CN109502647A - A kind of preparation method of molybdenum oxide bouquet - Google Patents
A kind of preparation method of molybdenum oxide bouquet Download PDFInfo
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- CN109502647A CN109502647A CN201710844209.XA CN201710844209A CN109502647A CN 109502647 A CN109502647 A CN 109502647A CN 201710844209 A CN201710844209 A CN 201710844209A CN 109502647 A CN109502647 A CN 109502647A
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- molybdenum oxide
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- 229910000476 molybdenum oxide Inorganic materials 0.000 title claims abstract description 19
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- 239000007788 liquid Substances 0.000 claims description 36
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 14
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 238000006243 chemical reaction Methods 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000012153 distilled water Substances 0.000 claims description 12
- 239000000047 product Substances 0.000 claims description 8
- 235000019270 ammonium chloride Nutrition 0.000 claims description 7
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 claims description 7
- 238000013019 agitation Methods 0.000 claims description 6
- 229940116298 l- malic acid Drugs 0.000 claims description 6
- 239000012046 mixed solvent Substances 0.000 claims description 6
- 230000020477 pH reduction Effects 0.000 claims description 6
- 239000012265 solid product Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims description 2
- 239000005751 Copper oxide Substances 0.000 claims description 2
- 229910000431 copper oxide Inorganic materials 0.000 claims description 2
- 235000018660 ammonium molybdate Nutrition 0.000 claims 1
- 239000011609 ammonium molybdate Substances 0.000 claims 1
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims 1
- 229940010552 ammonium molybdate Drugs 0.000 claims 1
- 235000015393 sodium molybdate Nutrition 0.000 claims 1
- 239000011684 sodium molybdate Substances 0.000 claims 1
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 7
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 2
- 230000005622 photoelectricity Effects 0.000 abstract description 2
- 239000002086 nanomaterial Substances 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- 238000003911 water pollution Methods 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000001632 sodium acetate Substances 0.000 description 1
- 235000017281 sodium acetate Nutrition 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- -1 therefore 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
- C01G39/02—Oxides; Hydroxides
-
- 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
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/24—Chromium, molybdenum or tungsten
- B01J23/28—Molybdenum
-
- 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
- B01J35/39—Photocatalytic properties
-
- 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
- C01P2004/32—Spheres
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
A kind of preparation method of molybdenum oxide bouquet obtains acquisition size using hydro-thermal method method and is distributed uniform molybdenum oxide bouquet.This method is easy to operate, quick, safe operation, at low cost, reproducible.Molybdenum oxide bouquet obtained in this method air-sensitive, photoelectricity, solar battery, in terms of have huge application prospect.
Description
Technical field
The invention belongs to micro Nano material synthesis technical fields, and in particular to a kind of hydro-thermal method synthesis molybdenum oxide bouquet and its
Preparation method.The uniform molybdenum oxide bouquet of morphology and size is obtained, which is expected to further apply light-catalyzed reaction.
Background technique
With the fast development of human society, water resource pollution is got worse, therefore how effectively to solve water pollution problems
At countries in the world focus of attention.Wherein waste water from dyestuff is an important pollution sources of water pollution.In recent years, semiconductor is utilized
Nano material is as photochemical catalyst, harmful organic substance molecule in catalytic degradation waste water from dyestuff, as one to curb environmental pollution
The effective method of kind is studied extensively by environment scholar both domestic and external.Conductor photocatalysis degradation technique is because having high-efficient, energy consumption
It is low, easy to operate, reaction condition is mild, use scope is wide, reusable and can reduce the outstanding features such as secondary pollution, in ring
By the favor of people in terms of the pollution control of border.
Molybdenum oxide is a kind of novel semiconductor material, and forbidden bandwidth is 3.15~3.3eV, has high electric conductivity, good
Good uv absorption property and strong chemical stability, are widely used in the fields such as air-sensitive, photoelectricity, solar battery, sensor.
Currently, mostly can be the compound with semiconductor property with photocatalyst, therefore, copper oxide answering in terms of photocatalysis
With increasingly attracting people's attention.
Summary of the invention
The present invention provides a kind of simple processes, the synthetic method of molybdenum oxide nano material at low cost, as follows
It carries out:
(1) suitable molybdate, D are weighed, L MALIC ACID is added in 20mL distilled water, and electromagnetic agitation 30min obtains A liquid；
(2) 2mmol ammonium chloride is weighed, 20ml mixed solvent is added and obtains B liquid；
(3) B liquid is added dropwise in A liquid, stirs 30min, added the hydrochloric acid acidification 30min of 2ml 3mol/l, obtain C
Liquid；
(4) it measures 20ml liquid to be put into 20ml reaction kettle, maintains the temperature at 160 DEG C of standing 6h；
(5) solid product obtained in reaction kettle is washed with distilled water 3 times, then with ethanol washing 2 times, obtains product guarantor
60 DEG C are held, dry 8h obtains molybdenum oxide nanometer bouquet.
The present invention is raw material using sodium acetate and ammonium chloride, and the pattern of product, tool are adjusted using hydrochloric acid and surfactant
There is the features such as equipment is simple, easy to operate, is advantageously implemented large-scale industrial production.What more importantly the present invention obtained receives
Popped rice ball molybdenum oxide has very bigger serface, has excellent performance in terms of photocatalysis.
Detailed description of the invention
Fig. 1 is scanning electron microscope prepared by example 1 (SEM) photo.
Fig. 2 is X ray diffracting spectrum prepared by example 1.
Specific embodiment
The present invention will be described in further detail below with reference to the embodiments of the drawings.
Embodiment 1:
A kind of preparation method of molybdenum oxide nanometer bouquet, includes the following steps:
(1) suitable molybdate, D are weighed, L MALIC ACID is added in 20mL distilled water, and electromagnetic agitation 30min obtains A liquid；
(2) 2mmol ammonium chloride is weighed, 20ml mixed solvent is added and obtains B liquid；
(3) B liquid is added dropwise in A liquid, stirs 30min, added the hydrochloric acid acidification 30min of 2ml 3mol/l, obtain C
Liquid；
(4) it measures 20ml liquid to be put into 20ml reaction kettle, maintains the temperature at 160 DEG C of standing 6h；
(5) solid product obtained in reaction kettle is washed with distilled water 3 times, then with ethanol washing 2 times, obtains product guarantor
60 DEG C are held, dry 8h obtains molybdenum oxide nanometer bouquet.
Embodiment 2:
(1) suitable molybdate, D are weighed, L MALIC ACID is added in 20mL distilled water, and electromagnetic agitation 30min obtains A liquid；
(2) 2mmol ammonium chloride is weighed, 20ml mixed solvent is added and obtains B liquid；
(3) B liquid is added dropwise in A liquid, stirs 30min, added the hydrochloric acid acidification 30min of 2ml 3mol/l, obtain C
Liquid；
(4) it measures 20ml liquid to be put into 20ml reaction kettle, maintains the temperature at 160 DEG C of standing 8h；
(5) solid product obtained in reaction kettle is washed with distilled water 3 times, then with ethanol washing 2 times, obtains product guarantor
60 DEG C are held, dry 8h obtains molybdenum oxide nanometer bouquet.
Embodiment 3:
(1) suitable molybdate, D are weighed, L MALIC ACID is added in 20mL distilled water, and electromagnetic agitation 30min obtains A liquid；
(2) 2mmol ammonium chloride is weighed, 20ml mixed solvent is added and obtains B liquid；
(3) B liquid is added dropwise in A liquid, stirs 30min, added the hydrochloric acid acidification 30min of 2ml 3mol/l, obtain C
Liquid；
(4) it measures 20ml liquid to be put into 20ml reaction kettle, maintains the temperature at 160 DEG C of standing 10h；
(5) solid product obtained in reaction kettle is washed with distilled water 3 times, then with ethanol washing 2 times, obtains product guarantor
60 DEG C are held, dry 8h obtains molybdenum oxide nanometer bouquet.
Embodiment 4:
(1) suitable molybdate, D are weighed, L MALIC ACID is added in 20mL distilled water, and electromagnetic agitation 30min obtains A liquid；
(2) 2mmol ammonium chloride is weighed, 20ml mixed solvent is added and obtains B liquid；
(3) B liquid is added dropwise in A liquid, stirs 30min, added the hydrochloric acid acidification 30min of 2ml 3mol/l, obtain C
Liquid；
(4) it measures 20ml liquid to be put into 20ml reaction kettle, maintains the temperature at 160 DEG C of standing 4h；
(5) solid product obtained in reaction kettle is washed with distilled water 3 times, then with ethanol washing 2 times, obtains product guarantor
60 DEG C are held, dry 8h obtains molybdenum oxide nanometer bouquet.
Claims (3)
1. a kind of preparation method of copper oxide microballoon, it is characterized by including the following steps:
(1) suitable molybdate, D are weighed, L MALIC ACID is added in 20mL distilled water, and electromagnetic agitation 30min obtains A liquid；
(2) 2mmol ammonium chloride is weighed, 20ml mixed solvent is added and obtains B liquid；
(3) B liquid is added dropwise in A liquid, stirs 30min, added the hydrochloric acid acidification 30min of 2ml 3mol/l, obtain C liquid；
(4) it measures 20ml liquid to be put into 20ml reaction kettle, maintains the temperature at 160 DEG C of standing 6h；
(5) solid product obtained in reaction kettle is washed with distilled water 3 times, then with ethanol washing 2 times, obtains product and keeps 60
DEG C, dry 8h obtains molybdenum oxide nanometer bouquet.
2. by the preparation method of molybdenum oxide bouquet described in claim 1, it is characterized in that: water solubility described in the step (1)
Molybdate can be sodium molybdate, ammonium molybdate.
3. being pure molybdenum oxide bouquet by the resulting product of claim 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710844209.XA CN109502647A (en) | 2017-09-14 | 2017-09-14 | A kind of preparation method of molybdenum oxide bouquet |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710844209.XA CN109502647A (en) | 2017-09-14 | 2017-09-14 | A kind of preparation method of molybdenum oxide bouquet |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109502647A true CN109502647A (en) | 2019-03-22 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710844209.XA Pending CN109502647A (en) | 2017-09-14 | 2017-09-14 | A kind of preparation method of molybdenum oxide bouquet |
Country Status (1)
| Country | Link |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102557138A (en) * | 2011-12-27 | 2012-07-11 | 江西稀有金属钨业控股集团有限公司 | Method for preparing molybdenum trioxide |
| CN106976909A (en) * | 2017-01-19 | 2017-07-25 | 青岛科技大学 | A kind of hexagonal phase h MoO3The preparation method and photocatalytic applications of micron bar |
-
2017
- 2017-09-14 CN CN201710844209.XA patent/CN109502647A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102557138A (en) * | 2011-12-27 | 2012-07-11 | 江西稀有金属钨业控股集团有限公司 | Method for preparing molybdenum trioxide |
| CN106976909A (en) * | 2017-01-19 | 2017-07-25 | 青岛科技大学 | A kind of hexagonal phase h MoO3The preparation method and photocatalytic applications of micron bar |
Non-Patent Citations (4)
| Title |
|---|
| YI SHEN ET AL.: "Hydrothermal deposition and the photochromic properties of molybdenum oxide hydrate (MoO3▪ (H2O)0.69) films induced by D, L-malic acid", 《JOURNAL OF ALLOYS AND COMPOUNDS》 * |
| YUELI LIU ET AL.: "Hydrothermal synthesis of h-MoO3 microrods and their gas sensingproperties to ethanol", 《APPLIED SURFACE SCIENCE》 * |
| ZHIRI YU ET AL.: "Synthesis of MoO3 nanostructures and their photocatalytic properties", 《ADVANCED MATERIALS RESEARCH》 * |
| 蔡万玲等: "MoO2 纳米球的水热合成与光催化性能", 《西南大学学报(自然科学版)》 * |
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