CN105152214A - Device and method for producing spherical molybdenum trioxide powder - Google Patents
Device and method for producing spherical molybdenum trioxide powder Download PDFInfo
- Publication number
- CN105152214A CN105152214A CN201510633528.7A CN201510633528A CN105152214A CN 105152214 A CN105152214 A CN 105152214A CN 201510633528 A CN201510633528 A CN 201510633528A CN 105152214 A CN105152214 A CN 105152214A
- Authority
- CN
- China
- Prior art keywords
- refrigerant
- communicated
- spherical
- room
- molybdic oxide
- 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.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
- C01G39/02—Oxides; Hydroxides
-
- 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
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25B—REFRIGERATION MACHINES, PLANTS OR SYSTEMS; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS
- F25B39/00—Evaporators; Condensers
- F25B39/04—Condensers
-
- 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
- B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
- B01J2208/00796—Details of the reactor or of the particulate material
- B01J2208/00946—Features relating to the reactants or products
- B01J2208/00955—Sampling of the particulate material, the reactants or the products
- B01J2208/00964—Reactants
-
- 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
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25B—REFRIGERATION MACHINES, PLANTS OR SYSTEMS; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS
- F25B2339/00—Details of evaporators; Details of condensers
- F25B2339/04—Details of condensers
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Dispersion Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Mechanical Engineering (AREA)
- Thermal Sciences (AREA)
- General Engineering & Computer Science (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention provides a device for producing spherical molybdenum trioxide powder. The device for producing the spherical molybdenum trioxide powder comprises a compressed air storage tank, a resistance furnace, a condenser and a cloth bag collector which are communicated in sequence. A compressed air outlet is formed in the compressed air storage tank. A first air inlet is formed in the lower portion of the resistance furnace, a first exhaust port is formed in the upper portion of the resistance furnace, a condensation chamber is formed inside the condenser, a second air inlet is formed in the lower portion of the condensation chamber, a second exhaust port is formed in the upper portion of the condensation chamber, a condensation product collection chamber is formed at the bottom of the condensation chamber, the condenser is communicated with a refrigerator, and a third air inlet is formed in the cloth bag collector. The invention further provides a method for producing the spherical molybdenum trioxide powder by utilizing the device. Spherical high-purity fine-grained molybdenum trioxide is produced by adopting a sublimation and desublimation method, the device is ingenious in design, the requirement for the production device is low, the molybdenum trioxide is fine-grained and spherical in morphology, product consistency is good, and the spherical molybdenum trioxide powder is suitable for large-scale production.
Description
Technical field
The invention belongs to molybdenum Chemicals preparing technical field, be specifically related to a kind of device and method preparing spherical molybdic oxide powder.
Background technology
Molybdic oxide is a kind of important molybdenum Chemicals, but also is the main raw material of Mo powder production, is used as catalyzer in the oil industry, also can be used for enamel glaze pigment and medicine etc.The preparation method of molybdic oxide is a lot, mainly comprises the precipitator method, hydrothermal method, chemical Vapor deposition process, gel casting forming method, sol-gel method etc.The molybdic oxide of different-shape can be prepared at present by above different methods, comprising: threadiness, crystal whisker-shaped, flake, bar-shaped, wire, fine granularity pipe, fine granularity band, spherical etc.In the molybdenum trioxide material of above-mentioned pattern, the spherical molybdic oxide of fine granularity, owing to having polymolecularity and high-specific surface area, can improve the catalytic performance of catalyzer greatly, makes it have very large application prospect at catalyst industry.In addition, the spherical molybdic oxide of fine granularity can be used for the spherical IF-MoS of class synthesizing ultralow friction coefficient
2material.
The preparation method of the spherical molybdic oxide of current fine granularity is mainly template and sonochemical method, and preparation method is loaded down with trivial details, and reaction soln digestion time is 12h, is unfavorable for that industrialization promotion is produced.By comparison, take industrial molybdenum oxide as raw material, the preparation method adopting subliming method to prepare sphericalshaped fine-grain degree molybdic oxide can yet be regarded as a kind of easy, quick, technique of having larger industrial applications prospect.
At present, adopt though have the research of legal system for high-purity molybdenum trioxide that distils-sublimate both at home and abroad, made molybdic oxide is needle-like structures.Up to now, about adopting the method that distils-sublimate to prepare, crystal formation is unified, there is not been reported in the correlative study of complete spherical molybdic oxide.
Summary of the invention
Technical problem to be solved by this invention is for above-mentioned the deficiencies in the prior art, provides a kind of device preparing spherical molybdic oxide powder.This device passes into the pressurized air of certain flow in resistance furnace exit, be used for the molybdic oxide gas after preliminary cooling distillation on the one hand, be used for the flue gas of transfer line on the other hand, compressed-air actuated input can guarantee the molybdic oxide flue gas dispersion entering condenser, prevent mutual collision from growing up into other patterns gradually, finally can obtain the spherical molybdic oxide that crystal formation is unified, complete.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of device preparing spherical molybdic oxide powder, is characterized in that, comprises the compressed air reservoir, resistance furnace, condenser and the cloth bag collector that are communicated with successively;
Described compressed air reservoir is provided with compressed air outlet, the bottom of described resistance furnace is provided with the first inlet mouth, the top of described resistance furnace is provided with first row gas port, condensing chamber is provided with in described condenser, the bottom of described condensing chamber is provided with the second inlet mouth, the top of described condensing chamber is provided with second exhaust port, the bottom of described condensing chamber is provided with condensate collection chamber, described condenser with for providing the refrigerator of refrigerant to be communicated with to it, described cloth bag collector is provided with the 3rd inlet mouth;
Described compressed air outlet is communicated with the first channel of the first three-way piece, the second passage of described first three-way piece is communicated with the first inlet mouth by the first gas flow adjuster, the third channel of described first three-way piece is communicated with the first channel of the second three-way piece by the second gas flow adjuster, the second passage of described second three-way piece is communicated with first row gas port, the third channel of described second three-way piece is communicated with the second inlet mouth, and described second exhaust port is communicated with the 3rd inlet mouth.
Above-mentioned a kind of device preparing spherical molybdic oxide powder, it is characterized in that, described condensing chamber periphery is surrounded with the first refrigerant room, described first bottom, refrigerant room is provided with the first refrigerant input aperture, described first top, refrigerant room is provided with the first refrigerant delivery port, described first refrigerant input aperture is communicated with the refrigerant output terminal of the first refrigerator, and described first refrigerant delivery port is communicated with the refrigerant input terminus of the first refrigerator.
Above-mentioned a kind of device preparing spherical molybdic oxide powder, it is characterized in that, the top of described condensing chamber is provided with the second refrigerant room, described second refrigerant room comprises the second refrigerant input room and the second refrigerant exports room, described second refrigerant input top, room is provided with the second refrigerant input aperture, described second refrigerant exports top, room and is provided with the second refrigerant delivery port, described second refrigerant input aperture is communicated with the refrigerant output terminal of the second refrigerator, and described second refrigerant delivery port is communicated with the refrigerant input terminus of the second refrigerator;
Also be provided with the second refrigerant input tube in described condensing chamber and be sleeved on the second refrigerant output tube outside the second refrigerant input tube, the both ends open of described second refrigerant input tube, wherein one end and the second refrigerant input room and are communicated with, the other end is positioned at the second refrigerant output tube, one end of described second refrigerant output tube is closed, and the other end and the second refrigerant export room and be communicated with.
Above-mentioned a kind of device preparing spherical molybdic oxide powder, is characterized in that, be movably set with and cut somebody's hair in described condensing chamber, described in cut somebody's hair and to be connected with cylinder by push rod.
Above-mentioned a kind of device preparing spherical molybdic oxide powder, is characterized in that, described cloth bag collector is provided with induced draft fan.
Above-mentioned a kind of device preparing spherical molybdic oxide powder, it is characterized in that, in described cloth bag collector, the material of cloth bag is glass or terylene.
In addition, present invention also offers a kind of method utilizing said apparatus to prepare spherical molybdic oxide powder, it is characterized in that, the method comprises the following steps:
Step one, quartz sand uniform spreading to be located in material boat, then molybdenum raw material uniform spreading to be located on quartz sand; Described molybdenum raw material is molybdenum powder, industrial molybdenum oxide or high-purity molybdenum trioxide;
Step 2, the material boat being equipped with quartz sand and molybdenum raw material in step one is placed in resistance furnace, then compressed air reservoir is utilized to pass into pressurized air in resistance furnace, and utilize the first gas flow adjuster and the second gas flow adjuster to regulate compressed-air actuated flow, under compressed-air actuated flow after regulating through the first gas flow adjuster and the compressed-air actuated flow after the second gas flow adjuster regulates are the condition of 1L/min ~ 10L/min, being incubated 2h after temperature in resistance furnace being risen to 800 DEG C ~ 1050 DEG C makes molybdenum raw material be gaseous state by solid state sublimation, be elevated gas,
Step 3, sublimation gases described in step 2 is passed in condensing chamber, then adopt air, water or liquid nitrogen to sublimate process to sublimation gases as refrigerant, in collecting chamber and cloth bag collector, all obtain the spherical molybdenum trioxide powder that granularity is 0.02 μm ~ 1.5 μm.
Above-mentioned method, is characterized in that, in high-purity molybdenum trioxide described in step one, the mass percentage of molybdic oxide is not less than 99.95%.
The present invention compared with prior art has the following advantages:
1, the preparation method of the spherical molybdic oxide of fine granularity provided by the present invention, molybdenum raw material can adopt industrial molybdenum oxide, high-purity molybdenum trioxide, molybdenum powder etc.Compared with the preparation method of the high-purity molybdenum trioxide of routine, the pattern of the made molybdic oxide of the present invention is that fine granularity is spherical, and the consistence of product is good; And method of the present invention is less demanding to production unit, is suitable for scale operation.
2, the present invention is by passing into the pressurized air of certain flow in resistance furnace exit, be used for the molybdic oxide gas after preliminary cooling distillation on the one hand, be used for the flue gas of transfer line on the other hand, compressed-air actuated input can guarantee the molybdic oxide flue gas dispersion entered in condenser, prevent mutual collision from growing up into other patterns gradually, become the Important Action that spherical molybdic oxide is formed.
3, the present invention have developed a kind of many media condenser with quenching effect, for the formation of spherical molybdic oxide provides guarantee, can ensure below the dispersed molybdic oxide flue gas very fast cooling down to de-sublimation temperature that enters.
4, the power adjustment that the pressurized air that the present invention is passed into by resistance furnace bottom is carried mainly as flue gas.
5, the present invention can adopt the multiple mediums such as water, air, liquid nitrogen as cooling medium, only just need can prepare the molybdic oxide of different crystal morphology by changing cooling medium, comprising: the patterns such as spherical, faller gill shape.
6, process of the test of the present invention is all carried out at normal pressure, and simple equipments, preparation technology are brief, efficient, are suitable for suitability for industrialized production.
7, the molybdenum raw material in the present invention can adopt industrial molybdenum oxide, high-purity molybdenum trioxide, molybdenum powder etc. containing molybdenum product, if this technique adopts quality purity to be not less than 99.95% high-purity molybdenum trioxide, regulated by technology controlling and process of the present invention, the molybdenum trioxide product that quality purity is not less than 99.99% can be prepared, be applicable to industrialization scale operation.
Below in conjunction with drawings and Examples, the present invention is described in further detail.
Accompanying drawing explanation
Fig. 1 is the structural representation that the present invention prepares the device of spherical molybdic oxide powder.
Fig. 2 is the structural representation of condenser of the present invention.
Fig. 3 is the SEM photo of molybdic oxide powder prepared by the embodiment of the present invention 2.
Fig. 4 is the SEM photo of molybdic oxide powder prepared by the embodiment of the present invention 4.
Fig. 5 is the TEM photo of molybdic oxide powder prepared by the embodiment of the present invention 5.
Fig. 6 is the SEM photo of molybdic oxide powder prepared by the embodiment of the present invention 6.
Fig. 7 is the SEM photo of the molybdic oxide powder of comparative example 1 of the present invention preparation.
Fig. 8 is the SEM photo of the molybdic oxide powder of comparative example 2 of the present invention preparation.
Description of reference numerals:
1-compressed air reservoir; 1-1-compressed air outlet; 2-resistance furnace;
2-1-the first inlet mouth; 2-2-first row gas port; 3-condenser;
3-1-condensing chamber; 3-2-the first refrigerant room; 3-3-the second refrigerant input room;
3-4-the second refrigerant exports room; 3-5-condensate collection chamber; 3-6-the second refrigerant input tube;
3-7-the second refrigerant output tube; 3-8-the second inlet mouth; 3-9-the second air outlet;
3-10-the first refrigerant input aperture; 3-11-the first refrigerant delivery port; 3-12-the second refrigerant input aperture;
3-13-the second refrigerant delivery port; 3-14-cut somebody's hair; 3-15-push rod;
3-16-cylinder; 4-cloth bag collector; 4-1-the 3rd inlet mouth;
4-2-induced draft fan; 6-the first refrigerator; 7-the second refrigerator;
8-the first three-way piece; 9-the second three-way piece; 10-the first gas flow adjuster;
11-the second gas flow adjuster.
Embodiment
The device that the present invention prepares spherical molybdic oxide powder is described by embodiment 1.
Embodiment 1
As depicted in figs. 1 and 2, the device that the present embodiment prepares spherical molybdic oxide powder comprises the compressed air reservoir 1, resistance furnace 2, condenser 3 and the cloth bag collector 4 that are communicated with successively;
Described compressed air reservoir 1 is provided with compressed air outlet 1-1, the bottom of described resistance furnace 2 is provided with the first inlet mouth 2-1, the top of described resistance furnace 2 is provided with first row gas port 2-2, condensing chamber 3-1 is provided with in described condenser 3, the bottom of described condensing chamber 3-1 is provided with the second inlet mouth 3-8, the top of described condensing chamber 3-1 is provided with second exhaust port 3-9, the bottom of described condensing chamber 3-1 is provided with condensate collection chamber 3-5, described condenser 3 with for providing the refrigerator of refrigerant to be communicated with to it, described cloth bag collector 4 is provided with the 3rd inlet mouth 4-1,
Described compressed air outlet 1-1 is communicated with the first channel of the first three-way piece 8, the second passage of described first three-way piece 8 is communicated with the first inlet mouth 2-1 by the first gas flow adjuster 10, the third channel of described first three-way piece 8 is communicated with the first channel of the second three-way piece 9 by the second gas flow adjuster 11, the second passage of described second three-way piece 9 is communicated with first row gas port 2-2, the third channel second inlet mouth 3-8 of described second three-way piece 9 is communicated with, and described second exhaust port 3-9 is communicated with the 3rd inlet mouth 4-1.
As depicted in figs. 1 and 2, described condensing chamber 3-1 periphery is surrounded with the first refrigerant room 3-2, described first 3-2 bottom, refrigerant room is provided with the first refrigerant input aperture 3-10, described first 3-2 top, refrigerant room is provided with the first refrigerant delivery port 3-11, described first refrigerant input aperture 3-10 is communicated with the refrigerant output terminal of the first refrigerator 6, and described first refrigerant delivery port 3-11 is communicated with the refrigerant input terminus of the first refrigerator 6.
As depicted in figs. 1 and 2, the top of described condensing chamber 3-1 is provided with the second refrigerant room, described second refrigerant room comprises the second refrigerant input room 3-3 and the second refrigerant exports room 3-4, described second refrigerant input 3-3 top, room is provided with the second refrigerant input aperture 3-12, described second refrigerant exports 3-4 top, room and is provided with the second refrigerant delivery port 3-13, described second refrigerant input aperture 3-12 is communicated with the refrigerant output terminal of the second refrigerator 7, and described second refrigerant delivery port 3-12 is communicated with the refrigerant input terminus of the second refrigerator 7;
As depicted in figs. 1 and 2, also be provided with the second refrigerant input tube 3-6 in described condensing chamber 3-1 and be sleeved on the second refrigerant output tube 3-7 outside the second refrigerant input tube 3-6, the both ends open of described second refrigerant input tube 3-6, wherein one end and the second refrigerant input room 3-3 and are communicated with, the other end is positioned at the second refrigerant output tube 3-7, one end of described second refrigerant output tube 3-7 is closed, and the other end and the second refrigerant export room 3-4 and be communicated with.
As depicted in figs. 1 and 2, in described condensing chamber 3-1, be movably set with the 3-14 that cuts somebody's hair, described in the 3-14 that cuts somebody's hair be connected with cylinder 3-16 by push rod 3-15.
As depicted in figs. 1 and 2, described cloth bag collector 4 is provided with induced draft fan 4-2.
In the present embodiment, in described cloth bag collector 4, the material of cloth bag is glass or terylene.
The method that the present invention utilizes device as described in Example 1 to prepare spherical molybdic oxide powder is described by embodiment 2-7 and comparative example 1-2.
Embodiment 2
Composition graphs 1 and Fig. 2, the method that the present embodiment prepares spherical molybdic oxide powder comprises the following steps:
Step one, quartz sand uniform spreading to be located in material boat, then molybdenum raw material uniform spreading to be located on quartz sand; Described molybdenum raw material is industrial molybdenum oxide;
Step 2, the material boat being equipped with quartz sand and molybdenum raw material in step one is placed in resistance furnace 2, then compressed air reservoir 1 is utilized to pass into pressurized air in resistance furnace 2, and utilize the first gas flow adjuster 10 and the second gas flow adjuster 11 to regulate compressed-air actuated flow, under the compressed-air actuated flow passing into the first inlet mouth 2-1 after regulating through the first gas flow adjuster 10 and the compressed-air actuated flow passing into the second three-way piece 9 after the second gas flow adjuster 11 regulates are the condition of 5L/min, being incubated 2h after temperature in resistance furnace 2 is risen to 1000 DEG C makes molybdenum raw material be gaseous state by solid state sublimation, be elevated gas,
Step 3, pass in condensing chamber 3-1 by sublimation gases described in step 2, then adopting air, water or liquid nitrogen to sublimate process to sublimation gases as refrigerant, is all obtain solid of sublimating in the cloth bag collector 4 of terylene at collecting chamber 3-5 and material.
The present embodiment utilizes the first refrigerator 6 to input the first refrigerant in the first refrigerant room 3-2 in condenser 3, condensation can be carried out from outside to the sublimation gases entered in condensing chamber 3-1, utilize the second refrigerator 7 to indoor input second refrigerant of the second refrigerant in condenser 3, condensation can be carried out to the sublimation gases entered in condensing chamber 3-1 from inside.Inside and outside act on simultaneously, make sublimation gases realize quenching rapidly for solid of sublimating.
Detect through XRD and FIIR and learn, the solid of sublimating that the present embodiment obtains in collecting chamber 3-5 and cloth bag collector 4 is molybdic oxide.As shown in Figure 3, the present embodiment products obtained therefrom regular appearance, unification as shown in Figure 3, and be spherical, granularity is within the scope of 0.2 μm ~ 1.0 μm for the SEM photo of the molybdic oxide powder prepared by the present embodiment.
Embodiment 3
Composition graphs 1 and Fig. 2, the method that the present embodiment prepares spherical molybdic oxide powder comprises the following steps:
Step one, quartz sand uniform spreading to be located in material boat, then molybdenum raw material uniform spreading to be located on quartz sand; Described molybdenum raw material is industrial molybdenum oxide;
Step 2, the material boat being equipped with quartz sand and molybdenum raw material in step one is placed in resistance furnace 2, then compressed air reservoir 1 is utilized to pass into pressurized air in resistance furnace 2, and utilize the first gas flow adjuster 10 and the second gas flow adjuster 11 to regulate compressed-air actuated flow, under the compressed-air actuated flow passing into the first inlet mouth 2-1 after regulating through the first gas flow adjuster 10 and the compressed-air actuated flow passing into the second three-way piece 9 after the second gas flow adjuster 11 regulates are the condition of 6L/min, being incubated 2h after temperature in resistance furnace 2 is risen to 900 DEG C makes molybdenum raw material be gaseous state by solid state sublimation, be elevated gas,
Step 3, pass in condensing chamber 3-1 by sublimation gases described in step 2, then adopting air, water or liquid nitrogen to sublimate process to sublimation gases as refrigerant, is all obtain solid of sublimating in the cloth bag collector 4 of terylene at collecting chamber 3-5 and material.
The present embodiment utilizes the first refrigerator 6 to input the first refrigerant in the first refrigerant room 3-2 in condenser 3, condensation can be carried out from outside to the sublimation gases entered in condensing chamber 3-1, utilize the second refrigerator 7 to indoor input second refrigerant of the second refrigerant in condenser 3, condensation can be carried out to the sublimation gases entered in condensing chamber 3-1 from inside.Inside and outside act on simultaneously, make sublimation gases realize quenching rapidly for solid of sublimating.
Detect through XRD and FIIR and learn, the solid of sublimating that the present embodiment obtains in collecting chamber 3-5 and cloth bag collector 4 is molybdic oxide.By regular equally to sem analysis known the present embodiment products obtained therefrom pattern of the molybdic oxide powder prepared by the present embodiment, unified, and be spherical, granularity is within the scope of 0.2 μm ~ 1.0 μm.
Embodiment 4
Composition graphs 1 and Fig. 2, the method that the present embodiment prepares spherical molybdic oxide powder comprises the following steps:
Step one, quartz sand uniform spreading to be located in material boat, then molybdenum raw material uniform spreading to be located on quartz sand; Described molybdenum raw material is molybdenum powder;
Step 2, the material boat being equipped with quartz sand and molybdenum raw material in step one is placed in resistance furnace 2, then compressed air reservoir 1 is utilized to pass into pressurized air in resistance furnace 2, and utilize the first gas flow adjuster 10 and the second gas flow adjuster 11 to regulate compressed-air actuated flow, under the compressed-air actuated flow passing into the first inlet mouth 2-1 after the first gas flow adjuster 10 adjustment and the condition of the equal 1L/min of compressed-air actuated flow passing into the second three-way piece 9 after the second gas flow adjuster 11 regulates, be incubated 2h after temperature in resistance furnace 2 is risen to 1000 DEG C and make molybdenum raw material by solid-state through atmospheric oxidation, distillation is gaseous state, be elevated gas,
Step 3, pass in condensing chamber 3-1 by sublimation gases described in step 2, then adopting air, water or liquid nitrogen to sublimate process to sublimation gases as refrigerant, is all obtain solid of sublimating in the cloth bag collector 4 of terylene at collecting chamber 3-5 and material.
The present embodiment utilizes the first refrigerator 6 to input the first refrigerant in the first refrigerant room 3-2 in condenser 3, condensation can be carried out from outside to the sublimation gases entered in condensing chamber 3-1, utilize the second refrigerator 7 to indoor input second refrigerant of the second refrigerant in condenser 3, condensation can be carried out to the sublimation gases entered in condensing chamber 3-1 from inside.Inside and outside act on simultaneously, make sublimation gases realize quenching rapidly for solid of sublimating.
Detect through XRD and FIIR and learn, the solid of sublimating that the present embodiment obtains in collecting chamber 3-5 and cloth bag collector 4 is molybdic oxide.As shown in Figure 4, the present embodiment products obtained therefrom regular appearance, unification as shown in Figure 4, and be spherical, granularity is within the scope of 0.2 μm ~ 1.2 μm for the SEM photo of the molybdic oxide powder prepared by the present embodiment.
Embodiment 5
Composition graphs 1 and Fig. 2, the method that the present embodiment prepares spherical molybdic oxide powder comprises the following steps:
Step one, quartz sand uniform spreading to be located in material boat, then molybdenum raw material uniform spreading to be located on quartz sand; Described molybdenum raw material is molybdenum powder;
Step 2, the material boat being equipped with quartz sand and molybdenum raw material in step one is placed in resistance furnace 2, then compressed air reservoir 1 is utilized to pass into pressurized air in resistance furnace 2, and utilize the first gas flow adjuster 10 and the second gas flow adjuster 11 to regulate compressed-air actuated flow, under the compressed-air actuated flow passing into the first inlet mouth 2-1 after regulating through the first gas flow adjuster 10 and the compressed-air actuated flow passing into the second three-way piece 9 after the second gas flow adjuster 11 regulates are the condition of 10L/min, be incubated 2h after temperature in resistance furnace 2 is risen to 800 DEG C and make molybdenum raw material by solid-state through atmospheric oxidation, distillation is gaseous state, be elevated gas,
Step 3, pass in condensing chamber 3-1 by sublimation gases described in step 2, then adopting air, water or liquid nitrogen to sublimate process to sublimation gases as refrigerant, is all obtain solid of sublimating in the cloth bag collector 4 of glass at collecting chamber 3-5 and material.
The present embodiment utilizes the first refrigerator 6 to input the first refrigerant in the first refrigerant room 3-2 in condenser 3, condensation can be carried out from outside to the sublimation gases entered in condensing chamber 3-1, utilize the second refrigerator 7 to indoor input second refrigerant of the second refrigerant in condenser 3, condensation can be carried out to the sublimation gases entered in condensing chamber 3-1 from inside.Inside and outside act on simultaneously, make sublimation gases realize quenching rapidly for solid of sublimating.
Detect through XRD and FIIR and learn, the solid of sublimating that the present embodiment obtains in collecting chamber 3-5 and cloth bag collector 4 is molybdic oxide.By to the TEM photo of the molybdic oxide powder prepared by the present embodiment as shown in Figure 5, as shown in Figure 5, the present embodiment products obtained therefrom pattern is regular equally, unified, and is spherical, and granularity is within the scope of 0.02 μm ~ 0.29 μm.
Embodiment 6
Composition graphs 1 and Fig. 2, the method that the present embodiment prepares spherical molybdic oxide powder comprises the following steps:
Step one, quartz sand uniform spreading to be located in material boat, then molybdenum raw material uniform spreading to be located on quartz sand; Described molybdenum raw material is the high-purity molybdenum trioxide that mass percentage is not less than 99.95%;
Step 2, the material boat being equipped with quartz sand and molybdenum raw material in step one is placed in resistance furnace 2, then compressed air reservoir 1 is utilized to pass into pressurized air in resistance furnace 2, and utilize the first gas flow adjuster 10 and the second gas flow adjuster 11 to regulate compressed-air actuated flow, under the compressed-air actuated flow passing into the first inlet mouth 2-1 after regulating through the first gas flow adjuster 10 and the compressed-air actuated flow passing into the second three-way piece 9 after the second gas flow adjuster 11 regulates are the condition of 3L/min, being incubated 2h after temperature in resistance furnace 2 is risen to 800 DEG C makes molybdenum raw material be gaseous state by solid state sublimation, be elevated gas,
Step 3, pass in condensing chamber 3-1 by sublimation gases described in step 2, then adopting air, water or liquid nitrogen to sublimate process to sublimation gases as refrigerant, is all obtain solid of sublimating in the cloth bag collector 4 of glass at collecting chamber 3-5 and material.
The present embodiment utilizes the first refrigerator 6 to input the first refrigerant in the first refrigerant room 3-2 in condenser 3, condensation can be carried out from outside to the sublimation gases entered in condensing chamber 3-1, utilize the second refrigerator 7 to indoor input second refrigerant of the second refrigerant in condenser 3, condensation can be carried out to the sublimation gases entered in condensing chamber 3-1 from inside.Inside and outside act on simultaneously, make sublimation gases realize quenching rapidly for solid of sublimating.
Detect through XRD and FIIR and learn, the solid of sublimating that the present embodiment obtains in collecting chamber 3-5 and cloth bag collector 4 is molybdic oxide.As shown in Figure 6, the present embodiment products obtained therefrom regular appearance, unification as shown in Figure 6, and be spherical, granularity is within the scope of 0.3 μm ~ 1.2 μm for the SEM photo of the molybdic oxide powder prepared by the present embodiment.
Embodiment 7
Composition graphs 1 and Fig. 2, the method that the present embodiment prepares spherical molybdic oxide powder comprises the following steps:
Step one, quartz sand uniform spreading to be located in material boat, then molybdenum raw material uniform spreading to be located on quartz sand; Described molybdenum raw material is the high-purity molybdenum trioxide that mass percentage is not less than 99.95%;
Step 2, the material boat being equipped with quartz sand and molybdenum raw material in step one is placed in resistance furnace 2, then compressed air reservoir 1 is utilized to pass into pressurized air in resistance furnace 2, and utilize the first gas flow adjuster 10 and the second gas flow adjuster 11 to regulate compressed-air actuated flow, under the compressed-air actuated flow passing into the first inlet mouth 2-1 after regulating through the first gas flow adjuster 10 and the compressed-air actuated flow passing into the second three-way piece 9 after the second gas flow adjuster 11 regulates are the condition of 7L/min, being incubated 2h after temperature in resistance furnace 2 is risen to 950 DEG C makes molybdenum raw material be gaseous state by solid state sublimation, be elevated gas,
Step 3, pass in condensing chamber 3-1 by sublimation gases described in step 2, then adopting air, water or liquid nitrogen to sublimate process to sublimation gases as refrigerant, is all obtain solid of sublimating in the cloth bag collector 4 of glass at collecting chamber 3-5 and material.
The present embodiment utilizes the first refrigerator 6 to input the first refrigerant in the first refrigerant room 3-2 in condenser 3, condensation can be carried out from outside to the sublimation gases entered in condensing chamber 3-1, utilize the second refrigerator 7 to indoor input second refrigerant of the second refrigerant in condenser 3, condensation can be carried out to the sublimation gases entered in condensing chamber 3-1 from inside.Inside and outside act on simultaneously, make sublimation gases realize quenching rapidly for solid of sublimating.
Detect through XRD and FIIR and learn, the solid of sublimating that the present embodiment obtains in collecting chamber 3-5 and cloth bag collector 4 is molybdic oxide.By regular equally to sem analysis known the present embodiment products obtained therefrom pattern of the molybdic oxide powder prepared by the present embodiment, unified, and be spherical, granularity is within the scope of 0.3 μm ~ 1.5 μm.
Comparative example 1
The difference of this comparative example and embodiment 2 is only: the first gas flow adjuster 10 described in step 2 passes into the first inlet mouth 2-1 compressed-air actuated flow after regulating and the compressed-air actuated flow passing into the second three-way piece 9 after the second gas flow adjuster 11 regulates are 0L/min.
Detect through XRD and FIIR and learn, the solid of sublimating that this comparative example obtains in collecting chamber 3-5 and cloth bag collector 4 is molybdic oxide.As shown in Figure 7, this comparative example products obtained therefrom is faller gill shape to the SEM photo of the molybdic oxide powder prepared by this comparative example as shown in Figure 7, and width is about 50 μm, and length can reach 500 μm.
Comparative example 2
The difference of this comparative example and embodiment 2 is only: the first gas flow adjuster 10 described in step 2 passes into the first inlet mouth 2-1 compressed-air actuated flow after regulating and the compressed-air actuated flow passing into the second three-way piece 9 after the second gas flow adjuster 11 regulates are 80L/min.
Detect through XRD and FIIR and learn, the solid of sublimating that this comparative example obtains in collecting chamber 3-5 and cloth bag collector 4 is molybdic oxide.The SEM photo of the molybdic oxide powder prepared by this comparative example as shown in Figure 8, this comparative example products obtained therefrom contains two kinds of crystal morphologies as shown in Figure 8: faller gill shape and spherical, wherein faller gill shape product width is less than 4 μm, and length is about 10-20 μm, and spherical product size range is below 2 μm.
By being analyzed known by embodiment 2 with comparative example 1-2, the present invention, by the pressurized air passing into certain flow at resistance furnace entrance and exit place, can control product pattern and size, the spherical molybdic oxide that final acquisition crystal formation is unified, complete.
The above is only preferred embodiment of the present invention, not imposes any restrictions the present invention.Every above embodiment is done according to invention technical spirit any simple modification, change and equivalence change, all still belong in the protection domain of technical solution of the present invention.
Claims (8)
1. prepare a device for spherical molybdic oxide powder, it is characterized in that, comprise the compressed air reservoir (1), resistance furnace (2), condenser (3) and the cloth bag collector (4) that are communicated with successively;
Described compressed air reservoir (1) is provided with compressed air outlet (1-1), the bottom of described resistance furnace (2) is provided with the first inlet mouth (2-1), the top of described resistance furnace (2) is provided with first row gas port (2-2), condensing chamber (3-1) is provided with in described condenser (3), the bottom of described condensing chamber (3-1) is provided with the second inlet mouth (3-8), the top of described condensing chamber (3-1) is provided with second exhaust port (3-9), the bottom of described condensing chamber (3-1) is provided with condensate collection chamber (3-5), described condenser (3) with for providing the refrigerator of refrigerant to be communicated with to it, described cloth bag collector (4) is provided with the 3rd inlet mouth (4-1),
Described compressed air outlet (1-1) is communicated with the first channel of the first three-way piece (8), the second passage of described first three-way piece (8) is communicated with the first inlet mouth (2-1) by the first gas flow adjuster (10), the third channel of described first three-way piece (8) is communicated with the first channel of the second three-way piece (9) by the second gas flow adjuster (11), the second passage of described second three-way piece (9) is communicated with first row gas port (2-2), the third channel of described second three-way piece (9) is communicated with the second inlet mouth (3-8), described second exhaust port (3-9) is communicated with the 3rd inlet mouth (4-1).
2. a kind of device preparing spherical molybdic oxide powder according to claim 1, it is characterized in that, described condensing chamber (3-1) periphery is surrounded with the first refrigerant room (3-2), described first refrigerant room (3-2) bottom is provided with the first refrigerant input aperture (3-10), described first refrigerant room (3-2) top is provided with the first refrigerant delivery port (3-11), described first refrigerant input aperture (3-10) is communicated with the refrigerant output terminal of the first refrigerator (6), described first refrigerant delivery port (3-11) is communicated with the refrigerant input terminus of the first refrigerator (6).
3. a kind of device preparing spherical molybdic oxide powder according to claim 2, it is characterized in that, the top of described condensing chamber (3-1) is provided with the second refrigerant room, described second refrigerant room comprises the second refrigerant input room (3-3) and the second refrigerant exports room (3-4), described second refrigerant input room (3-3) top is provided with the second refrigerant input aperture (3-12), described second refrigerant exports room (3-4) top and is provided with the second refrigerant delivery port (3-13), described second refrigerant input aperture (3-12) is communicated with the refrigerant output terminal of the second refrigerator (7), described second refrigerant delivery port (3-12) is communicated with the refrigerant input terminus of the second refrigerator (7),
Also be provided with the second refrigerant input tube (3-6) in described condensing chamber (3-1) and be sleeved on the second refrigerant input tube (3-6) the second refrigerant output tube (3-7) outward, the both ends open of described second refrigerant input tube (3-6), wherein one end and the second refrigerant input room (3-3) and are communicated with, the other end is positioned at the second refrigerant output tube (3-7), one end of described second refrigerant output tube (3-7) is closed, and the other end and the second refrigerant export room (3-4) and be communicated with.
4. a kind of device preparing spherical molybdic oxide powder according to claim 1,2 or 3, it is characterized in that, be movably set with cut somebody's hair (3-14) in described condensing chamber (3-1), described in cut somebody's hair (3-14) be connected with cylinder (3-16) by push rod (3-15).
5. a kind of device preparing spherical molybdic oxide powder according to claim 1,2 or 3, is characterized in that, described cloth bag collector (4) is provided with induced draft fan (4-2).
6. a kind of device preparing spherical molybdic oxide powder according to claim 1,2 or 3, is characterized in that, in described cloth bag collector (4), the material of cloth bag is glass or terylene.
7. utilize device as described in claim 1,2 or 3 to prepare a method for spherical molybdic oxide powder, it is characterized in that, the method comprises the following steps:
Step one, quartz sand uniform spreading to be located in material boat, then molybdenum raw material uniform spreading to be located on quartz sand; Described molybdenum raw material is molybdenum powder, industrial molybdenum oxide or high-purity molybdenum trioxide;
Step 2, the material boat being equipped with quartz sand and molybdenum raw material in step one is placed in resistance furnace (2), then compressed air reservoir (1) is utilized to pass into pressurized air in resistance furnace (2), and utilize the first gas flow adjuster (10) and the second gas flow adjuster (11) to regulate compressed-air actuated flow, under compressed-air actuated flow after regulating through the first gas flow adjuster (10) and the compressed-air actuated flow after the second gas flow adjuster (11) regulates are the condition of 1L/min ~ 10L/min, being incubated 2h after temperature in resistance furnace (2) is risen to 800 DEG C ~ 1050 DEG C makes molybdenum raw material be gaseous state by solid state sublimation, be elevated gas,
Step 3, sublimation gases described in step 2 is passed in condensing chamber (3-1), then adopt air, water or liquid nitrogen to sublimate process to sublimation gases as refrigerant, in collecting chamber (3-5) and cloth bag collector (4), all obtain the spherical molybdenum trioxide powder that granularity is 0.02 μm ~ 1.5 μm.
8. method according to claim 7, is characterized in that, in high-purity molybdenum trioxide described in step one, the mass percentage of molybdic oxide is not less than 99.95%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510633528.7A CN105152214B (en) | 2015-09-29 | 2015-09-29 | Device and method for producing spherical molybdenum trioxide powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510633528.7A CN105152214B (en) | 2015-09-29 | 2015-09-29 | Device and method for producing spherical molybdenum trioxide powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105152214A true CN105152214A (en) | 2015-12-16 |
| CN105152214B CN105152214B (en) | 2017-01-11 |
Family
ID=54793342
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510633528.7A Active CN105152214B (en) | 2015-09-29 | 2015-09-29 | Device and method for producing spherical molybdenum trioxide powder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105152214B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109415207A (en) * | 2016-06-29 | 2019-03-01 | Dic株式会社 | The manufacturing device of metal oxide and the manufacturing method of aforementioned metal oxides |
| CN111036342A (en) * | 2019-12-05 | 2020-04-21 | 四川大学 | Preparation device and preparation process of polymer-based spherical powder |
| CN112266021A (en) * | 2020-11-25 | 2021-01-26 | 中南大学 | Synchronous preparation phase pure alpha-MoO3And beta-MoO3Method (2) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN202988768U (en) * | 2012-10-12 | 2013-06-12 | 嵩县开拓者钼业有限公司 | High-purity superfine molybdenum trioxide production device |
| CN104858443A (en) * | 2015-05-25 | 2015-08-26 | 常熟锐钛金属制品有限公司 | Preparation method for high-purity nanoscale titanium-nickel alloy powder |
-
2015
- 2015-09-29 CN CN201510633528.7A patent/CN105152214B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN202988768U (en) * | 2012-10-12 | 2013-06-12 | 嵩县开拓者钼业有限公司 | High-purity superfine molybdenum trioxide production device |
| CN104858443A (en) * | 2015-05-25 | 2015-08-26 | 常熟锐钛金属制品有限公司 | Preparation method for high-purity nanoscale titanium-nickel alloy powder |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109415207A (en) * | 2016-06-29 | 2019-03-01 | Dic株式会社 | The manufacturing device of metal oxide and the manufacturing method of aforementioned metal oxides |
| US11472712B2 (en) | 2016-06-29 | 2022-10-18 | Dic Corporation | Metal oxide production apparatus and metal oxide production method |
| CN111036342A (en) * | 2019-12-05 | 2020-04-21 | 四川大学 | Preparation device and preparation process of polymer-based spherical powder |
| CN112266021A (en) * | 2020-11-25 | 2021-01-26 | 中南大学 | Synchronous preparation phase pure alpha-MoO3And beta-MoO3Method (2) |
| CN112266021B (en) * | 2020-11-25 | 2021-11-16 | 中南大学 | Synchronous preparation phase pure alpha-MoO3And beta-MoO3Method (2) |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105152214B (en) | 2017-01-11 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Liu et al. | Synthesis of Ce-doped In2O3 nanostructure for gas sensor applications | |
| Lu et al. | Hydrothermal synthesis of prism-like mesocrystal CeO2 | |
| Hao et al. | Visible light photocatalytic properties of metastable γ-Bi2O3 with different morphologies | |
| CN202988768U (en) | High-purity superfine molybdenum trioxide production device | |
| CN104118908B (en) | A kind of regulation and control preparation method of orderly titanium dioxide nano material | |
| KR101516900B1 (en) | Preparation method of industrial purple nano-needle tungsten oxide | |
| CN105152214A (en) | Device and method for producing spherical molybdenum trioxide powder | |
| CN101182197A (en) | W-Sn nano composite metal oxide gas-sensing material and preparation method thereof | |
| Liu et al. | Controlled fabrication and characterization of microspherical FeCO3 and α-Fe2O3 | |
| CN101264942A (en) | Method and device for producing high-grade nickel oxide | |
| CN106622331B (en) | A kind of preparation method of high-specific surface area graphite phase carbon nitride photochemical catalyst | |
| CN109019534A (en) | A kind of preparation method of ultrathin boron nitride nanosheet | |
| CN102603005A (en) | Method for preparing nanometer molybdenum trioxide | |
| CN105540640A (en) | Preparation method of flower-shaped nanometer zinc oxide | |
| CN107262139A (en) | A kind of preparation method of catalyst of modified molecular screen ZSM 5 and its application in biomass pyrolytic | |
| CN101891184A (en) | Method for continuously synthesizing single-wall carbon nano tube by high temperature chemical vapor deposition method | |
| CN101323977A (en) | Preparation of big length to diameter ratio aluminum oxide nanowire | |
| CN106215968B (en) | A kind of carbon coating CuO composite material and preparation methods of doping nitrogen | |
| CN103420427A (en) | Preparation method for bismuth ferrite Bi2Fe4O9 monocrystal nanosheets | |
| CN106964315B (en) | A kind of preparation method and application of hollow magnetic Co/ carbon nanotube | |
| CN116354744B (en) | Titanium dioxide antibacterial self-cleaning baking-free glaze and application method thereof | |
| CN106809808A (en) | A kind of preparation method of uniform hollow ball-shape VN nano particles | |
| CN105967167B (en) | A kind of method for preparing one-dimensional carbon nano material | |
| CN100372770C (en) | Method for preparing magnesia with high specific surface | |
| CN1321942C (en) | Method for preparing Nano crystal of metal oxide of anti agglomeration |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |