CN106698516B - A kind of preparation method of magnesium molybdate nanometer sheet - Google Patents
A kind of preparation method of magnesium molybdate nanometer sheet Download PDFInfo
- Publication number
- CN106698516B CN106698516B CN201611011720.3A CN201611011720A CN106698516B CN 106698516 B CN106698516 B CN 106698516B CN 201611011720 A CN201611011720 A CN 201611011720A CN 106698516 B CN106698516 B CN 106698516B
- Authority
- CN
- China
- Prior art keywords
- solution
- magnesium
- mixed solution
- deionized water
- dissolved
- 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.)
- Active
Links
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
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
Abstract
A kind of preparation method of magnesium molybdate nanometer sheet, Sodium Molybdate Dihydrate is dissolved in ethylene glycol first and configures solution A, magnesium chloride hexahydrate is dissolved in deionized water and configures solution B, then solution A is slowly added into and homogeneous mixed solution is formed in solution B, it is transferred in reaction kettle and seals after stirring, a few hours are reacted under the conditions of certain temperature, cooled to room temperature afterwards, finally, by products therefrom deionized water and alcohol mixed solution centrifuge washing for several times, it is dried overnight afterwards, obtain cream-colored laminar magnesium molybdate, sheet magnesium molybdate has been synthesized by a step hydro-thermal reaction first, it is formulated simple and practical, cost is low, it is easy to repeat, reaction condition is gentle, it is adapted to low-coat scale production.
Description
Technical field
The invention belongs to field of inorganic nano-material preparation, more particularly to a kind of preparation method of magnesium molybdate nanometer sheet.
Background technology
Molybdate is a kind of important functional material, energy storage, catalysis, luminescence generated by light, photonic crystal, scintillator material,
The fields such as magnetic material, light filler material have extensive use.Wherein, nano flake crystal has with its unique structure and is permitted
More unusual physics, the performance such as chemically and electrically, have important scientific research meaning and are widely applied prospect, its research is drawn
The very big concern of people is played.Therefore, it is substantial amounts of to make great efforts to have been devoted to new molybdate (CoMoO4, FeMoO4, CuMoO4,
NiMoO4Deng) synthesis.Supercritical ultrasonics technology and ultrasound-molten-salt growth method synthesis are utilized as Chinese patent CN 201410827872.5 is disclosed
Copper molybdate nanometer sheet antimicrobial powder (Cu3Mo2O9), wherein sonochemistry intermediate processing is mainly short using wavelength and is easy to improve poly-
The characteristics of burnt ability, product thickness are about 50nm, and long * wide is 250*400nm.Ultrasound-molten-salt growth method synthesis can significantly reduce synthesis
Temperature and shortening reaction time, the product thickness prepared are about 100nm, and long * wide is 0.7*2.5 μm.Above two method
Microwave reactor has been used, has been unfavorable for the industrialization low-coat scale production of product, and the larger (50- of its product size thickness
100nm), be unfavorable for the application of the characteristics such as such product small-size effect and quantum effect, thus this method in size Control and
Low cost preparation etc. still has skill upgrading space.
Wherein, synthetically prepared be reported seldom, nano particle that only prepared by sintering process, the electrostatic spinning method of magnesium molybdate
Magnesium molybdate nanometer particle film prepared by the structure of the fibrous web-like of preparation, leaching Tu.Therefore, there is special appearance magnesium molybdate
MgMoO4The design synthesis of nano material still has larger challenge.
The content of the invention
In order to overcome the above-mentioned deficiencies of the prior art, it is an object of the invention to propose a kind of preparation of magnesium molybdate nanometer sheet
Method, can use one step hydro thermal method prepare the magnesium molybdate nanometer sheet that stable appearance, purity are high, crystallinity is high, be adapted to it is low into
This large-scale production, has the characteristics that simple and convenient, cost is low, good product quality.
To achieve these goals, the technical solution adopted by the present invention is：
A kind of preparation method of magnesium molybdate nanometer sheet, step are as follows：
Step 1：Sodium Molybdate Dihydrate is dissolved in the solution A that configuration concentration in ethylene glycol is 0.2-0.5 mol/Ls, by six water
It is 0.2-0.5 mol/L solution Bs that magnesium chloride, which is dissolved in configuration concentration in deionized water,；
Step 2：Under electromagnetic agitation, solution A is slowly added into homogeneous mixed solution is formed in solution B, solution A with
The volume ratio of solution B is 1:1；
Step 3：After step 2 gained mixed solution is stirred 10-15 minutes, it is transferred in reaction kettle, seals, in 140-
When reaction 5-10 is small under 180 DEG C of temperature conditionss, after reaction, cooled to room temperature；
Step 4：By step 3 products therefrom deionized water and alcohol mixed solution centrifuge washing for several times, afterwards 60 DEG C it is dry
It is dry overnight, obtain cream-colored laminar magnesium molybdate.
The deionized water and alcohol mixed solution is that volume ratio is 1:1.
The present invention has the advantages that compared with prior art：
The present invention has been synthesized sheet magnesium molybdate by a step hydro-thermal reaction, has been formulated first using conventional magnesium salts and molybdate
It is simple and practical, cost is low, is easy to repeat, reaction condition is gentle, be adapted to low-coat scale production.The sheet magnesium molybdate prepared is thick
Spend for 35nm, purity is high, crystallization is complete, provides convenience condition to significantly improve the performance such as its energy storage, catalysis.
Brief description of the drawings
Fig. 1 is the XRD diagram of magnesium molybdate nanometer sheet.
Fig. 2 (a) is magnesium molybdate nanometer sheet low range magnified sweep electron microscope, and Fig. 2 (b) is put for magnesium molybdate nanometer sheet high magnification
Expose thoroughly electron microscope.
Embodiment
The present invention is described in further detail with reference to the accompanying drawings and examples.
Embodiment one：
Step 1：Sodium Molybdate Dihydrate is dissolved in the solution A 15mL that configuration concentration in ethylene glycol is 0.5 mol/L, by six water
It is 0.5 mol/L solution B 25mL that magnesium chloride, which is dissolved in configuration concentration in deionized water, is stirred 5 minutes；
Step 2：Under electromagnetic agitation, solution A is slowly added into homogeneous mixed solution is formed in solution B, solution A with
The volume ratio of solution B is 1:1；
Step 3：By the stirring of step 2 gained mixed solution after ten minutes, it is transferred in 50mL reaction kettles, seals, at 180 DEG C
When hydro-thermal 5 is small under temperature conditionss, after reaction, cooled to room temperature；
Step 4：By step 3 products therefrom volume ratio 1:1 deionized water and alcohol mixed solution centrifuge washing 5 times,
It is dried overnight for 60 DEG C afterwards, obtains cream-colored laminar magnesium molybdate.
XRD diagram by observing Fig. 1 can determine magnesium molybdate thing phase composition, and Fig. 2 is molybdenum prepared by the embodiment of the present invention one
The scanning electron microscope diagram of sour magnesium nanometer sheet, the thickness of obtained nano material is in 35nm or so.
Embodiment two：
Step 1：Sodium Molybdate Dihydrate is dissolved in the solution A 15mL that configuration concentration in ethylene glycol is 0.2 mol/L, by six water
It is 0.2 mol/L solution B 25mL that magnesium chloride, which is dissolved in configuration concentration in deionized water, is stirred 5 minutes；
Step 2：Under electromagnetic agitation, solution A is slowly added into homogeneous mixed solution is formed in solution B, solution A with
The volume ratio of solution B is 1:1；
Step 3：After step 2 gained mixed solution is stirred 15 minutes, it is transferred in 50mL reaction kettles, seals, at 160 DEG C
When hydro-thermal 10 is small under temperature conditionss, after reaction, cooled to room temperature；
Step 4：By step 3 products therefrom volume ratio 1:1 deionized water and alcohol mixed solution centrifuge washing 5 times,
It is dried overnight for 60 DEG C afterwards, obtains laminar magnesium molybdate.
Embodiment three：
Step 1：Sodium Molybdate Dihydrate is dissolved in the solution A 15mL that configuration concentration in ethylene glycol is 0.4 mol/L, by six water
It is 0.4 mol/L solution B 25mL that magnesium chloride, which is dissolved in configuration concentration in deionized water, is stirred 5 minutes；
Step 2：Under electromagnetic agitation, solution A is slowly added into homogeneous mixed solution is formed in solution B, solution A with
The volume ratio of solution B is 1:1；
Step 3：After step 2 gained mixed solution is stirred 12 minutes, it is transferred in 50mL reaction kettles, seals, at 140 DEG C
When hydro-thermal 8 is small under temperature conditionss, after reaction, cooled to room temperature；
Step 4：By step 3 products therefrom volume ratio 1:1 deionized water and alcohol mixed solution centrifuge washing 6 times,
It is dried overnight for 60 DEG C afterwards, obtains laminar magnesium molybdate.
Claims (5)
1. a kind of preparation method of magnesium molybdate nanometer sheet, it is characterised in that comprise the following steps：
Step 1：Sodium Molybdate Dihydrate is dissolved in the solution A that configuration concentration in ethylene glycol is 0.2-0.5 mol/Ls, by six water chlorinations
It is 0.2-0.5 mol/L solution Bs that magnesium, which is dissolved in configuration concentration in deionized water,；
Step 2：Under electromagnetic agitation, solution A is slowly added into homogeneous mixed solution, solution A and solution are formed in solution B
The volume ratio of B is 1:1；
Step 3：After step 2 gained mixed solution is stirred 10-15 minutes, it is transferred in reaction kettle, seals, at 140-180 DEG C
When reaction 5-10 is small under temperature conditionss, after reaction, cooled to room temperature；
Step 4：By step 3 products therefrom deionized water and alcohol mixed solution centrifuge washing for several times, afterwards 60 DEG C it is dried
At night, obtain cream-colored laminar magnesium molybdate.
A kind of 2. preparation method of magnesium molybdate nanometer sheet according to claim 1, it is characterised in that the deionized water
It is that volume ratio is 1 with alcohol mixed solution:1.
3. the preparation method of a kind of magnesium molybdate nanometer sheet according to claim 1, it is characterised in that comprise the following steps：
Step 1：Sodium Molybdate Dihydrate is dissolved in the solution A 15mL that configuration concentration in ethylene glycol is 0.5 mol/L, by six water chlorinations
It is 0.5 mol/L solution B 25mL that magnesium, which is dissolved in configuration concentration in deionized water, is stirred 5 minutes；
Step 2：Under electromagnetic agitation, solution A is slowly added into homogeneous mixed solution, solution A and solution are formed in solution B
The volume ratio of B is 1:1；
Step 3：By the stirring of step 2 gained mixed solution after ten minutes, it is transferred in 50mL reaction kettles, seals, in 180 DEG C of temperature
Under the conditions of hydro-thermal 5 it is small when, after reaction, cooled to room temperature；
Step 4：By step 3 products therefrom volume ratio 1:1 deionized water and alcohol mixed solution centrifuge washing 5 times, afterwards
60 DEG C are dried overnight, and obtain cream-colored laminar magnesium molybdate.
4. the preparation method of a kind of magnesium molybdate nanometer sheet according to claim 1, it is characterised in that comprise the following steps：
Step 1：Sodium Molybdate Dihydrate is dissolved in the solution A 15mL that configuration concentration in ethylene glycol is 0.2 mol/L, by six water chlorinations
It is 0.2 mol/L solution B 25mL that magnesium, which is dissolved in configuration concentration in deionized water, is stirred 5 minutes；
Step 2：Under electromagnetic agitation, solution A is slowly added into homogeneous mixed solution, solution A and solution are formed in solution B
The volume ratio of B is 1:1；
Step 3：After step 2 gained mixed solution is stirred 15 minutes, it is transferred in 50mL reaction kettles, seals, in 160 DEG C of temperature
Under the conditions of hydro-thermal 10 it is small when, after reaction, cooled to room temperature；
Step 4：By step 3 products therefrom volume ratio 1:1 deionized water and alcohol mixed solution centrifuge washing 5 times, afterwards
60 DEG C are dried overnight, and obtain laminar magnesium molybdate.
5. the preparation method of a kind of magnesium molybdate nanometer sheet according to claim 1, it is characterised in that comprise the following steps：
Step 1：Sodium Molybdate Dihydrate is dissolved in the solution A 15mL that configuration concentration in ethylene glycol is 0.4 mol/L, by six water chlorinations
It is 0.4 mol/L solution B 25mL that magnesium, which is dissolved in configuration concentration in deionized water, is stirred 5 minutes；
Step 2：Under electromagnetic agitation, solution A is slowly added into homogeneous mixed solution, solution A and solution are formed in solution B
The volume ratio of B is 1:1；
Step 3：After step 2 gained mixed solution is stirred 12 minutes, it is transferred in 50mL reaction kettles, seals, in 140 DEG C of temperature
Under the conditions of hydro-thermal 8 it is small when, after reaction, cooled to room temperature；
Step 4：By step 3 products therefrom volume ratio 1:1 deionized water and alcohol mixed solution centrifuge washing 6 times, afterwards
60 DEG C are dried overnight, and obtain laminar magnesium molybdate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611011720.3A CN106698516B (en) | 2016-11-17 | 2016-11-17 | A kind of preparation method of magnesium molybdate nanometer sheet |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611011720.3A CN106698516B (en) | 2016-11-17 | 2016-11-17 | A kind of preparation method of magnesium molybdate nanometer sheet |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106698516A CN106698516A (en) | 2017-05-24 |
| CN106698516B true CN106698516B (en) | 2018-04-13 |
Family
ID=58939810
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611011720.3A Active CN106698516B (en) | 2016-11-17 | 2016-11-17 | A kind of preparation method of magnesium molybdate nanometer sheet |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106698516B (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107382315B (en) * | 2017-06-30 | 2020-10-23 | 武汉工程大学 | Sodium lanthanum molybdate nano 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 |
| CN109761279B (en) * | 2018-12-14 | 2020-10-09 | 辽宁星空钠电电池有限公司 | Rapid precipitation preparation of two-dimensional BaMoO4Method (2) |
| CN110482606B (en) * | 2019-08-16 | 2021-09-24 | 陕西科技大学 | Magnesium molybdate-carbon composite nanospheres and preparation method thereof |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104437470B (en) * | 2014-11-06 | 2016-11-23 | 上海市纳米科技与产业发展促进中心 | A kind of homogeneity egg yolk-shell structure Bi2moO6microsphere and preparation method thereof, application |
| CN104374810B (en) * | 2014-11-14 | 2017-02-22 | 湖北大学 | Method for preparing hydrogen sensitive element based on quadrature-phase molybdenum oxide nano-belt |
-
2016
- 2016-11-17 CN CN201611011720.3A patent/CN106698516B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN106698516A (en) | 2017-05-24 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106698516B (en) | A kind of preparation method of magnesium molybdate nanometer sheet | |
| Ma et al. | Microwave synthesis of cellulose/CuO nanocomposites in ionic liquid and its thermal transformation to CuO | |
| CN106904655B (en) | A kind of molybdic acid copper nano particles and its preparation method and application | |
| Zheng et al. | Customized dielectric-magnetic balance enhanced electromagnetic wave absorption performance in CuxS/CoFe2O4 composites | |
| CN106064832B (en) | A kind of nanoscale cuboid alkali formula copper molybdate and preparation method thereof | |
| CN106099063A (en) | A kind of Hydrothermal Synthesis metal-oxide/graphene nanocomposite material and its preparation method and application | |
| CN104876257B (en) | A kind of preparation method of water solublity cadmiumsulfide quantum dot | |
| CN107670672B (en) | A kind of barium titanate composite sulfur cadmium nano composite photo-catalyst and preparation method thereof | |
| CN107337237A (en) | A kind of copper molybdate and preparation method thereof | |
| CN103232058A (en) | Method for preparing copper sulphide/graphene nano-composite material | |
| CN108585018A (en) | A kind of size is less than the Cu of 100nm2The preparation method of O nanospheres | |
| CN105000588A (en) | Preparation method for water-soluble copper sulphide quantum dots | |
| CN104860345B (en) | A kind of preparation method of water-soluble stannous sulfide quantum dot | |
| CN104817104B (en) | A kind of preparation method of water solublity copper sulfide zinc quantum dot | |
| CN105664921B (en) | A kind of nanometer W0.4Mo0.6O3The preparation method of high-performance optical catalyst | |
| CN102179526A (en) | Method for preparing cubic crystal nano silver material by oil-water interface method | |
| CN102786075B (en) | Preparation method of flower-like nanometer copper oxide powder | |
| CN105060346A (en) | Preparation method of molybdenum trioxide nanobelt colloid automatically and stably dispersed in water | |
| Song et al. | Low-temperature molten salt synthesis and characterization of CoWO4 nano-particles | |
| CN101805009A (en) | Simple and controllable method for preparing lobate micron/nano copper oxide two-dimensional assembly | |
| CN107452865B (en) | Gold nanoparticle-coated nanosheet structure Sb2Te3Method for manufacturing thermoelectric material | |
| CN103056385B (en) | CTAB is the method for oil-water interfaces legal system for oil-soluble nano silver of surfactant | |
| CN116037954B (en) | Gold iridium core-shell nanowire and preparation method thereof | |
| CN104445340A (en) | Method for preparing octahedral cerium oxide self-assembled by nano blocks | |
| CN104925870A (en) | Solvothermal method for preparing nano-grade ferroferric oxide |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20221226 Address after: 230000 B-1015, wo Yuan Garden, 81 Ganquan Road, Shushan District, Hefei, Anhui. Patentee after: HEFEI MINGLONG ELECTRONIC TECHNOLOGY Co.,Ltd. Address before: 710021 Shaanxi province Xi'an Weiyang university campus of Shaanxi University of Science and Technology Patentee before: SHAANXI University OF SCIENCE & TECHNOLOGY |
|
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20230424 Address after: 246000 No. 8 Dangui Road, Daguan Economic Development Zone, Anqing City, Anhui Province Patentee after: Anqing Bike Flame Retardant Technology Co.,Ltd. Address before: 230000 B-1015, wo Yuan Garden, 81 Ganquan Road, Shushan District, Hefei, Anhui. Patentee before: HEFEI MINGLONG ELECTRONIC TECHNOLOGY Co.,Ltd. |
|
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20230621 Address after: 246000 No. 8 Dangui Road, Fenghuang Circular Economy Industrial Park, Daguan District, Anqing City, Anhui Province Patentee after: Anqing YueTong Molybdenum Industry Co.,Ltd. Address before: 246000 No. 8 Dangui Road, Daguan Economic Development Zone, Anqing City, Anhui Province Patentee before: Anqing Bike Flame Retardant Technology Co.,Ltd. |