CN108940259A - A kind of porous MoO of hierarchical structure2Photochemical catalyst microballoon and preparation method thereof - Google Patents
A kind of porous MoO of hierarchical structure2Photochemical catalyst microballoon and preparation method thereof Download PDFInfo
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- CN108940259A CN108940259A CN201810236398.7A CN201810236398A CN108940259A CN 108940259 A CN108940259 A CN 108940259A CN 201810236398 A CN201810236398 A CN 201810236398A CN 108940259 A CN108940259 A CN 108940259A
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- 239000003054 catalyst Substances 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 54
- 239000000243 solution Substances 0.000 claims abstract description 41
- 238000007146 photocatalysis Methods 0.000 claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims abstract description 19
- 239000011259 mixed solution Substances 0.000 claims abstract description 13
- QXYJCZRRLLQGCR-UHFFFAOYSA-N molybdenum(IV) oxide Inorganic materials O=[Mo]=O QXYJCZRRLLQGCR-UHFFFAOYSA-N 0.000 claims description 21
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 238000000889 atomisation Methods 0.000 claims description 6
- 239000003595 mist Substances 0.000 claims description 4
- 238000004458 analytical method Methods 0.000 claims description 3
- 230000008859 change Effects 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 17
- 230000001699 photocatalysis Effects 0.000 abstract description 16
- 238000005507 spraying Methods 0.000 abstract description 15
- 238000013019 agitation Methods 0.000 abstract description 9
- 230000008569 process Effects 0.000 abstract description 8
- 230000008901 benefit Effects 0.000 abstract description 3
- 239000004005 microsphere Substances 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 230000010148 water-pollination Effects 0.000 abstract description 3
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 2
- 239000000446 fuel Substances 0.000 abstract description 2
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 2
- 239000002904 solvent Substances 0.000 abstract description 2
- 238000003911 water pollution Methods 0.000 abstract 1
- 238000002485 combustion reaction Methods 0.000 description 13
- 238000005245 sintering Methods 0.000 description 12
- 238000001816 cooling Methods 0.000 description 8
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 6
- 229960000907 methylthioninium chloride Drugs 0.000 description 6
- 239000006199 nebulizer Substances 0.000 description 6
- 238000010792 warming Methods 0.000 description 6
- 238000005303 weighing Methods 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 5
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 5
- 229940043267 rhodamine b Drugs 0.000 description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 230000001681 protective effect Effects 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000009841 combustion method Methods 0.000 description 2
- 238000005049 combustion synthesis Methods 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 150000002894 organic compounds Chemical class 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical group [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 230000026676 system process Effects 0.000 description 1
Classifications
-
- 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
-
- B01J35/39—
-
- B01J35/51—
-
- B01J35/651—
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
Abstract
A kind of porous MoO of hierarchical structure2Photochemical catalyst microballoon and preparation method thereof belongs to photochemical catalyst microballoon and preparation method thereof.Porous MoO of the invention2Photochemical catalyst microballoon is made of porous shell and internal netted porous skeleton；For the method using citric acid as fuel, ammonium paramolybdate is raw material, and water is solvent, is configured to mixed solution through magnetic agitation, and then solution is sprayed onto 400~500 DEG C of tube furnace by ullrasonic spraying, and the hollow porous MoO of hierarchical structure is prepared2Photochemical catalyst microballoon.Preparation system of the invention has many advantages, such as that process is easy to operate, and raw material is cheap and economically feasible.Prepared by the method catalyst has special hierarchical structure, but also there is hollow porous shape characteristic, partial size is tiny, be evenly distributed soilless sticking, microsphere diameter is between 0.5~2 μm, photocatalysis performance is good, and hydrophily is good, is conducive to the application in fields such as photocatalysis, water pollution processing, lithium ion battery, supercapacitor, gas sensors.
Description
Technical field
The present invention relates to a kind of photochemical catalyst microballoon and preparation method thereof, especially a kind of porous MoO of hierarchical structure2Light is urged
Agent microballoon and preparation method thereof
Background technique
Photocatalysis oxidation technique is considered as one of the most promising technology for solving problem of environmental pollution.So far
Until, it has been found that there are more than 3000 kinds of organic compounds difficult to degrade that can degrade rapidly by photochemical catalytic oxidation.It is urged in light
In the common semiconductor of change technology, MoO2Preparation cost relative moderate, and have lower crystallization and growth temperature, be easy to make
Standby multiplicity pattern and structure, and cause people and more and more pay close attention to.But MoO2Preparation difficulty it is higher, preparing
MoO is easily oxidized in journey3, reduce its purity, and MoO2There is also solar energy utilization ratio is low and current-carrying in practical applications
The high problem of sub- recombination rate.Currently, the method mainly used has pattern control, building multiple to further increase photocatalysis performance
Zoarium is, doping and auxiliary agent surface are modified etc..
For traditional conductor oxidate catalysis material, the modification by the appearance and size to catalyst is to improve light
The most simple effective method of catalytic performance.Currently, control MoO2The preparation method of pattern has very much, wherein solution combustion is closed
At being most widely used one of the method for preparing catalyst of most study.Solution combustion method belongs to wet chemical synthesis, it is utilized
External energy induces reactant and chemically reacts, and the heat released promotes to react the automatic spreading in the form of combustion wave, tool
Have the advantages that preparation process is simple, synthesis temperature is low, the time is short and synthetic powder size is small.The synthetic technology mainly passes through adjusting
The release heat of combustion process and its rate regulate and control the performances such as the object phase composition of synthetic powder, particle size, microscopic appearance.So
And the above method is because there are preparation temperature is uncontrollable, and the catalyst prepared is easy to reunite, recycling rate of waterused is poor, and solution is caused to fire
Burnt together at catalyst photocatalysis performance it is poor, limit the application of photocatalysis technology in actual production.
Because solution combustion synthesis is that the heat released by organic compound combustion carries out to maintain to react, most
Research work is all to concentrate on influence of the selection to product morphology of organic-fuel.But regardless of which kind of organic matter selected, finally
What is obtained is all serious foam-like oxide powder of reuniting, and the influence to product morphology is little.
Summary of the invention
In view of the foregoing drawbacks, the purpose of the present invention is to provide a kind of porous MoO of hierarchical structure2Photochemical catalyst microballoon and its
Preparation method solves existing solution combustion method and is difficult to prepare MoO2Catalyst, temperature is uncontrollable, easy to reunite, and recycling rate of waterused is poor
The problem of.
The object of the present invention is achieved like this, comprising: porous MoO2Photochemical catalyst microballoon and porous MoO2Photochemical catalyst
The preparation method of microballoon.
The porous MoO2Photochemical catalyst microballoon is made of porous shell and internal netted porous skeleton.
The porous MoO2The diameter of photochemical catalyst microballoon is 0.5~2 μm.
The porous MoO2The netted porous bore dia in the inside of photochemical catalyst microballoon is 50~200nm.
The porous MoO2The preparation method of photochemical catalyst microballoon, comprising the following steps:
Step 1, configuration solution: ammonium paramolybdate and citric acid are added in water, magnetic agitation is configured to mixed solution；Its
Middle water 10mL；1.5~2.5mmol of ammonium paramolybdate；1~3mmol of citric acid；Wherein, the purity of the ammonium paramolybdate is
99.6%；The purity of citric acid is that analysis is pure；The water is deionized water.
The configured mixed solution of step 1 is placed in ultrasonic atomizer by step 2, will be mixed by ultrasonic atomizer molten
Liquid mist；The mixed solution of atomization is blown into tubular heater by air, and air carries the flow of the mixed solution of atomization
For 20~40 mL/h；Porous MoO is obtained in the outlet end of tube furnace2Photochemical catalyst microballoon.
The tube furnace has work lumen, and the input end for the lumen that works has threeway, and one end is passed through to work lumen, one end
It is connect with the output end of ultrasonic atomizer, one end is connect with air output end；There is heating device outside work lumen, work lumen
Middle position temperature be 400~500 DEG C, the temperature at both ends is room temperature；The outlet end of work lumen is products export.
Beneficial effect, as the above scheme is adopted, in solution, water as solvent, ammonium paramolybdate is molybdenum source, and citric acid is combustion
Material；By configured solution by ultrasonic atomizer, sprayed into the rate of 20~40mL/h into 400~500 DEG C of tube furnace,
Entire spray process carries out in air atmosphere, and ammonium paramolybdate generates tiny under the reduction of citric acid in combustion process
MoO2Nano particle, furnace cooling after the completion of burning, in cooling procedure, nano particle are constituted in microsphere surface accumulative crystallization
Hierarchical structure ultimately produces porous MoO2Photochemical catalyst microballoon.
The combining ullrasonic spraying with solution combustion of the invention, reduces the reunion between catalyst, system
For porous oxide evenly dispersed out, through being roughly calculated, 10mL solution is atomized into countless 1 μm of drops by ullrasonic spraying,
It is equivalent to and solution is refined as 239,000,000,000 reaction members, this will greatly improve the rate and homogenization degree of reaction, will be ultrasonic
The spraying preparation combined with solution combustion for photochemical catalyst, there is presently no what is synthesized about ullrasonic spraying solution combustion
Report.
The porous MoO of hierarchical structure that ullrasonic spraying synthetic method of solution burning of the invention is prepared2Microballoon, and it is traditional
Solution combustion synthesis is compared, and the synthesis of ullrasonic spraying solution combustion because solution is with ultra-fine droplet form presence, faster more fill by reaction
Point, the catalyst prepared is not easy to reunite, also has hierarchical structure and porous special appearance.
(1) solution combustion is refine to by micron level by ullrasonic spraying, it is molten compared to ullrasonic spraying compared with conventional solution burning
The reaction time of liquid burning is shorter more sufficiently, and the microscopic dimensions of product are smaller and not easy to reunite, and hydrophily is more preferable.
(2) under the conditions of not adding comburant, solution combustion reaction will not occur for ammonium paramolybdate, and the present invention is by solution mist
Change to micron level, shorten the distance of Reaction-diffusion terms, so that some reactions for being difficult to synthesize by solution combustion can be by super
It is prepared by sound spray solution conbustion synthesis.
(3) MoO prepared by2With hierarchical structure and porous special appearance, the catalyst Heterosis of this structure
: hierarchical structure can be more advantageous to transporting for substance on the basis of keeping nanostructure characteristic；Porous structure can be improved
The selectivity of catalyst improves reaction rate, provides more low coordination atoms and promotes catalysis, increases the scattering and absorption of light.
Advantage: preparation system process of the invention is easy to operate, and raw material is cheap and economically feasible.It is made using the present invention
Standby photochemical catalyst microballoon has special hierarchical structure, but also has hollow porous shape characteristic, and partial size is tiny, distribution
Uniform soilless sticking, for microsphere diameter between 0.5~2 μm, photocatalysis performance is good, and hydrophily is good, is conducive in photocatalysis, water
The application in the fields such as pollution processing, lithium ion battery, supercapacitor, gas sensor.
Detailed description of the invention
Fig. 1 is preparation process schematic diagram of the present invention；
Fig. 2 is the porous MoO of the present invention2The object phase composition XRD diagram of photochemical catalyst microballoon；
The MoO that Fig. 3 (a) is prepared under the conditions of being 400 DEG C2SEM figure；
The MoO that Fig. 3 (b) is prepared under the conditions of being 500 DEG C2SEM figure；
Fig. 3 (c) is the partial enlarged view of Fig. 3 (a)；
Fig. 3 (d) is the partial enlarged view of Fig. 3 (b)；
Fig. 4 (a) is with the methylene blue of 30mg/L and rhodamine B；
The MoO that Fig. 4 (b) is measured using the methylene blue of 30mg/L as pollutant2With commercially available TiO2Photocatalysis curve graph.
Specific embodiment
As shown in Figure 1, the porous MoO of hierarchical structure of the invention2Photochemical catalyst microballoon includes:
The porous MoO2Photochemical catalyst microballoon is made of porous shell and internal netted porous skeleton.
The porous MoO2The diameter of photochemical catalyst microballoon is 0.5~2 μm.
The porous MoO2The netted porous bore dia in the inside of photochemical catalyst microballoon is 50~200nm.
A kind of porous MoO2The preparation method of photochemical catalyst microballoon the following steps are included:
Step 1, configuration solution: ammonium paramolybdate and citric acid are added in water, magnetic agitation is configured to mixed solution；Its
Middle water 10mL；1.5~2.5mmol of ammonium paramolybdate；1~3mmol of citric acid；Wherein, the purity of the ammonium paramolybdate is
99.6%；The purity of citric acid is that analysis is pure；The water is deionized water.
The configured mixed solution of step 1 is placed in ultrasonic atomizer by step 2, will be mixed by ultrasonic atomizer molten
Liquid mist；The mixed solution of atomization is blown into tubular heater by air, and air carries the flow of the mixed solution of atomization
For 20~40 mL/h；Porous MoO is obtained in the outlet end of tube furnace2Photochemical catalyst microballoon.
As shown in Fig. 2, the tube furnace has work lumen, the input end for the lumen that works has threeway, and one end is passed through to work
Make lumen, the output end connection of one end and ultrasonic atomizer, one end is connect with air output end；There is heating to fill outside work lumen
It sets, the middle position temperature for the lumen that works is 400~500 DEG C, and the temperature at both ends is room temperature；The outlet end of work lumen is product
Outlet.
Technical solution of the invention is further described below by some embodiments, but these embodiments cannot understand
To be the limitation to technical solution.
Embodiment 1: weighing 1.5mmol ammonium paramolybdate respectively, and 1mmol citric acid is dissolved in 10mL deionized water, room
The lower magnetic agitation 1h of temperature, then configured solution is moved in ultrasonic nebulizer, tube furnace is warming up to 400 DEG C in advance, so
Afterwards by solution with the rate ullrasonic spraying of 20mL/h into tube furnace, entire sintering process is completed in air atmosphere, is not needed
Protective gas, about 1 μm of diameter of porous MoO can be obtained in furnace cooling after the completion of sintering2Photochemical catalyst microballoon.
The MoO prepared under the conditions of 400 DEG C of attached drawing 3 (a)2SEM figure and Fig. 3 (a) partial enlarged view Fig. 3 (c) shown in.
The MoO prepared under the conditions of 400 DEG C of attached drawing 4 (a)2To methylene blue photocatalysis curve, (b) to rhodamine B photocatalysis curve and with
Commercial TiO2Photocatalysis performance comparison.
Embodiment 2: weighing 2mmol ammonium paramolybdate respectively, and 2mmol citric acid is dissolved in 10mL deionized water, room temperature
Lower magnetic agitation 1h, then moves to configured solution in ultrasonic nebulizer, tube furnace is warming up to 400 DEG C in advance, then
By solution with the rate ullrasonic spraying of 30mL/h into tube furnace, entire sintering process is completed in air atmosphere, does not need to protect
Gas is protected, about 1.5 μm of diameter of porous MoO can be obtained in furnace cooling after the completion of sintering2Photochemical catalyst microballoon.
The MoO prepared under the conditions of 400 DEG C of attached drawing 3 (a)2SEM figure and Fig. 3 (a) partial enlarged view Fig. 3 (c) shown in.
The MoO prepared under the conditions of 400 DEG C of attached drawing 4 (a)2To methylene blue photocatalysis curve, (b) to rhodamine B photocatalysis curve and with
Commercial TiO2Photocatalysis performance comparison.
Embodiment 3: weighing 2.5mmol ammonium paramolybdate respectively, and 3mmol citric acid is dissolved in 10mL deionized water, room
The lower magnetic agitation 1h of temperature, then configured solution is moved in ultrasonic nebulizer, tube furnace is warming up to 450 DEG C in advance, so
Afterwards by solution with the rate ullrasonic spraying of 40mL/h into tube furnace, entire sintering process is completed in air atmosphere, is not needed
Protective gas, about 2 μm of diameter of porous MoO can be obtained in furnace cooling after the completion of sintering2Photochemical catalyst microballoon.
Embodiment 4: weighing 1.5mmol ammonium paramolybdate respectively, and 1mmol citric acid is dissolved in 10mL deionized water, room
The lower magnetic agitation 1h of temperature, then configured solution is moved in ultrasonic nebulizer, tube furnace is warming up to 450 DEG C in advance, so
Afterwards by solution with the rate ullrasonic spraying of 20mL/h into tube furnace, entire sintering process is completed in air atmosphere, is not needed
Protective gas, about 1 μm of diameter of porous MoO can be obtained in furnace cooling after the completion of sintering2Photochemical catalyst microballoon.
Embodiment 5: weighing 2mmol ammonium paramolybdate respectively, and 2mmol citric acid is dissolved in 10mL deionized water, room temperature
Lower magnetic agitation 1h, then moves to configured solution in ultrasonic nebulizer, tube furnace is warming up to 500 DEG C in advance, then
By solution with the rate ullrasonic spraying of 30mL/h into tube furnace, entire sintering process is completed in air atmosphere, does not need to protect
Gas is protected, about 1.5 μm of diameter of porous MoO can be obtained in furnace cooling after the completion of sintering2Photochemical catalyst microballoon.
The MoO prepared under the conditions of 500 DEG C of attached drawing 3 (b)2SEM figure and Fig. 3 (b) partial enlarged view Fig. 3 (d) shown in.
The MoO prepared under the conditions of 500 DEG C of attached drawing 4 (a)2To methylene blue photocatalysis curve, (b) to rhodamine B photocatalysis curve and with
Commercial TiO2Photocatalysis performance comparison.
Embodiment 6: weighing 2.5mmol ammonium paramolybdate respectively, and 3mmol citric acid is dissolved in 10mL deionized water, room
The lower magnetic agitation 1h of temperature, then configured solution is moved in ultrasonic nebulizer, tube furnace is warming up to 500 DEG C in advance, so
Afterwards by solution with the rate ullrasonic spraying of 40mL/h into tube furnace, entire sintering process is completed in air atmosphere, is not needed
Protective gas, about 2 μm of diameter of porous MoO can be obtained in furnace cooling after the completion of sintering2Photochemical catalyst microballoon.
The MoO prepared under the conditions of 500 DEG C of attached drawing 3 (b)2SEM figure and Fig. 3 (b) partial enlarged view Fig. 3 (d) shown in.
The MoO prepared under the conditions of 500 DEG C of attached drawing 4 (a)2To methylene blue photocatalysis curve, (b) to rhodamine B photocatalysis curve and with
Commercial TiO2Photocatalysis performance comparison.
Claims (4)
1. a kind of porous MoO of hierarchical structure2Photochemical catalyst microballoon, it is characterized in that: porous MoO2Photochemical catalyst microballoon is by porous
Shell and internal netted porous skeleton are constituted.
2. the porous MoO of hierarchical structure according to claim 12Photochemical catalyst microballoon, it is characterized in that: porous MoO2Photocatalysis
The diameter of agent microballoon is 1 ~ 2 μm.
3. the porous MoO of hierarchical structure according to claim 12Photochemical catalyst microballoon, it is characterized in that: porous MoO2Photocatalysis
The netted porous bore dia in the inside of agent microballoon is 50 ~ 200 nm.
4. a kind of prepare the porous MoO of hierarchical structure described in claim 12The preparation method of photochemical catalyst microballoon, it is characterised in that:
Porous MoO2The preparation method of photochemical catalyst microballoon, comprising the following steps:
Step 1, configuration solution: ammonium paramolybdate and citric acid are added in water, solution is made, wherein 10 mL of water；Ammonium paramolybdate
1.5~2.5 mmol；1 ~ 3 mmol of citric acid；Wherein, the purity of the ammonium paramolybdate is 99.6%；The purity of citric acid is point
It analyses pure；The water is deionized water；
Step 2, by step 1 configured mixed solution merging ultrasonic atomizer, by ultrasonic atomizer by mixed solution mist
Change；The mixed solution of atomization is blown into tubular heater by air, air carry atomization mixed solution flow be 20 ~
40 mL/h；Porous MoO is obtained in the outlet end of tube furnace2Photochemical catalyst microballoon；
The tube furnace has work lumen, and the input end for the lumen that works has a threeway, and one end is passed through to work lumen, one end and super
The output end of sound atomizer connects, and one end is connect with air output end；There is heating device outside work lumen, in the lumen that works
Between position temperature be 400 ~ 500 DEG C, the temperature at both ends is room temperature；The outlet end of work lumen is products export.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114849692A (en) * | 2022-04-14 | 2022-08-05 | 三峡大学 | TiO 2 2 -C-MoO 2 Preparation method and application of nano composite material |
Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7438948B2 (en) * | 2005-03-21 | 2008-10-21 | Ppg Industries Ohio, Inc. | Method for coating a substrate with an undercoating and a functional coating |
| CN101475146A (en) * | 2009-01-19 | 2009-07-08 | 华中师范大学 | Universal method for synthesizing metallic oxide hollow sphere by H3BO3 induced ultrasonic atomization |
| CN103145198A (en) * | 2013-03-08 | 2013-06-12 | 南昌大学 | Method for producing nanometer structure cobalt tetroxide sub-micron hollow balls |
| CN103894211A (en) * | 2014-04-09 | 2014-07-02 | 莆田学院 | Multi-metal sulfide semiconductor photocatalytic material and preparation method thereof |
| CN104150536A (en) * | 2014-08-06 | 2014-11-19 | 徐州工程学院 | Preparation method and application of MoO2 powder with favorable photoelectric properties |
| CN105366726A (en) * | 2015-12-16 | 2016-03-02 | 中国科学院理化技术研究所 | Preparation method of hollow spherical molybdenum disulfide of laminated shell layer structure |
| CN105561976A (en) * | 2015-12-17 | 2016-05-11 | 西安交通大学 | Preparation method of Bi2WO6 microspheres with visible light activity |
| CN106745194A (en) * | 2016-12-15 | 2017-05-31 | 西安航空学院 | The preparation method of ZnO hollow Nano particles |
| CN107221643A (en) * | 2017-06-28 | 2017-09-29 | 福建师范大学 | A kind of ultrasonic atomizatio preparation method of the spherical tertiary cathode material of porous hollow |
| CN107275635A (en) * | 2017-06-28 | 2017-10-20 | 福建师范大学 | A kind of ultrasonic atomizatio preparation method of the spherical tertiary cathode material of porous hollow |
| CN107285384A (en) * | 2017-07-20 | 2017-10-24 | 西安理工大学 | A kind of preparation method of flower-shaped molybdenum dioxide nanometer powder |
-
2018
- 2018-03-21 CN CN201810236398.7A patent/CN108940259B/en active Active
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7438948B2 (en) * | 2005-03-21 | 2008-10-21 | Ppg Industries Ohio, Inc. | Method for coating a substrate with an undercoating and a functional coating |
| CN101475146A (en) * | 2009-01-19 | 2009-07-08 | 华中师范大学 | Universal method for synthesizing metallic oxide hollow sphere by H3BO3 induced ultrasonic atomization |
| CN103145198A (en) * | 2013-03-08 | 2013-06-12 | 南昌大学 | Method for producing nanometer structure cobalt tetroxide sub-micron hollow balls |
| CN103894211A (en) * | 2014-04-09 | 2014-07-02 | 莆田学院 | Multi-metal sulfide semiconductor photocatalytic material and preparation method thereof |
| CN104150536A (en) * | 2014-08-06 | 2014-11-19 | 徐州工程学院 | Preparation method and application of MoO2 powder with favorable photoelectric properties |
| CN105366726A (en) * | 2015-12-16 | 2016-03-02 | 中国科学院理化技术研究所 | Preparation method of hollow spherical molybdenum disulfide of laminated shell layer structure |
| CN105561976A (en) * | 2015-12-17 | 2016-05-11 | 西安交通大学 | Preparation method of Bi2WO6 microspheres with visible light activity |
| CN106745194A (en) * | 2016-12-15 | 2017-05-31 | 西安航空学院 | The preparation method of ZnO hollow Nano particles |
| CN107221643A (en) * | 2017-06-28 | 2017-09-29 | 福建师范大学 | A kind of ultrasonic atomizatio preparation method of the spherical tertiary cathode material of porous hollow |
| CN107275635A (en) * | 2017-06-28 | 2017-10-20 | 福建师范大学 | A kind of ultrasonic atomizatio preparation method of the spherical tertiary cathode material of porous hollow |
| CN107285384A (en) * | 2017-07-20 | 2017-10-24 | 西安理工大学 | A kind of preparation method of flower-shaped molybdenum dioxide nanometer powder |
Non-Patent Citations (1)
| Title |
|---|
| H. CHOI等: ""Continuous synthesis of molybdenum oxide microspheres by ultrasonic spray pyrolysis"", 《JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114849692A (en) * | 2022-04-14 | 2022-08-05 | 三峡大学 | TiO 2 2 -C-MoO 2 Preparation method and application of nano composite material |
| CN114849692B (en) * | 2022-04-14 | 2023-10-27 | 三峡大学 | TiO (titanium dioxide) 2 -C-MoO 2 Preparation method and application of nanocomposite |
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