CN106064832B - A kind of nanoscale cuboid alkali formula copper molybdate and preparation method thereof - Google Patents
A kind of nanoscale cuboid alkali formula copper molybdate and preparation method thereof Download PDFInfo
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- CN106064832B CN106064832B CN201610529932.4A CN201610529932A CN106064832B CN 106064832 B CN106064832 B CN 106064832B CN 201610529932 A CN201610529932 A CN 201610529932A CN 106064832 B CN106064832 B CN 106064832B
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- molybdate
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- 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 31
- 239000003513 alkali Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 12
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000011684 sodium molybdate Substances 0.000 claims abstract description 7
- 235000015393 sodium molybdate Nutrition 0.000 claims abstract description 7
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 4
- 239000011259 mixed solution Substances 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 6
- 239000012535 impurity Substances 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 4
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 3
- 238000009413 insulation Methods 0.000 claims description 3
- 235000017281 sodium acetate Nutrition 0.000 claims description 3
- 239000001632 sodium acetate Substances 0.000 claims description 3
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 2
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 2
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 2
- 238000001291 vacuum drying Methods 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 6
- 239000002086 nanomaterial Substances 0.000 abstract description 6
- 230000015572 biosynthetic process Effects 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000003786 synthesis reaction Methods 0.000 abstract description 4
- 238000006555 catalytic reaction Methods 0.000 abstract description 3
- 238000004146 energy storage Methods 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000002904 solvent Substances 0.000 abstract 1
- 230000006641 stabilisation Effects 0.000 abstract 1
- 238000011105 stabilization Methods 0.000 abstract 1
- 238000000034 method Methods 0.000 description 10
- 239000010949 copper Substances 0.000 description 7
- 239000000047 product Substances 0.000 description 7
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 5
- 229910052802 copper Inorganic materials 0.000 description 5
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 description 4
- VLAPMBHFAWRUQP-UHFFFAOYSA-L molybdic acid Chemical compound O[Mo](O)(=O)=O VLAPMBHFAWRUQP-UHFFFAOYSA-L 0.000 description 3
- 230000008859 change Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 235000010755 mineral Nutrition 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 229910015667 MoO4 Inorganic materials 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 208000012826 adjustment disease Diseases 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- HNJBEVLQSNELDL-UHFFFAOYSA-N pyrrolidin-2-one Chemical compound O=C1CCCN1 HNJBEVLQSNELDL-UHFFFAOYSA-N 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- -1 transition metal molybdate Chemical class 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
-
- 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
-
- 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
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
-
- 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
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
Abstract
The invention discloses the invention provides a kind of preparation method of nanoscale cuboid alkali formula copper molybdate.With copper acetate and sodium molybdate as raw material, water and ethylene glycol mixed solution are solvent, step Synthesized by Hydrothermal Method level cuboid alkali formula copper molybdate.The alkali formula copper molybdate of synthesis is about 100nm 300nm, and thickness is about 100nm.The preparation method is simple to operate, and reaction condition is general, can be directly used for industrial-scale production.The alkali formula copper molybdate appearance of nano material stabilization prepared using the present invention, purity is high, and crystallinity is high, and theoretical foundation and practical experience are provided to significantly improve the performances such as its energy storage, catalysis.
Description
【Technical field】
The invention belongs to field of inorganic nano material, it is related to a kind of nanoscale cuboid alkali formula copper molybdate and its preparation side
Method.
【Background technology】
Molybdate micro Nano material is the important functional material of a class, in catalysis, absorption, electromagnetism, sensor, energy storage
There is extensive use Deng field.In inorganic molybdate micro Nano material, transition metal molybdate has because it there is unoccupied orbital
Special crystal structure and catalytic performance receives people and more and more payes attention to.Such as Chinese patent CN201110347395.9
Disclosed with CN201110347508.5 and prepare hyperstructure and radial molybdic acid copper micron ball using microwave reaction
(Cu3Mo2O9), the method reaction time is shorter, but has used microwave reactor, is unfavorable for the industrialization low-coat scale of product
Production, and its product size is larger (5 μm -15 μm), is unfavorable for answering for the characteristics such as such product small-size effect and quantum effect
With, therefore the method still has skill upgrading space at the aspect such as size Control and low cost preparation.Additionally, Chinese patent
CN201410827872.5 and CN201410827892.2 individually disclose supercritical ultrasonics technology combination ultrasound-molten-salt growth method and prepare copper molybdate
Nanometer sheet (CuMoO4) and silver molybdate-molybdic acid copper composite powders preparation method.Such method synthesis step is more, and after reaction
Need to carry out high-temperature post-treatment, therefore such method is improving the aspect such as reaction efficiency and optimum synthesis technique still with certain
Room for improvement.Alkali formula copper molybdate Cu3(OH)2(MO4)2, also known as lindgrenite, it is a kind of rare mineral.At present, closed with artificial means
Do not have into this natural minerals and report on a large scale.Relative to other copper-based molybdates, the pattern of alkali formula copper molybdate is also relatively more single
One, mainly based on micron ball, as Chinese patent CN201510096407.3 discloses a kind of spherical alkali formula copper molybdate of micron
Preparation method, but its product diameter is about 20 μm, and the pH value of accurate adjustment reaction solution is needed in preparation process, therefore should
In size Control and efficiently, the aspect such as preparation still has skill upgrading space to method.
【The content of the invention】
It is an object of the invention to solve above-mentioned problem of the prior art, there is provided a kind of nanoscale cuboid alkali formula copper molybdate
And preparation method thereof, the method simply and easily prepares stable appearance using one step hydro thermal method, and purity is high, and crystallinity is high to be received
Meter level cuboid alkali formula copper molybdate, is adapted to industrial-scale production.
To reach above-mentioned purpose, the present invention is achieved using following technical scheme：
A kind of preparation method of nanoscale cuboid alkali formula copper molybdate, comprises the following steps：
1) mixing for the sodium acetate of the polyvinylpyrrolidone of 10mg and 10mg being added into deionized water and ethylene glycol is molten
In liquid, and stir, obtain mixed liquor；
2) to copper acetate is added in mixed liquor, after stirring, sodium molybdate is added, and is stirred, obtain mixing former
Feed liquid；Wherein, sodium molybdate and copper acetate are according to 1:2 mol ratio is added in mixed liquor；
3) mixed material liquid is transferred in reactor, the hydro-thermal insulation 5h at a temperature of 180 DEG C；
4) room temperature is naturally cooled to after hydro-thermal process terminates, and centrifuge washing is carried out to product with deionized water and ethanol
The removal of impurity, then carries out vacuum drying treatment at a temperature of 80 DEG C, obtains a nanometer cuboid alkali formula copper molybdate.
The present invention is further improved：
The step 1) in, mixing time is 5min.
The step 2) in, copper acetate is added, sodium molybdate is added after stirring 3min, then it is stirred for 10min.
The step 4) in, the volume ratio of deionized water and ethanol is 1:1.
The step 4) in, to product centrifuge washing 5 times going the removal of impurity.
A kind of nanoscale cuboid alkali formula copper molybdate, the length of alkali formula copper molybdate is 100nm~300nm, and width is
100nm, thickness is 100nm.
Compared with prior art, the invention has the advantages that：
The present invention has synthesized nanoscale cuboid alkali formula molybdic acid first using conventional mantoquita and molybdate by a step hydro-thermal
Copper, is formulated simple and practical.The method reaction time is short, and reaction condition is gentle, it is easy to repeat, and is adapted to low-coat scale production.System
For the alkali formula copper molybdate stable appearance for going out, purity is high, and crystallinity is high, and change response parameter easily can also be carried out to its size
Regulation and control are copper molybdate class nano material in energy storage, and the extensive use in the field such as catalysis provides theoretical foundation and practical experience.
【Brief description of the drawings】
Fig. 1 is alkali formula copper molybdate nanometer cuboid low range magnified sweep electron microscope；
Fig. 2 is alkali formula copper molybdate nanometer cuboid high magnification enlarged drawing；
Fig. 3 is alkali formula copper molybdate nanometer cuboid XRD.
【Specific embodiment】
The present invention is described in further detail below in conjunction with the accompanying drawings：
The mixed solution of 40ml deionized waters and ethylene glycol is configured first.Then under electromagnetic agitation, appropriate poly- second is added
Alkene pyrrolidone and sodium acetate, stir 5min.Again under vigorous stirring, after first adding copper acetate stirring 3min, molybdic acid is added
Sodium, continues to stir；After stirring 10min, mixed solution is transferred in 50ml reactors, sealed, in 180 DEG C of hydro-thermal insulation 5h.
After reaction terminates, room temperature is naturally cooled to.Synthesized product, with deionized water and ethanol (volume ratio 1:1) centrifuge washing 5
It is secondary.Remove after impurity, be vacuum dried at 80 DEG C.Final product is absinthe-green nanometer cuboid alkali formula copper molybdate.
Fig. 1 and 2 is that copper molybdate prepared by the present invention receives the scanning electron microscope diagram of cuboid, wherein obtained nanometer material
, in 100-300nm, wide in 100nm, height is in 100nm or so for the length of material.Thing phase composition can be determined by the XRD for observing Fig. 3
It is Cu3(MoO4)2(OH)2。
The present invention completes the preparation of alkali formula copper molybdate using the preparation condition of raw material and simple and effective cheap and easy to get, and
The nanoscale cuboid pattern of novelty is obtained.For the design synthesis of copper-based molybdate nano material provides good theoretical foundation
And practical experience.
Above content is only explanation technological thought of the invention, it is impossible to limit protection scope of the present invention with this, every to press
According to technological thought proposed by the present invention, any change done on the basis of technical scheme each falls within claims of the present invention
Protection domain within.
Claims (5)
1. a kind of preparation method of nanoscale cuboid alkali formula copper molybdate, it is characterised in that comprise the following steps：
1) sodium acetate of the polyvinylpyrrolidone of 10mg and 10mg is added in the mixed solution of deionized water and ethylene glycol,
And stir, obtain mixed liquor；
2) to copper acetate is added in mixed liquor, after stirring, sodium molybdate is added, and is stirred, obtain mixed material liquid；
Wherein, sodium molybdate and copper acetate are according to 1:2 mol ratio is added in mixed liquor；
3) mixed material liquid is transferred in reactor, the hydro-thermal insulation 5h at a temperature of 180 DEG C；
4) room temperature is naturally cooled to after hydro-thermal process terminates, and centrifuge washing is carried out to product with deionized water and ethanol and go removal of impurities
Matter, then carries out vacuum drying treatment at a temperature of 80 DEG C, obtains a nanometer cuboid alkali formula copper molybdate.
2. the preparation method of nanoscale cuboid alkali formula copper molybdate according to claim 1, it is characterised in that the step
1) in, mixing time is 5min.
3. the preparation method of nanoscale cuboid alkali formula copper molybdate according to claim 1, it is characterised in that the step
2) in, copper acetate is added, sodium molybdate is added after stirring 3min, be then stirred for 10min.
4. the preparation method of nanoscale cuboid alkali formula copper molybdate according to claim 1, it is characterised in that the step
4) in, the volume ratio of deionized water and ethanol is 1:1.
5. the preparation method of nanoscale cuboid alkali formula copper molybdate according to claim 1, it is characterised in that the step
4) in, to product centrifuge washing 5 times going the removal of impurity.
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| CN106908497B (en) * | 2017-01-19 | 2018-11-30 | 华南师范大学 | It is a kind of with the heterogeneous optical electro-chemistry sensor for becoming photoelectric activity substance of copper molybdate/barium titanate p-n and its construction method and application |
| CN106904655B (en) * | 2017-03-22 | 2018-08-21 | 陕西科技大学 | A kind of molybdic acid copper nano particles and its preparation method and application |
| CN107221670A (en) * | 2017-06-20 | 2017-09-29 | 扬州大学 | A kind of synthetic method of lithium ion battery negative material nanometer rods |
| CN107382315B (en) * | 2017-06-30 | 2020-10-23 | 武汉工程大学 | Sodium lanthanum molybdate nano material and preparation method thereof |
| CN107570165A (en) * | 2017-09-24 | 2018-01-12 | 柳州若思纳米材料科技有限公司 | A kind of preparation method of copper molybdate photochemical catalyst |
| CN107570164A (en) * | 2017-09-24 | 2018-01-12 | 柳州若思纳米材料科技有限公司 | A kind of preparation method of copper-molybdenum oxide catalyst |
| CN107930574A (en) * | 2017-11-29 | 2018-04-20 | 长沙埃比林环保科技有限公司 | A kind of alkali formula copper tungstate sorbing material and preparation method thereof |
| CN108993362A (en) * | 2018-09-03 | 2018-12-14 | 湖北中澳纳米材料技术有限公司 | A kind of device and method preparing high-purity nm molybdic acid potassium solution |
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| CN104692462A (en) * | 2015-03-04 | 2015-06-10 | 同济大学 | Method for preparing alkali type copper molybdate microsphere having surface nano-whisker structure |
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