CN105152214B - Device and method for producing spherical molybdenum trioxide powder - Google Patents
Device and method for producing spherical molybdenum trioxide powder Download PDFInfo
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- CN105152214B CN105152214B CN201510633528.7A CN201510633528A CN105152214B CN 105152214 B CN105152214 B CN 105152214B CN 201510633528 A CN201510633528 A CN 201510633528A CN 105152214 B CN105152214 B CN 105152214B
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- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
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- 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
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- B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
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- 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
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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 chemical products preparing technical field, be specifically related to a kind of dress preparing spherical molybdenum trioxide powder body
Put and method.
Background technology
Molybdenum trioxide is a kind of important molybdenum chemical products, but also is the primary raw material of Mo powder production, in petroleum industry
In be used as catalyst, it may also be used for enamel glaze pigment and medicine etc..The preparation method of molybdenum trioxide is a lot, mainly includes precipitation
Method, hydro-thermal method, chemical vapour deposition technique, gel casting forming method, sol-gel process etc..At present can by above distinct methods
Prepare the molybdenum trioxide of different-shape, including: threadiness, crystal whisker-shaped, flake, bar-shaped, wire, fine granularity pipe, particulate
Degree band, spherical etc..In the molybdenum trioxide material of above-mentioned pattern, the spherical molybdenum trioxide of fine granularity is owing to having polymolecularity and high ratio
Surface area, it is possible to be greatly improved the catalytic performance of catalyst so that it is have the biggest application prospect at catalyst industry.It addition, it is thin
The spherical molybdenum trioxide of granularity can be used for synthesizing the spherical IF-MoS of class of ultralow friction coefficient2Material.
The preparation method of the spherical molybdenum trioxide of fine granularity is mainly template and sonochemical method at present, and preparation method is numerous
Trivial, reaction solution digestion time is 12h, is unfavorable for that industrialization promotion produces.By comparison, with industrial molybdenum oxide as raw material, adopt
With sublimed method prepare the preparation method of sphericalshaped fine-grain degree molybdenum trioxide can yet be regarded as a kind of easy, quick, have bigger industrial applications
The technique of prospect.
At present, though there being the research using the method that distils-sublimate to prepare high-purity molybdenum trioxide both at home and abroad, but made molybdenum trioxide is
Needle-like structures.Up to now, about using the method that distils-sublimate to prepare the relevant of unified, the complete spherical molybdenum trioxide of crystal formation
There is not been reported in research.
Summary of the invention
The technical problem to be solved is for above-mentioned the deficiencies in the prior art, it is provided that one prepares spherical three
The device of molybdenum oxide powder body.This device is passed through the compressed air of certain flow in resistance furnace exit, on the one hand for the coldest
But the molybdenum trioxide gas after distillation, on the other hand for the flue gas of transfer pipeline, compressed-air actuated input can ensure that entrance is cold
The molybdenum trioxide flue gas dispersion of condenser, prevents from mutually colliding other patterns of the longest great achievement, is finally obtained in that crystal formation is unified, complete
Whole spherical molybdenum trioxide.
For solving above-mentioned technical problem, the technical solution used in the present invention is: a kind of prepare spherical molybdenum trioxide powder body
Device, it is characterised in that include compressed air reservoir, resistance furnace, condenser and the cloth bag catcher being sequentially communicated；
Being provided with compressed air outlet on described compressed air reservoir, the bottom of described resistance furnace is provided with the first air inlet
Mouthful, the top of described resistance furnace is provided with first row QI KOU, is provided with condensation chamber, the bottom of described condensation chamber in described condenser
Being provided with the second air inlet, the top of described condensation chamber is provided with second exhaust port, and the bottom of described condensation chamber is provided with condensation
Thing collecting chamber, described condenser, with for it provides the refrigerator of coolant connect, described cloth bag catcher is provided with the 3rd
Air inlet；
The first passage connection of described compressed air outlet and the first three-way piece, the second channel of described first three-way piece leads to
Crossing the first gas flow adjuster and the connection of the first air inlet, the third channel of described first three-way piece passes through the second gas flow
The first passage connection of actuator and the second three-way piece, the second channel of described second three-way piece connects with first row QI KOU, institute
Stating third channel and the connection of the second air inlet of the second three-way piece, described second exhaust port connects with the 3rd air inlet.
Above-mentioned a kind of device preparing spherical molybdenum trioxide powder body, it is characterised in that described condensation chamber peripheral ring winding
Being equipped with the first coolant room, described first bottom, coolant room is provided with the first coolant input port, and described first top, coolant room is arranged
The first coolant delivery outlet, described first coolant input port is had to connect with the coolant outfan of the first refrigerator, described first coolant
The coolant input connection of delivery outlet and the first refrigerator.
Above-mentioned a kind of device preparing spherical molybdenum trioxide powder body, it is characterised in that the top of described condensation chamber is arranged
Having the second coolant room, described second coolant room to include the second coolant input room and the second coolant output room, described second coolant is defeated
Top of entering the room is provided with the second coolant input port, and described second coolant output top, room is provided with the second coolant delivery outlet, described
Second coolant input port connects with the coolant outfan of the second refrigerator, described second coolant delivery outlet and the second refrigerator cold
Matchmaker's input connects；
The second coolant input pipe and the second coolant being sleeved on outside the second coolant input pipe it is additionally provided with in described condensation chamber
Outlet tube, the both ends open of described second coolant input pipe, wherein one end connects with the second coolant input room, and the other end is positioned at the
In two coolant outlet tubes, one end of described second coolant outlet tube is closed, the other end and the second coolant output room connection.
Above-mentioned a kind of device preparing spherical molybdenum trioxide powder body, it is characterised in that described condensation indoor activity is arranged
Cut somebody's hair, described in cut somebody's hair and be connected with cylinder by push rod.
Above-mentioned a kind of device preparing spherical molybdenum trioxide powder body, it is characterised in that arrange on described cloth bag catcher
There is air-introduced machine.
Above-mentioned a kind of device preparing spherical molybdenum trioxide powder body, it is characterised in that cloth bag in described cloth bag catcher
Material be glass or terylene.
It addition, present invention also offers a kind of method utilizing said apparatus to prepare spherical molybdenum trioxide powder body, its feature
Being, the method comprises the following steps:
Step one, quartz sand uniform spreading is located at material boat in, then molybdenum raw material uniform spreading is 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 utilizes compression
Air reservoir is passed through compressed air in resistance furnace, and utilizes the first gas flow adjuster and the second gas flow adjuster pair
Compressed-air actuated flow is adjusted, at the compressed-air actuated flow after the first gas flow adjuster regulation and through second
Under conditions of compressed-air actuated flow after gas flow adjuster regulation is 1L/min～10L/min, by resistance furnace
Temperature is incubated 2h after rising to 800 DEG C～1050 DEG C makes molybdenum raw material be gaseous state by solid state sublimation, is elevated gas；
Step 3, sublimation gases described in step 2 is passed through in condensation chamber, then uses empty gas and water or liquid nitrogen as cold
Sublimation gases is sublimated process by matchmaker, and all obtaining granularity in collecting chamber and cloth bag catcher is 0.02 μm～the ball of 1.5 μm
Shape molybdenum trioxide powder.
Above-mentioned method, it is characterised in that described in step one, in high-purity molybdenum trioxide, the percent mass of molybdenum trioxide contains
Amount is not less than 99.95%.
The present invention compared with prior art has the advantage that
1, the preparation method of the spherical molybdenum trioxide of fine granularity provided by the present invention, molybdenum raw material can use industrial molybdenum oxide,
High-purity molybdenum trioxide, molybdenum powder etc..Compared with the preparation method of conventional high-purity molybdenum trioxide, the shape of the made molybdenum trioxide of the present invention
Looks are that fine granularity is spherical, and the concordance of product is good；And the method for the present invention is the highest to producing equipment requirements, be suitable to extensive raw
Produce.
2, the present invention by being passed through the compressed air of certain flow in resistance furnace exit, on the one hand for tentatively cooling down liter
Molybdenum trioxide gas after China, on the other hand for the flue gas of transfer pipeline, compressed-air actuated input can ensure that entrance condenser
In molybdenum trioxide flue gas dispersion, prevent from mutually colliding other patterns of the longest great achievement, become spherical molybdenum trioxide formed weight
Want behave.
3, the present invention have developed a kind of many media condenser with quenching effect, and the formation for spherical molybdenum trioxide provides
Ensure, it is possible to ensure that the dispersed very fast cooling down of molybdenum trioxide flue gas that enters is to below de-sublimation temperature.
4, the power adjustment that the compressed air that the present invention is passed through by resistance furnace bottom carries mainly as flue gas.
5, the present invention can use the multiple mediums such as water, air, liquid nitrogen as cooling medium, only need to be by changing cooling medium
Just the molybdenum trioxide of different crystal morphology can be prepared, including: 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, is suitable to industry metaplasia
Produce.
7, the molybdenum raw material in the present invention can use industrial molybdenum oxide, high-purity molybdenum trioxide, molybdenum powder etc. containing molybdenum product, this technique
If using quality purity not less than 99.95% high-purity molybdenum trioxide, regulated by technology controlling and process of the present invention, it is possible to system
The standby mass purity molybdenum trioxide product not less than 99.99%, it is adaptable to industrialization large-scale production.
With embodiment, the present invention is described in further detail below in conjunction with the accompanying drawings.
Accompanying drawing explanation
Fig. 1 is the structural representation that the present invention prepares the device of spherical molybdenum trioxide powder body.
Fig. 2 is the structural representation of condenser of the present invention.
Fig. 3 is the SEM photograph of the molybdenum trioxide powder body of the embodiment of the present invention 2 preparation.
Fig. 4 is the SEM photograph of the molybdenum trioxide powder body of the embodiment of the present invention 4 preparation.
Fig. 5 is the TEM photo of the molybdenum trioxide powder body of the embodiment of the present invention 5 preparation.
Fig. 6 is the SEM photograph of the molybdenum trioxide powder body of the embodiment of the present invention 6 preparation.
Fig. 7 is the SEM photograph of the molybdenum trioxide powder body of comparative example 1 of the present invention preparation.
Fig. 8 is the SEM photograph of the molybdenum trioxide powder body of comparative example 2 of the present invention preparation.
Description of reference numerals:
1 compressed air reservoir；1-1 compressed air outlet；2 resistance furnaces；
2-1 the first air inlet；2-2 first row QI KOU；3 condensers；
3-1 condensation chamber；3-2 the first coolant room；3-3 the second coolant input room；
3-4 the second coolant output room；3-5 condensate collection chamber；3-6 the second coolant input pipe；
3-7 the second coolant outlet tube；3-8 the second air inlet；3-9 the second gas outlet；
3-10 the first coolant input port；3-11 the first coolant delivery outlet；3-12 the second coolant input port；
3-13 the second coolant delivery outlet；3-14 cuts somebody's hair；3-15 push rod；
3-16 cylinder；4 cloth bag catchers；4-1 the 3rd air inlet；
4-2 air-introduced machine；6 first refrigerators；7 second refrigerators；
8 first three-way pieces；9 second three-way pieces；10 first gas flow adjusters；
11 second gas flow adjusters.
Detailed description of the invention
The present invention is prepared the device of spherical molybdenum trioxide powder body and is described by embodiment 1.
Embodiment 1
As depicted in figs. 1 and 2, to prepare the compression that the device of spherical molybdenum trioxide powder body includes being sequentially communicated empty for the present embodiment
Gas storage tank 1, resistance furnace 2, condenser 3 and cloth bag catcher 4；
Being provided with compressed air outlet 1-1 on described compressed air reservoir 1, the bottom of described resistance furnace 2 is provided with first
Air inlet 2-1, the top of described resistance furnace 2 is provided with first row QI KOU 2-2, is provided with condensation chamber 3-1 in described condenser 3,
The bottom of described condensation chamber 3-1 is provided with the second air inlet 3-8, and the top of described condensation chamber 3-1 is provided with second exhaust port 3-
9, the bottom of described condensation chamber 3-1 is provided with condensate collection chamber 3-5, described condenser 3 and the system for it provides coolant
Cooler connects, and described cloth bag catcher 4 is provided with the 3rd air inlet 4-1；
The first passage connection of described compressed air outlet 1-1 and the first three-way piece 8, the second of described first three-way piece 8
Passage is connected with the first air inlet 2-1 by the first gas flow adjuster 10, and the third channel of described first three-way piece 8 passes through
Second gas flow adjuster 11 connects with the first passage of the second three-way piece 9, the second channel of described second three-way piece 9 and
One air vent 2-2 connection, third channel the second air inlet 3-8 connection of described second three-way piece 9, described second exhaust port 3-9
Connect with the 3rd air inlet 4-1.
As depicted in figs. 1 and 2, described condensation chamber 3-1 periphery is surrounded with the first coolant room 3-2, described first coolant
3-2 bottom, room is provided with the first coolant input port 3-10, and described first 3-2 top, coolant room is provided with the first coolant delivery outlet 3-
11, the coolant outfan connection of described first coolant input port 3-10 and the first refrigerator 6, described first coolant delivery outlet 3-11
Connect with the coolant input of the first refrigerator 6.
As depicted in figs. 1 and 2, the top of described condensation chamber 3-1 is provided with the second coolant room, and described second coolant room includes
Second coolant input room 3-3 and the second coolant output room 3-4, described second coolant input 3-3 top, room is provided with the second coolant
Input port 3-12, described second coolant output 3-4 top, room is provided with the second coolant delivery outlet 3-13, described second coolant input
The coolant outfan connection of mouth 3-12 and the second refrigerator 7, described second coolant delivery outlet 3-12 and the coolant of the second refrigerator 7
Input connects；
As depicted in figs. 1 and 2, it is additionally provided with the second coolant input pipe 3-6 in described condensation chamber 3-1 and to be sleeved on second cold
The second coolant outlet tube 3-7 outside matchmaker input pipe 3-6, the both ends open of described second coolant input pipe 3-6, wherein one end and the
Two coolant input room 3-3 connections, the other end is positioned at the second coolant outlet tube 3-7, one end of described second coolant outlet tube 3-7
Close, the other end and the output room 3-4 connection of the second coolant.
As depicted in figs. 1 and 2, be movably set with, in described condensation chamber 3-1, the 3-14 that cuts somebody's hair, described in the 3-14 that cuts somebody's hair pass through push rod
3-15 is connected with cylinder 3-16.
As depicted in figs. 1 and 2, described cloth bag catcher 4 is provided with air-introduced machine 4-2.
In the present embodiment, in described cloth bag catcher 4, the material of cloth bag is glass or terylene.
The present invention utilize device as described in Example 1 prepare the method for spherical molybdenum trioxide powder body by embodiment 2-7 with
And comparative example 1-2 is described.
Embodiment 2
In conjunction with Fig. 1 and Fig. 2, the present embodiment is prepared the method for spherical molybdenum trioxide powder body and is comprised the following steps:
Step one, quartz sand uniform spreading is located at material boat in, then molybdenum raw material uniform spreading is 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 utilizes compression
Air reservoir 1 is passed through compressed air in resistance furnace 2, and utilizes the first gas flow adjuster 10 and the regulation of the second gas flow
Compressed-air actuated flow is adjusted by device 11, is being passed through the first air inlet 2-1 after the first gas flow adjuster 10 regulation
Compressed-air actuated flow and after the second gas flow adjuster 11 regulation, be passed through the compressed-air actuated stream of the second three-way piece 9
Under conditions of amount is 5L/min, it is incubated 2h after the temperature in resistance furnace 2 is risen to 1000 DEG C and makes the molybdenum raw material by solid state sublimation be
Gaseous state, is elevated gas；
Step 3, sublimation gases described in step 2 is passed through in condensation chamber 3-1, then uses empty gas and water or liquid nitrogen to make
Sublimation gases sublimated process for coolant, all sublimated in collecting chamber 3-5 and cloth bag catcher 4 that material is terylene
Solid.
The present embodiment inputs the first coolant in utilizing first refrigerator 6, first coolant room 3-2 in condenser 3, it is possible to
The sublimation gases entered in condensation chamber 3-1 is condensed from outside, utilizes the second refrigerator 7 second in condenser 3 cold
Matchmaker indoor input the second coolant, it is possible to the sublimation gases entered in condensation chamber 3-1 is condensed from inside.Inside and outside make simultaneously
With so that it is solid of sublimating that sublimation gases realizes quenching rapidly.
Learning through XRD and FIIR detection, the present embodiment is obtained sublimating admittedly in collecting chamber 3-5 and cloth bag catcher 4
Body is molybdenum trioxide.The SEM photograph of the molybdenum trioxide powder body prepared by the present embodiment is as it is shown on figure 3, this enforcement as shown in Figure 3
Example products obtained therefrom regular appearance, unification, and it is spherical, granularity is in 0.2 μm～1.0 μ m.
Embodiment 3
In conjunction with Fig. 1 and Fig. 2, the present embodiment is prepared the method for spherical molybdenum trioxide powder body and is comprised the following steps:
Step one, quartz sand uniform spreading is located at material boat in, then molybdenum raw material uniform spreading is 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 utilizes compression
Air reservoir 1 is passed through compressed air in resistance furnace 2, and utilizes the first gas flow adjuster 10 and the regulation of the second gas flow
Compressed-air actuated flow is adjusted by device 11, is being passed through the first air inlet 2-1 after the first gas flow adjuster 10 regulation
Compressed-air actuated flow and after the second gas flow adjuster 11 regulation, be passed through the compressed-air actuated stream of the second three-way piece 9
Under conditions of amount is 6L/min, it is incubated 2h after the temperature in resistance furnace 2 is risen to 900 DEG C and makes molybdenum raw material be gas by solid state sublimation
State, is elevated gas；
Step 3, sublimation gases described in step 2 is passed through in condensation chamber 3-1, then uses empty gas and water or liquid nitrogen to make
Sublimation gases sublimated process for coolant, all sublimated in collecting chamber 3-5 and cloth bag catcher 4 that material is terylene
Solid.
The present embodiment inputs the first coolant in utilizing first refrigerator 6, first coolant room 3-2 in condenser 3, it is possible to
The sublimation gases entered in condensation chamber 3-1 is condensed from outside, utilizes the second refrigerator 7 second in condenser 3 cold
Matchmaker indoor input the second coolant, it is possible to the sublimation gases entered in condensation chamber 3-1 is condensed from inside.Inside and outside make simultaneously
With so that it is solid of sublimating that sublimation gases realizes quenching rapidly.
Learning through XRD and FIIR detection, the present embodiment is obtained sublimating admittedly in collecting chamber 3-5 and cloth bag catcher 4
Body is molybdenum trioxide.Produce by the sem analysis of the molybdenum trioxide powder body prepared by the present embodiment is understood the present embodiment gained
Product pattern is the most regular, unified, and is spherical, and granularity is in 0.2 μm～1.0 μ m.
Embodiment 4
In conjunction with Fig. 1 and Fig. 2, the present embodiment is prepared the method for spherical molybdenum trioxide powder body and is comprised the following steps:
Step one, quartz sand uniform spreading is located at material boat in, then molybdenum raw material uniform spreading is 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 utilizes compression
Air reservoir 1 is passed through compressed air in resistance furnace 2, and utilizes the first gas flow adjuster 10 and the regulation of the second gas flow
Compressed-air actuated flow is adjusted by device 11, is being passed through the first air inlet 2-1 after the first gas flow adjuster 10 regulation
Compressed-air actuated flow and after the second gas flow adjuster 11 regulation, be passed through the compressed-air actuated stream of the second three-way piece 9
Under conditions of measuring equal 1L/min, it is incubated 2h after the temperature in resistance furnace 2 is risen to 1000 DEG C and makes molybdenum raw material by solid-state through air oxygen
Change, rise Huawei's gaseous state, be elevated gas；
Step 3, sublimation gases described in step 2 is passed through in condensation chamber 3-1, then uses empty gas and water or liquid nitrogen to make
Sublimation gases sublimated process for coolant, all sublimated in collecting chamber 3-5 and cloth bag catcher 4 that material is terylene
Solid.
The present embodiment inputs the first coolant in utilizing first refrigerator 6, first coolant room 3-2 in condenser 3, it is possible to
The sublimation gases entered in condensation chamber 3-1 is condensed from outside, utilizes the second refrigerator 7 second in condenser 3 cold
Matchmaker indoor input the second coolant, it is possible to the sublimation gases entered in condensation chamber 3-1 is condensed from inside.Inside and outside make simultaneously
With so that it is solid of sublimating that sublimation gases realizes quenching rapidly.
Learning through XRD and FIIR detection, the present embodiment is obtained sublimating admittedly in collecting chamber 3-5 and cloth bag catcher 4
Body is molybdenum trioxide.The SEM photograph of the molybdenum trioxide powder body prepared by the present embodiment as shown in Figure 4, this enforcement as shown in Figure 4
Example products obtained therefrom regular appearance, unification, and it is spherical, granularity is in 0.2 μm～1.2 μ m.
Embodiment 5
In conjunction with Fig. 1 and Fig. 2, the present embodiment is prepared the method for spherical molybdenum trioxide powder body and is comprised the following steps:
Step one, quartz sand uniform spreading is located at material boat in, then molybdenum raw material uniform spreading is 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 utilizes compression
Air reservoir 1 is passed through compressed air in resistance furnace 2, and utilizes the first gas flow adjuster 10 and the regulation of the second gas flow
Compressed-air actuated flow is adjusted by device 11, is being passed through the first air inlet 2-1 after the first gas flow adjuster 10 regulation
Compressed-air actuated flow and after the second gas flow adjuster 11 regulation, be passed through the compressed-air actuated stream of the second three-way piece 9
Under conditions of amount is 10L/min, it is incubated 2h after the temperature in resistance furnace 2 is risen to 800 DEG C and makes molybdenum raw material by solid-state through air
Oxidation, rises Huawei's gaseous state, is elevated gas；
Step 3, sublimation gases described in step 2 is passed through in condensation chamber 3-1, then uses empty gas and water or liquid nitrogen to make
Sublimation gases sublimated process for coolant, all sublimated in collecting chamber 3-5 and cloth bag catcher 4 that material is glass
Solid.
The present embodiment inputs the first coolant in utilizing first refrigerator 6, first coolant room 3-2 in condenser 3, it is possible to
The sublimation gases entered in condensation chamber 3-1 is condensed from outside, utilizes the second refrigerator 7 second in condenser 3 cold
Matchmaker indoor input the second coolant, it is possible to the sublimation gases entered in condensation chamber 3-1 is condensed from inside.Inside and outside make simultaneously
With so that it is solid of sublimating that sublimation gases realizes quenching rapidly.
Learning through XRD and FIIR detection, the present embodiment is obtained sublimating admittedly in collecting chamber 3-5 and cloth bag catcher 4
Body is molybdenum trioxide.By to the TEM photo of the molybdenum trioxide powder body prepared by the present embodiment as it is shown in figure 5, can by Fig. 5
Knowing, the present embodiment products obtained therefrom pattern is the most regular, unified, and is spherical, and granularity is in 0.02 μm～0.29 μ m.
Embodiment 6
In conjunction with Fig. 1 and Fig. 2, the present embodiment is prepared the method for spherical molybdenum trioxide powder body and is comprised the following steps:
Step one, quartz sand uniform spreading is located at material boat in, then molybdenum raw material uniform spreading is located on quartz sand；Described molybdenum
Raw material is the high-purity molybdenum trioxide that weight/mass percentage composition 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 utilizes compression
Air reservoir 1 is passed through compressed air in resistance furnace 2, and utilizes the first gas flow adjuster 10 and the regulation of the second gas flow
Compressed-air actuated flow is adjusted by device 11, is being passed through the first air inlet 2-1 after the first gas flow adjuster 10 regulation
Compressed-air actuated flow and after the second gas flow adjuster 11 regulation, be passed through the compressed-air actuated stream of the second three-way piece 9
Under conditions of amount is 3L/min, it is incubated 2h after the temperature in resistance furnace 2 is risen to 800 DEG C and makes molybdenum raw material be gas by solid state sublimation
State, is elevated gas；
Step 3, sublimation gases described in step 2 is passed through in condensation chamber 3-1, then uses empty gas and water or liquid nitrogen to make
Sublimation gases sublimated process for coolant, all sublimated in collecting chamber 3-5 and cloth bag catcher 4 that material is glass
Solid.
The present embodiment inputs the first coolant in utilizing first refrigerator 6, first coolant room 3-2 in condenser 3, it is possible to
The sublimation gases entered in condensation chamber 3-1 is condensed from outside, utilizes the second refrigerator 7 second in condenser 3 cold
Matchmaker indoor input the second coolant, it is possible to the sublimation gases entered in condensation chamber 3-1 is condensed from inside.Inside and outside make simultaneously
With so that it is solid of sublimating that sublimation gases realizes quenching rapidly.
Learning through XRD and FIIR detection, the present embodiment is obtained sublimating admittedly in collecting chamber 3-5 and cloth bag catcher 4
Body is molybdenum trioxide.The SEM photograph of the molybdenum trioxide powder body prepared by the present embodiment as shown in Figure 6, this enforcement as shown in Figure 6
Example products obtained therefrom regular appearance, unification, and it is spherical, granularity is in 0.3 μm～1.2 μ m.
Embodiment 7
In conjunction with Fig. 1 and Fig. 2, the present embodiment is prepared the method for spherical molybdenum trioxide powder body and is comprised the following steps:
Step one, quartz sand uniform spreading is located at material boat in, then molybdenum raw material uniform spreading is located on quartz sand；Described molybdenum
Raw material is the high-purity molybdenum trioxide that weight/mass percentage composition 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 utilizes compression
Air reservoir 1 is passed through compressed air in resistance furnace 2, and utilizes the first gas flow adjuster 10 and the regulation of the second gas flow
Compressed-air actuated flow is adjusted by device 11, is being passed through the first air inlet 2-1 after the first gas flow adjuster 10 regulation
Compressed-air actuated flow and after the second gas flow adjuster 11 regulation, be passed through the compressed-air actuated stream of the second three-way piece 9
Under conditions of amount is 7L/min, it is incubated 2h after the temperature in resistance furnace 2 is risen to 950 DEG C and makes molybdenum raw material be gas by solid state sublimation
State, is elevated gas；
Step 3, sublimation gases described in step 2 is passed through in condensation chamber 3-1, then uses empty gas and water or liquid nitrogen to make
Sublimation gases sublimated process for coolant, all sublimated in collecting chamber 3-5 and cloth bag catcher 4 that material is glass
Solid.
The present embodiment inputs the first coolant in utilizing first refrigerator 6, first coolant room 3-2 in condenser 3, it is possible to
The sublimation gases entered in condensation chamber 3-1 is condensed from outside, utilizes the second refrigerator 7 second in condenser 3 cold
Matchmaker indoor input the second coolant, it is possible to the sublimation gases entered in condensation chamber 3-1 is condensed from inside.Inside and outside make simultaneously
With so that it is solid of sublimating that sublimation gases realizes quenching rapidly.
Learning through XRD and FIIR detection, the present embodiment is obtained sublimating admittedly in collecting chamber 3-5 and cloth bag catcher 4
Body is molybdenum trioxide.Produce by the sem analysis of the molybdenum trioxide powder body prepared by the present embodiment is understood the present embodiment gained
Product pattern is the most regular, unified, and is spherical, and granularity is in 0.3 μm～1.5 μ m.
Comparative example 1
This comparative example the difference is that only with embodiment 2: described in step 2, the first gas flow adjuster 10 is adjusted
It is passed through the compressed-air actuated flow of the first air inlet 2-1 after joint and is passed through second after the second gas flow adjuster 11 regulation
The compressed-air actuated flow of three-way piece 9 is 0L/min.
Learning through XRD and FIIR detection, this comparative example is obtained sublimating admittedly in collecting chamber 3-5 and cloth bag catcher 4
Body is molybdenum trioxide.The SEM photograph of the molybdenum trioxide powder body prepared by this comparative example is as it is shown in fig. 7, this contrast as shown in Figure 7
Example products obtained therefrom is faller gill shape, and width is about 50 μm, and length is up to 500 μm.
Comparative example 2
This comparative example the difference is that only with embodiment 2: described in step 2, the first gas flow adjuster 10 is adjusted
It is passed through the compressed-air actuated flow of the first air inlet 2-1 after joint and is passed through second after the second gas flow adjuster 11 regulation
The compressed-air actuated flow of three-way piece 9 is 80L/min.
Learning through XRD and FIIR detection, this comparative example is obtained sublimating admittedly in collecting chamber 3-5 and cloth bag catcher 4
Body is molybdenum trioxide.The SEM photograph of the molybdenum trioxide powder body prepared by this comparative example as shown in Figure 8, this contrast as shown in Figure 8
Example products obtained therefrom contains two kinds of crystal morphologies: faller gill shape and spherical, and wherein faller gill shape product width is less than 4 μm, length about 10-20
μm, spherical product particle size range is below 2 μm.
By embodiment 2 being analyzed with comparative example 1-2, the present invention is by resistance furnace entrance and exit
Place is passed through the compressed air of certain flow, it is possible to control product pattern and size, final obtain that crystal formation is unified, complete spherical three
Molybdenum oxide.
The above, be only presently preferred embodiments of the present invention, not impose any restrictions the present invention.Every according to invention skill
Any simple modification, change and the equivalence change that above example is made by art essence, all still falls within technical solution of the present invention
Protection domain in.
Claims (8)
1. the device preparing spherical molybdenum trioxide powder body, it is characterised in that include the compressed air reservoir being sequentially communicated
(1), resistance furnace (2), condenser (3) and cloth bag catcher (4)；
Being provided with compressed air outlet (1-1) on described compressed air reservoir (1), the bottom of described resistance furnace (2) is provided with
One air inlet (2-1), the top of described resistance furnace (2) is provided with first row QI KOU (2-2), and described condenser is provided with in (3)
Condensation chamber (3-1), the bottom of described condensation chamber (3-1) is provided with the second air inlet (3-8), the top of described condensation chamber (3-1)
Being provided with second exhaust port (3-9), the bottom of described condensation chamber (3-1) is provided with condensate collection chamber (3-5), described condenser
(3) with for it provides the refrigerator of coolant connect, described cloth bag catcher (4) is provided with the 3rd air inlet (4-1)；
Described compressed air outlet (1-1) connects with the first passage of the first three-way piece (8), the of described first three-way piece (8)
Two passages are connected with the first air inlet (2-1) by the first gas flow adjuster (10), the 3rd of described first three-way piece (8)
Passage is connected with the first passage of the second three-way piece (9) by the second gas flow adjuster (11), described second three-way piece (9)
Second channel connect with first row QI KOU (2-2), the third channel of described second three-way piece (9) and the second air inlet (3-8)
Connection, described second exhaust port (3-9) connects with the 3rd air inlet (4-1).
A kind of device preparing spherical molybdenum trioxide powder body the most according to claim 1, it is characterised in that described condensation chamber
(3-1) periphery is surrounded with the first coolant room (3-2), and described first coolant room (3-2) bottom is provided with the first coolant input
Mouth (3-10), described first coolant room (3-2) top is provided with the first coolant delivery outlet (3-11), described first coolant input port
(3-10) the coolant outfan with the first refrigerator (6) connects, described first coolant delivery outlet (3-11) and the first refrigerator (6)
Coolant input connection.
A kind of device preparing spherical molybdenum trioxide powder body the most according to claim 2, it is characterised in that described condensation chamber
(3-1) top is provided with the second coolant room, and described second coolant room includes that the second coolant input room (3-3) and the second coolant are defeated
Going out room (3-4), described second coolant input room (3-3) top is provided with the second coolant input port (3-12), described second coolant
Output room (3-4) top is provided with the second coolant delivery outlet (3-13), described second coolant input port (3-12) and the second refrigeration
The coolant outfan connection of device (7), described second coolant delivery outlet (3-12) connects with the coolant input of the second refrigerator (7)
Logical；
It is additionally provided with the second coolant input pipe (3-6) in described condensation chamber (3-1) and is sleeved on the second coolant input pipe (3-6) outward
The second coolant outlet tube (3-7), the both ends open of described second coolant input pipe (3-6), wherein one end is defeated with the second coolant
Enter the room (3-3) connection, the other end is positioned at the second coolant outlet tube (3-7), an end seal of described second coolant outlet tube (3-7)
Close, the other end and the second coolant output room (3-4) connection.
4. according to a kind of device preparing spherical molybdenum trioxide powder body described in claim 1,2 or 3, it is characterised in that described
Be movably set with, in condensation chamber (3-1), cut somebody's hair (3-14), described in cut somebody's hair (3-14) by push rod (3-15) and cylinder (3-16) even
Connect.
5. according to a kind of device preparing spherical molybdenum trioxide powder body described in claim 1,2 or 3, it is characterised in that described
Air-introduced machine (4-2) it is provided with on cloth bag catcher (4).
6. according to a kind of device preparing spherical molybdenum trioxide powder body described in claim 1,2 or 3, it is characterised in that described
In cloth bag catcher (4), the material of cloth bag is glass or terylene.
7. one kind utilizes the method that device as described in claim 1,2 or 3 prepares spherical molybdenum trioxide powder body, it is characterised in that
The method comprises the following steps:
Step one, quartz sand uniform spreading is located at material boat in, then molybdenum raw material uniform spreading is located on quartz sand；Described molybdenum raw material
For 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 utilizes compression sky
Gas storage tank (1) is passed through compressed air in resistance furnace (2), and utilizes the first gas flow adjuster (10) and the second gas flow
Compressed-air actuated flow is adjusted by actuator (11), the compressed air after regulating through the first gas flow adjuster (10)
Flow and through the second gas flow adjuster (11) regulate after compressed-air actuated flow be 1L/min's～10L/min
Under the conditions of, it is incubated 2h after the temperature in resistance furnace (2) is risen to 800 DEG C～1050 DEG C and makes molybdenum raw material be gaseous state by solid state sublimation,
It is elevated gas；
Step 3, sublimation gases described in step 2 is passed through in condensation chamber (3-1), then uses empty gas and water or liquid nitrogen conduct
Sublimation gases is sublimated process by coolant, all obtain in collecting chamber (3-5) and cloth bag catcher (4) granularity be 0.02 μm～
The spherical molybdenum trioxide powder of 1.5 μm.
Method the most according to claim 7, it is characterised in that molybdenum trioxide in high-purity molybdenum trioxide described in step one
Weight/mass percentage composition is not less than 99.95%.
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| 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 |
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| 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 |
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