CN104495932A - Method for solid-phase chemical reaction synthesis of nano molybdenum trioxide - Google Patents
Method for solid-phase chemical reaction synthesis of nano molybdenum trioxide Download PDFInfo
- Publication number
- CN104495932A CN104495932A CN201410695183.3A CN201410695183A CN104495932A CN 104495932 A CN104495932 A CN 104495932A CN 201410695183 A CN201410695183 A CN 201410695183A CN 104495932 A CN104495932 A CN 104495932A
- Authority
- CN
- China
- Prior art keywords
- nano
- solid
- solid state
- ammonium molybdate
- chemical reaction
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
- C01G39/02—Oxides; Hydroxides
-
- 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
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The invention aims to provide a preparation method for solid-phase chemical reaction synthesis of nano molybdenum oxide; the method adopts mild and controllable reaction conditions and an operation method having the advantages of simple and easy implementation and green environmental protection, and the nano-scale molybdenum trioxide material can be obtained through a simple solid-phase chemical reaction. On a basis of the solid-phase chemical reaction, common and easily available raw materials are adopted, a nano-sized precursor is obtained through a simple solid-solid chemical reaction, and the precursor is calcined to obtain the nano molybdenum trioxide. Because of the characteristics of simple preparation method, simple and convenient operation, high product yield, short process flow, simple equipment, and easy realization of large-scale production, the preparation method has extremely broad actual application prospects.
Description
Technical field
The present invention relates to a kind of method of solid state reaction synthesis of nano molybdic oxide.
Background technology
Molybdic oxide (MoO
3) be white or pale yellow rhomboidal crystal, common crystalline structure has three kinds: monoclinic phase (p-MoO
3), six side's phase (h-MoO
3) and orthorhombic phase (a-MoO
3).The former two is thermodynamically metastable phases, and the latter is thermodynamically stable phase under room temperature.But the essentially consist unit of above-mentioned three kinds of phase structures is the [MoO of distortion
6] octahedra.Wherein stable state MoO
3(a-MoO
3) crystalline structure belong to rhombic system, lattice parameter a=0.395nrn, b=l.381nm, c=0.369nm.Each [MoO in crystal
6] unit in one direction altogether limit be connected, summit is connected altogether in the other directions, forms the plane layer that a two dimension infinitely stretches, and this layer is double wave shape and perpendicular to b axle along exhibition.Orthorhombic phase MoO
3unique laminate structure can increase avtive spot and be conducive to entering and desorption of gas molecule, and this laminate structure is rarely found in metal oxide.
Nano material has the physical influences such as special small-size effect, quantum size effect, macro quanta tunnel effect, surface effects, these special effectses make nano material have the physics different from stock size material, chemical property, and nano material is with a wide range of applications in fields such as optical material, gas sensitive, electrode materials, catalytic material, magneticsubstances.Nano level molybdic oxide, as the oxide compound of transition metal, compared to industry molybdenum trioxide, has stronger catalytic activity, photoelectric characteristic, solidity to corrosion etc., is more conducive to its application in catalytic material, sensitive material, battery material etc.; Nano level molybdic oxide has tempting using value because it field such as to pretend in information displaying and storage, intelligence in addition, also more and more receives the concern of people.
At present, the synthetic method of nano-sized molybdenum oxide mainly contains the methods such as hydrothermal method, solvent-thermal method, sol-gel method, vapour deposition process, template, chemical precipitation method, ion exchange method.All building-up process is complicated mostly for these methods, and cost is high, and requirement for experiment condition is harsh, realizes large-scale commercial production and there is larger difficulty; And traditional high temperature solid-state method is high higher to equipment requirements because consuming energy, also bring inconvenience and difficulty to carrying out large-scale commercial production.Therefore, select a kind of simple and reliable, technical process is short, and the preparation method of environmental protection prepares nano-sized molybdenum oxide tool is of great significance.Solid-state chemical reaction method method step is simple, and reaction time is short and have highly selective, high yield, the advantages such as environmental pollution is little, has become a kind of simple method obtaining nano material.
Summary of the invention
The object of the present invention is to provide a kind of method of solid state reaction synthesis of nano molybdic oxide, the method is by using raw material simple and easy to get, adopt simple and feasible working method, gentle controlled reaction conditions, synthesizes nano-sized molybdenum oxide through solid state reaction.
Presoma, as reactant, at room temperature by solid state reaction synthesis of nano presoma, then is carried out calcining and can obtain nano-sized molybdenum oxide by the present invention's ammonium molybdate and organic acid.
Organic acid of the present invention is oxalic acid, phenylformic acid, Padil and citric acid.Compared with prior art, the present invention has the following advantages: adopt raw material cheap and easy to get, by simply grinding and calcination process, just can obtain nano-sized molybdenum oxide.Because preparation method of the present invention is simple, reaction conditions gentle controlled, product yield is high, environmental friendliness, be easy to realize the outstanding features such as production in enormous quantities and make the present invention have very wide application prospect.
Accompanying drawing explanation
Fig. 1 is the powder X-ray ray diffraction collection of illustrative plates of the nano-sized molybdenum oxide of orthorhombic phase prepared by first embodiment of the invention.(in figure, PDF#35-0609 is the X ray diffraction data of the molybdic oxide of orthorhombic phase).
Fig. 2 is the field emission scanning electron microscope photo of the nano-sized molybdenum oxide of orthorhombic phase prepared by first embodiment of the invention.
Embodiment
Below in conjunction with specific embodiment, the present invention is further elaborated.These embodiments are interpreted as only being not used in for illustration of the present invention limiting the scope of the invention.After having read the content that the present invention records, the various change made the present invention based on principle of the present invention or amendment have fallen into claims of the present invention limited range equally.
Embodiment one:
Precise 0.01 mol ammonium molybdate is placed in agate mortar porphyrize, add the oxalic acid of 0.03 mol porphyrize again, ground by this solid-phase reaction system after 30 minutes and at room temperature leave standstill after 3 days, at 300 DEG C, calcining obtains the nano-sized molybdenum oxide of metastable monoclinic phase and six side's phases for two hours; And at 500 DEG C, calcine the nano-sized molybdenum oxide obtaining stable orthorhombic phase after two hours.
Embodiment two:
Precise 0.01 mol ammonium molybdate is placed in agate mortar porphyrize, add the phenylformic acid of 0.06 mol porphyrize again, ground by this solid-phase reaction system after 40 minutes and at room temperature leave standstill after 4 days, at 300 DEG C, calcining obtains the nano-sized molybdenum oxide of metastable monoclinic phase and six side's phases for two hours; And at 500 DEG C, calcine the nano-sized molybdenum oxide obtaining stable orthorhombic phase after two hours.
Embodiment three:
Precise 0.01 mol ammonium molybdate is placed in agate mortar porphyrize, add the citric acid of 0.02 mol porphyrize again, ground by this solid-phase reaction system after 50 minutes and at room temperature leave standstill after 5 days, at 300 DEG C, calcining obtains the nano-sized molybdenum oxide of metastable monoclinic phase and six side's phases for two hours; And at 500 DEG C, calcine the nano-sized molybdenum oxide obtaining stable orthorhombic phase after two hours.
Embodiment four:
Precise 0.01 mol ammonium molybdate is placed in agate mortar porphyrize, add the Padil of 0.03 mol porphyrize again, ground by this solid-phase reaction system after 50 minutes and at room temperature leave standstill after 5 days, at 300 DEG C, calcining obtains the nano-sized molybdenum oxide of metastable monoclinic phase and six side's phases for two hours; And at 500 DEG C, calcine the nano-sized molybdenum oxide obtaining stable orthorhombic phase after two hours.
Claims (4)
1. the method for a solid state reaction synthesis of nano molybdic oxide, it comprises the following steps: after ammonium molybdate and organic acid being weighed according to certain stoichiometric ratio, at ambient temperature, carry out the presoma that solid state reaction obtains nano-scale in agate mortar, then presoma is carried out in retort furnace calcining under certain temperature and obtain nano-sized molybdenum oxide.
2. according to the method for a kind of solid state reaction synthesis of nano molybdic oxide described in claim 1, it is characterized in that: the organic acid used is oxalic acid, one in phenylformic acid, citric acid and Padil.
3. according to the method for a kind of solid state reaction synthesis of nano molybdic oxide described in claim 1, it is characterized in that: ammonium molybdate and organic acid stoichiometric ratio are ammonium molybdate and oxalic acid be 1:3, ammonium molybdate and phenylformic acid be 1:6, ammonium molybdate and citric acid be 1:2, ammonium molybdate and Padil is 1:3.
4. according to the method for a kind of solid state reaction synthesis of nano molybdic oxide described in claim 1, it is characterized in that: solid state reaction product calcines the nano-sized molybdenum oxide obtaining metastable monoclinic phase and six side's phases for two hours in retort furnace at 300 DEG C, and in retort furnace, at 500 DEG C, calcine the nano-sized molybdenum oxide obtaining stable orthorhombic phase for two hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410695183.3A CN104495932A (en) | 2014-11-27 | 2014-11-27 | Method for solid-phase chemical reaction synthesis of nano molybdenum trioxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410695183.3A CN104495932A (en) | 2014-11-27 | 2014-11-27 | Method for solid-phase chemical reaction synthesis of nano molybdenum trioxide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104495932A true CN104495932A (en) | 2015-04-08 |
Family
ID=52937412
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410695183.3A Pending CN104495932A (en) | 2014-11-27 | 2014-11-27 | Method for solid-phase chemical reaction synthesis of nano molybdenum trioxide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104495932A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105384194A (en) * | 2015-12-23 | 2016-03-09 | 新疆大学 | Method for synthesizing rare-earth doped nano molybdenum trioxide gas-sensing material through solid-phase chemical reaction |
| CN110217823A (en) * | 2019-05-27 | 2019-09-10 | 燕山大学 | Obtain the preparation method of the molybdenum trioxide of rhombic form and monoclinic form |
| CN112076716A (en) * | 2020-09-04 | 2020-12-15 | 江西善纳新材料科技有限公司 | Composite phase nano molybdenum trioxide adsorbent and preparation method thereof |
| WO2021060375A1 (en) * | 2019-09-24 | 2021-04-01 | Dic株式会社 | Molybdenum trioxide powder and method for producing same |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102351250A (en) * | 2011-07-21 | 2012-02-15 | 北京化工大学 | One-dimensional molybdenum oxide nano rod gas-sensitive material, preparation method and application thereof |
-
2014
- 2014-11-27 CN CN201410695183.3A patent/CN104495932A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102351250A (en) * | 2011-07-21 | 2012-02-15 | 北京化工大学 | One-dimensional molybdenum oxide nano rod gas-sensitive material, preparation method and application thereof |
Non-Patent Citations (2)
| Title |
|---|
| 杨爽: ""三氧化钼一维纳米材料的制备、性能及器件研究"", 《全国优秀硕士学位论文全文数据库 工程科技I辑》, no. 6, 15 June 2014 (2014-06-15) * |
| 王晓毅: ""一维氧化钨和氧化钼的制备及应用研究"", 《中国优秀硕士学位论文全文数据库 工程科技I辑》, no. 1, 15 December 2011 (2011-12-15) * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105384194A (en) * | 2015-12-23 | 2016-03-09 | 新疆大学 | Method for synthesizing rare-earth doped nano molybdenum trioxide gas-sensing material through solid-phase chemical reaction |
| CN110217823A (en) * | 2019-05-27 | 2019-09-10 | 燕山大学 | Obtain the preparation method of the molybdenum trioxide of rhombic form and monoclinic form |
| CN110217823B (en) * | 2019-05-27 | 2020-04-21 | 燕山大学 | Preparation method for obtaining orthorhombic or monoclinic molybdenum trioxide |
| WO2021060375A1 (en) * | 2019-09-24 | 2021-04-01 | Dic株式会社 | Molybdenum trioxide powder and method for producing same |
| JPWO2021060375A1 (en) * | 2019-09-24 | 2021-04-01 | ||
| JP7056807B2 (en) | 2019-09-24 | 2022-04-19 | Dic株式会社 | Molybdenum trioxide powder and its manufacturing method |
| TWI815040B (en) * | 2019-09-24 | 2023-09-11 | 日商迪愛生股份有限公司 | Molybdenum trioxide powder and manufacturing method thereof |
| CN112076716A (en) * | 2020-09-04 | 2020-12-15 | 江西善纳新材料科技有限公司 | Composite phase nano molybdenum trioxide adsorbent and preparation method thereof |
| CN112076716B (en) * | 2020-09-04 | 2023-03-03 | 江西善纳新材料科技有限公司 | Composite phase nano molybdenum trioxide adsorbent and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102580721B (en) | Method for preparing TiO2/BiVO4 composite photocatalyst by MH method | |
| CN102010004B (en) | Method for preparing vanadium disulphide nano powder | |
| CN110354867A (en) | A kind of Zn0.2Cd0.8The preparation method of S/rGO catalysis material | |
| CN104495932A (en) | Method for solid-phase chemical reaction synthesis of nano molybdenum trioxide | |
| CN103395837B (en) | Preparation method of Bi12TiO20 powder | |
| CN103359773B (en) | A kind of preparation method of zinc oxide nano rod | |
| CN104445402B (en) | The preparation method of the barium oxide of different valence state, crystal formation and pattern | |
| CN102153142B (en) | Molybdenum trioxide nanosheet and preparation method thereof | |
| CN104261472A (en) | Vanadium pentoxide nanobelt, and room-temperature synthesis method and application of vanadium pentoxide nanobelt | |
| CN102874874A (en) | Preparation method and application of multistage-structured flower-shaped molybdenum trioxide | |
| CN103864142B (en) | Single stage method prepares the method for anatase phase titanium dioxide nano-wire array | |
| CN102826597A (en) | Method for preparing nanometer titanium dioxide | |
| CN103318954B (en) | Method for preparing sodium trititanate nanorods through solid-phase chemical reaction | |
| CN102651470B (en) | Method for preparing whisker shaped lithium titanate (Li4Ti5O12) by low-temperature solid phase method | |
| CN104628263A (en) | Method for preparing indium oxide octahedral nanocrystal film | |
| CN103274458A (en) | One-dimensional necklace-shaped titanium dioxide nanocrystal and preparation method thereof | |
| CN103566925B (en) | A kind of preparation method of rear-earth-doped mesoporous pucherite | |
| Pang et al. | Polymorphs of Nb2O5 Compound and Their Electrical Energy Storage Applications | |
| CN103833080A (en) | Preparation method for cadmium molybdate porous spheres | |
| CN104477869A (en) | Method for synthesizing bismuth phosphate nano particles by room-temperature solid-phase chemical method | |
| CN104843804B (en) | Carbon-coated cobalt oxide and simple controllable preparation method thereof | |
| CN107500363A (en) | A kind of preparation method of prism hexa-prism nano-sized iron oxide | |
| CN103427076B (en) | A kind of solid state reaction prepares TiO2the method of-B nano material | |
| Ji et al. | Unexpected phase transformation from VO 2 (R) to VO 2 (A) during hydrothermal treatment in the V 2 O 5–H 2 C 2 O 4–H 2 O system | |
| CN105970281B (en) | A kind of simple preparation method of cadmium vanadate monocrystal nanowire |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20150408 |
|
| RJ01 | Rejection of invention patent application after publication |