—Physical properties of the active metal ingredient
- B01J35/393—Metal or metal oxide crystallite size
-
- 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
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
- B01J35/51—Spheres
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/348—Electrochemical processes, e.g. electrochemical deposition or anodisation
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Health & Medical Sciences (AREA)
- Plasma & Fusion (AREA)
- Toxicology (AREA)
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Abstract
A kind of method of micro nano structure copper molybdate growth in situ, can be used to quick, easy synthesis Cu3Mo2O9.With Na2MoO4·2H2O is raw material, and anodic oxidation growth in situ is first carried out on copper mesh into the CuMoO of micro-nano chondritic4, then calcined after vacuum oven is dry through tube furnace, finally obtain the stable micro-nano spherical Cu of performance3Mo2O9.The present invention is simple, conveniently, it is at low cost, industrial production can be used on a large scale, gained catalyst granules small (partial size only has 860nm), catalytic activity be high, it is renewable, reusable, do not generate poisonous and harmful substance in the process, with high economic benefits and social benefits.
Description
Technical field
The invention belongs to inorganic micro-nano semiconductor materials to synthesize field, and it is raw in situ to be related to a kind of micro nano structure copper molybdate
Long method makes to be formed on copper mesh and equally distributed stablizes micro-nano chondritic using simple anodizing
Cu3Mo2O9, the material after oxidation is placed in the calcining of tube furnace high temperature.It, can be with the present invention can obtain the material that performance is stable
It applies in the fields such as dilatancy fireproof coating and electrode material.
Background technique
Because of distinctive structure, electrical property and catalytic performance, metal molybdate nano material is had received widespread attention.Research
Show metal molybdate nano material not only in wastewater by photocatalysis, electrode material, seawater corrosion, pigment and negative expansion
There is a good application value in the fields such as material, and optics, fluorophor, humidity inductive and antibacterial field obtain also have it is excellent
Application potential.Therefore novel molybdate nano material is developed, had very important significance.
Metal molybdate have high-ratio surface, surface can, more active sites and the advantageous properties such as highly selective, receive very
The concern of more scholars.The country also discloses the method for some synthesis molybdates.Chinese invention patent CN 201510096407.3 is public
It has opened and a kind of has prepared the spherical alkali formula copper molybdate (Cu of micron3(OH)2(MO4)2) method, the spherical diameter of generated micron is
20 μm, though the spherical alkali formula copper molybdate (Cu of the micron that high-purity can be synthesized3(OH)2(MO4)2), but this method has the pH of solution
There is very high requirement.In addition, Chinese invention patent CN201110347508.5 discloses and a kind of prepares spoke using microwave reaction
Penetrate shape molybdic acid copper micron ball shape structure (Cu3Mo2O9) method, the method for use is novel, but the grain diameter synthesized is larger and anti-
It answers condition to need microwave, is not the best approach of synthetic alkali formula copper molybdate.To solve above-mentioned problem of the prior art, the present invention is mentioned
A kind of activity Cu is supplied3Mo2O9The preparation method of micro-nano chondritic.Not only the reaction time is short for this method, reflection mild condition
And prepared material has relatively good pattern and good stability.In addition, synthetic material particle of the present invention is by micro-
Nanosphere body composition and partial size only has 860nm, this is that big specific surface area and more is provided when material degradation organic pollutant
Reactivity site.
Summary of the invention
In view of the above-mentioned problems existing in the prior art, the applicant provides a kind of micro-nano ball that electrochemistry formated is stable
Shape structure C u3Mo2O9Method.The present invention is simple, conveniently, it is at low cost, industrial production, gained catalyst particles can be used on a large scale
Grain small (partial size only has 860nm), catalytic activity be high, it is renewable, reusable, do not generate poisonous and harmful substance in the process, tool
There are high economic benefit and social benefit.
Technical scheme is as follows: a kind of method of micro nano structure copper molybdate growth in situ includes the following steps,
H with the copper mesh of 2cm × 4cm through ethyl alcohol, 0.1mol/L2SO4, after deionized water cleaning pretreatment, it is dry to be placed in vacuum oven
It is dry, then carry out high-temperature calcination.Obtain final products: specific step is as follows:
(1) it pre-processes: with ethyl alcohol, the H of 0.1mol/L2SO4, deionized water be successively cleaned by ultrasonic 30min having a size of 2cm ×
It is dry to be placed in vacuum oven for the copper sheet of 4cm.
(2) anodic oxidation: using the copper sheet cleaned up in step (1) as anode, Pt piece is as cathode, to contain 5%
Sodium molybdate solution be electrolyte carry out anodic oxidation.The voltage of anodic oxidation be 3V, time 5min, 25 DEG C of temperature.Reaction
After, copper mesh is taken out and rinsed with deionized water from reaction system the solution of 3 removing material surfaces, obtains yellow green
The copper-based Cu of micro-nano chondritic3Mo2O9。
(3) it post-processes: the material after step (2) oxidation is placed in naturally dry in air.
(4) it calcines: the copper-based Cu of yellow green will be obtained in step (3)3Mo2O9The material of micro-nano chondritic is put into pipe
Calcination processing is carried out in formula furnace.Temperature is 450 DEG C, time 2h.
In step (1), the material can be also possible to copper sheet for copper mesh.Drying mode has: freeze-drying, air blast are dry
Dry, vacuum drying.When material is put into progress calcination processing in tube furnace, in air atmosphere.
Mode involved in step (2) with solution can be with are as follows: with glass bar stirring, ultrasonic treatment, magnetic agitation.Institute
Solvent is deionized water.
Washing time 3~6 times in step (1) (2).
The beneficial effects of the present invention are embodied in following three aspects:
(1) consersion unit is simple, and the reaction time is short, and reaction is convenient for operation.
(2) reaction raw materials are easy to get, and price is cheap, can be used for industrial production on a large scale.
(3) Cu synthesized3Mo2O9The more microsphere diameters of botryoidalis are small (860nm), can mention in degradable organic pollutant reaction
For big specific surface and more reactivity sites.
(4) entire reaction process does not generate any poisonous and harmful substance, belongs to clean manufacturing.
(5) serious catalyst surface substance can will be lost by ultrasonic cleaning to wash to realize catalyst regeneration,
To reduce cost.
Detailed description of the invention
Fig. 1 is the micro-nano spherical structure C u of synthesis3Mo2O9Preparation flow figure.
Fig. 2 is the Cu of synthesis3Mo2O9Under the different amplification of micro-nano chondritic SEM figure (figure b in illustration be
Pictorial diagram).
Fig. 3 is the Cu of synthesis3Mo2O9The Eds map of micro-nano chondritic.
Fig. 4 is the Cu of synthesis3Mo2O9The XRD diagram of micro-nano chondritic.
Specific embodiment
With reference to the accompanying drawing 1 and embodiment, the present invention is specifically described.
Embodiment 1
(1) with ethyl alcohol, the H of 0.1mol/L2SO4, deionized water be successively cleaned by ultrasonic copper of the 30min having a size of 2cm × 4cm
Piece, juxtaposition are dried in a vacuum drying oven.
(2) using the copper sheet cleaned up in step (1) as anode, Pt piece is as cathode, to be containing sodium molybdate solution
Electrolyte carries out anodic oxidation.The voltage of anodic oxidation be 3V, time 5min, 25 DEG C of temperature.After reaction, by copper mesh from
The solution that 3~5 removing material surfaces are taken out and rinsed with deionized water in reaction system, obtains the micro-nano spherical knot of yellow green
The copper-based Cu of structure3Mo2O9。
(3) material after step (2) oxidation is placed in naturally dry in air.
(4) the copper-based Cu of yellow green will be obtained in step (3)3Mo2O9The material of micro-nano chondritic, which is put into, leads to air
Tube furnace in carry out calcination processing.The process of calcination processing are as follows: 450 DEG C are warming up to the rate of 1 DEG C/min, then 450
2h is kept under the conditions of DEG C, and room temperature is finally down to the rate of 1 DEG C/min.
(5) material for obtaining step (4) carries out SEM characterization, by can be seen that synthesized substance is micro-nano in Fig. 2
Chondritic.Resulting materials catalyst granules is small (partial size only has 860nm).
(6) material for obtaining step (4) carries out EDS characterization, and Fig. 3 illustrates to contain tri- kinds of O, Cu, Mo in the material of synthesis
Element.The general proportions by can be seen that synthesized material each element in schematic diagram can be found out from table 1.
| Element | Weight% | Atomic% |
| O | 30.87 | 68.73 |
| Cu | 29.63 | 16.61 |
| Mo | 39.49 | 14.66 |
| Total | 100 | 100 |
(7) material for obtaining step (4) carries out XRD characterization, and as seen from Figure 4, substance synthesized by the present invention is
Cu3Mo2O9。
Claims (3)
1. a kind of method of micro nano structure copper molybdate growth in situ, includes the following steps:
(1) with ethyl alcohol, the H of 0.1mol/L2SO4, deionized water be successively cleaned by ultrasonic copper sheet of the 30min having a size of 2cm × 4cm, and
It is dry to be placed in vacuum oven.
(2) using the copper sheet after drying as anode, Pt piece is as cathode, to carry out anodic oxygen as electrolyte containing sodium molybdate solution
Change.The voltage of anodic oxidation be 3V, time 5min, 25 DEG C of temperature.After reaction, copper mesh is taken out simultaneously from reaction system
The solution that 3 removing material surfaces are rinsed with deionized water, obtains the copper-based Cu of the micro-nano chondritic of yellow green3Mo2O9。
(3) material after step (2) oxidation is placed in naturally dry in air.
(4) the copper-based Cu of yellow green will be obtained in step (3)3Mo2O9The material of micro-nano chondritic is placed in air tube furnace
Carry out calcination processing.
2. a kind of method of micro nano structure copper molybdate growth in situ according to claim 1, which is characterized in that the step
Suddenly the mass fraction of sodium molybdate is 5% in the electrolyte in (2), and when electrolyte quota will first weigh the sodium molybdate of 2.5g in 50mL
Glass beaker in, measure the deionized water of 50mL in beaker, electrolyte be stirred 2~5 minutes with glass bar and is obtained
Uniformly mixed electrolyte system.
3. a kind of method of micro nano structure copper molybdate growth in situ according to claim 1, which is characterized in that the step
Suddenly in (4) calcination processing process are as follows: be warming up to 450 DEG C with the rate of 1 DEG C/min, then keep 2h under the conditions of 450 DEG C, most
Room temperature is down to the rate of 1 DEG C/min afterwards.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811134947.6A CN109126814B (en) | 2018-09-28 | 2018-09-28 | Method for in-situ growth of copper molybdate with micro-nano structure |
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| CN201811134947.6A CN109126814B (en) | 2018-09-28 | 2018-09-28 | Method for in-situ growth of copper molybdate with micro-nano structure |
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| CN109126814A true CN109126814A (en) | 2019-01-04 |
| CN109126814B CN109126814B (en) | 2021-09-03 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113061954A (en) * | 2021-03-15 | 2021-07-02 | 深圳大学 | Method for preparing metal molybdate by anodic oxidation method, metal molybdate and application thereof |
| CN113880141A (en) * | 2021-11-01 | 2022-01-04 | 陕西科技大学 | Cu3Mo2O9 nanosheet array and preparation method thereof |
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