CN106698516A - Method for preparing magnesium molybdate nanosheets - Google Patents
Method for preparing magnesium molybdate nanosheets Download PDFInfo
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- CN106698516A CN106698516A CN201611011720.3A CN201611011720A CN106698516A CN 106698516 A CN106698516 A CN 106698516A CN 201611011720 A CN201611011720 A CN 201611011720A CN 106698516 A CN106698516 A CN 106698516A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
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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
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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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
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
Abstract
The invention discloses a method for preparing magnesium molybdate nanosheets. The method comprises the following steps: firstly, dissolving sodium molybdate dehydrate in ethylene glycol so as to prepare a solution A, dissolving magnesium chloride hexahydrate into deionized water so as to prepare a solution B, slowly adding the solution A into the solution B so as to form a uniform mixed solution, stirring, transferring into a reaction kettle, sealing, reacting for hours under a certain temperature condition, naturally cooling to the room temperature, finally, centrifugally washing an obtained product for multiple times by using a mixed solution of deionized water and ethanol, drying overnight so as to obtain cream colored flaky magnesium molybdate, and further performing a one-step hydrothermal reaction, thereby synthesizing flaky magnesium molybdate for the first time. The method is simple and practical in formula, low in cost, easy to repeat, gentle in reaction condition and applicable to low-cost large-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 the important functional material of a class, 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, with important scientific research meaning and are widely applied prospect, and its research is drawn
The very big concern of people is played.Therefore, substantial amounts of effort is devoted to new molybdate (CoMoO always4, FeMoO4, CuMoO4,
NiMoO4Deng) synthesis.As Chinese patent CN 201410827872.5 is disclosed using supercritical ultrasonics technology and ultrasound-molten-salt growth method synthesis
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 is about 50nm, a width of 250*400nm of * long.Ultrasound-molten-salt growth method synthesis can significantly reduce synthesis
Temperature and shortening reaction time, the product thickness prepared are about 100nm, a width of 0.7*2.5 μm of * long.Above two method
Microwave reactor is 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 the method in size Control and
The aspects such as low cost preparation still have skill upgrading space.
Wherein, synthetically prepared little, nano particle, the electrostatic spinning method that only prepared by sintering process being reported of magnesium molybdate
Magnesium molybdate nanometer particle film prepared by the structure of the fibrous web-like of preparation, leaching Tu.Therefore, with special appearance magnesium molybdate
MgMoO4The design synthesis of nano material is still present 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 prepare the magnesium molybdate nanometer sheet that stable appearance, purity are high, crystallinity is high using one step hydro thermal method, be adapted to it is low into
This large-scale production, the characteristics of with simple and convenient, low cost, 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 is as follows：
Step 1：Configuration concentration is the solution A of 0.2-0.5 mol/Ls during Sodium Molybdate Dihydrate is dissolved in into ethylene glycol, by six water
Configuration concentration is 0.2-0.5 mol/L solution Bs during magnesium chloride is dissolved 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 reactor, seals, in 140-
Reacted 5-10 hours under 180 DEG C of temperature conditionss, after reaction terminates, naturally cool 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 do
It is dry overnight, obtain cream-colored flake magnesium molybdate.
Described deionized water and alcohol mixed solution are that volume ratio is 1:1.
The present invention has the advantages that compared with prior art：
The present invention has synthesized sheet magnesium molybdate first using conventional magnesium salts and molybdate by a step hydro-thermal reaction, is formulated
Simple and practical, low cost, it is easy to repeat, reaction condition is gentle, is adapted to low-coat scale production.The sheet magnesium molybdate prepared is thick
It is 35nm to spend, and purity is high, perfect crystalline, and to significantly improve its energy storage, the performance such as catalysis is provided convenience condition.
Brief description of the drawings
Fig. 1 is the XRD 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.
Specific 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
Configuration concentration is 0.5 mol/L solution B 25mL during magnesium chloride is dissolved 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 10 minutes, it is transferred in 50mL reactors, seals, at 180 DEG C
Hydro-thermal 5 hours under temperature conditionss, after reaction terminates, naturally cool to room temperature；
Step 4：By step 3 products therefrom volume ratio 1:1 deionized water and alcohol mixed solution centrifuge washing 5 times,
60 DEG C are dried overnight afterwards, obtain cream-colored flake magnesium molybdate.
Magnesium molybdate thing phase composition can be determined by the XRD for observing Fig. 1, 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
Configuration concentration is 0.2 mol/L solution B 25mL during magnesium chloride is dissolved 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 reactors, seals, at 160 DEG C
Hydro-thermal 10 hours under temperature conditionss, after reaction terminates, naturally cool to room temperature；
Step 4：By step 3 products therefrom volume ratio 1:1 deionized water and alcohol mixed solution centrifuge washing 5 times,
60 DEG C are dried overnight afterwards, obtain 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
Configuration concentration is 0.4 mol/L solution B 25mL during magnesium chloride is dissolved 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 reactors, seals, at 140 DEG C
Hydro-thermal 8 hours under temperature conditionss, after reaction terminates, naturally cool to room temperature；
Step 4：By step 3 products therefrom volume ratio 1:1 deionized water and alcohol mixed solution centrifuge washing 6 times,
60 DEG C are dried overnight afterwards, obtain 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：Configuration concentration is the solution A of 0.2-0.5 mol/Ls during Sodium Molybdate Dihydrate is dissolved in into ethylene glycol, by six water chlorinations
Configuration concentration is 0.2-0.5 mol/L solution Bs during magnesium is dissolved 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 reactor, seals, at 140-180 DEG C
Reacted 5-10 hours under temperature conditionss, after reaction terminates, naturally cool 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 flake magnesium molybdate.
2. a kind of preparation method of magnesium molybdate nanometer sheet according to claim 1, it is characterised in that described 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
Configuration concentration is 0.5 mol/L solution B 25mL during magnesium is dissolved 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 10 minutes, it is transferred in 50mL reactors, seals, in 180 DEG C of temperature
Under the conditions of hydro-thermal 5 hours, after reaction terminates, naturally cool 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 flake 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
Configuration concentration is 0.2 mol/L solution B 25mL during magnesium is dissolved 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 reactors, seals, in 160 DEG C of temperature
Under the conditions of hydro-thermal 10 hours, after reaction terminates, naturally cool 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
Configuration concentration is 0.4 mol/L solution B 25mL during magnesium is dissolved 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 reactors, seals, in 140 DEG C of temperature
Under the conditions of hydro-thermal 8 hours, after reaction terminates, naturally cool 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.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107382315A (en) * | 2017-06-30 | 2017-11-24 | 武汉工程大学 | A kind of lanthanum molybdate sodium 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 |
| CN109761279A (en) * | 2018-12-14 | 2019-05-17 | 辽宁星空钠电电池有限公司 | A kind of rapid precipitation preparation two dimension BaMoO4Method |
| CN110482606A (en) * | 2019-08-16 | 2019-11-22 | 陕西科技大学 | A kind of magnesium molybdate carbon composite nano ball and preparation method thereof |
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| CN104374810A (en) * | 2014-11-14 | 2015-02-25 | 湖北大学 | Method for preparing hydrogen sensitive element based on quadrature-phase molybdenum oxide nano-belt |
| CN104437470A (en) * | 2014-11-06 | 2015-03-25 | 上海市纳米科技与产业发展促进中心 | Homogeneous yolk-shell structure Bi2MoO6 microsphere as well as preparation method and application thereof |
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| CN104437470A (en) * | 2014-11-06 | 2015-03-25 | 上海市纳米科技与产业发展促进中心 | Homogeneous yolk-shell structure Bi2MoO6 microsphere as well as preparation method and application thereof |
| CN104374810A (en) * | 2014-11-14 | 2015-02-25 | 湖北大学 | Method for preparing hydrogen sensitive element based on quadrature-phase molybdenum oxide nano-belt |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107382315A (en) * | 2017-06-30 | 2017-11-24 | 武汉工程大学 | A kind of lanthanum molybdate sodium nano material and preparation method thereof |
| 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 |
| CN109761279A (en) * | 2018-12-14 | 2019-05-17 | 辽宁星空钠电电池有限公司 | A kind of rapid precipitation preparation two dimension BaMoO4Method |
| CN110482606A (en) * | 2019-08-16 | 2019-11-22 | 陕西科技大学 | A kind of magnesium molybdate carbon composite nano ball and preparation method thereof |
| CN110482606B (en) * | 2019-08-16 | 2021-09-24 | 陕西科技大学 | Magnesium molybdate-carbon composite nanospheres and preparation method thereof |
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| CN106698516B (en) | 2018-04-13 |
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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. |
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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. |