CN105819511A - Device for preparing nano-scale high-purity molybdenum trioxide and using method of device - Google Patents
Device for preparing nano-scale high-purity molybdenum trioxide and using method of device Download PDFInfo
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- CN105819511A CN105819511A CN201610291418.1A CN201610291418A CN105819511A CN 105819511 A CN105819511 A CN 105819511A CN 201610291418 A CN201610291418 A CN 201610291418A CN 105819511 A CN105819511 A CN 105819511A
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- molybdenum trioxide
- circulatory pool
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- subliming furnace
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- C01G39/00—Compounds of molybdenum
- C01G39/02—Oxides; Hydroxides
Abstract
A device for preparing nano-scale high-purity molybdenum trioxide comprises a raw material sublimating device, a water dissolving device, a smashing device and a collecting device. The invention further relates to a using method of the device for preparing nano-scale high-purity molybdenum trioxide.
Description
Technical field
The present invention relates to non-ferrous metallurgy technology field, a kind of device preparing nanometer level high purity molybdenum trioxide and using method thereof.
Background technology
Molybdenum trioxide is most important intermediate in molybdenum metallurgy, and the compound of most of molybdenums is all direct or indirect preparing for raw material with it, and molybdenum trioxide is all widely used in fields such as catalyst, display device, sensor, camera batteries.The most i.e. there is more significant vapour pressure due to molybdenum trioxide, so molybdenum trioxide can be purified by sublimed method, under the operating condition of distillation, the magazine of symbiosis the most therewith or not there is volatility (such as silicate etc.) maybe can not condense and be removed.
US6468497 discloses the production method of a kind of nano-sized molybdenum oxide, industrial molybdenum oxide employing distillation-quenching method is produced nano-sized molybdenum oxide, production technology is as follows: by the industrial molybdenum oxide powder body (being generally made up of molybdenum trioxide and molybdenum dioxide) of granularity about 24～260 μm in subliming furnace sent into by controlled spiral conveyer, blasting air through entrance makes molybdenum dioxide be oxidized to molybdenum trioxide, subliming furnace electric power heats, in-furnace temperature is detected with thermocouple, when furnace temperature reaches 1100 DEG C, molybdenum trioxide starts distillation and is deposited on like in membranaceous feed pipe；The nano-sized molybdenum oxide liquid nitrogen stream distilled is quenched, enter hopper, then inflow filter, through blower fan sucking-off cold air, nano-sized molybdenum oxide product is discharged through funnel, reaction sublimation temperature is 1093～1260 DEG C, and the activity duration of subliming furnace is 120min, can the longest 100nm of output, wide 25nm, high 20nm in strip nanoscale molybdenum trioxide.This kind of method uses liquid nitrogen stream quenching, is not suitable for long-time production continuously, and annual production is the highest.
China Authorization Notice No. CN102603005B, Patent No. CN201210057610.6, authorized announcement date is that in December, 2013 patent of invention of 04 day includes non-ferrous metal metallurgical technology field, especially relate to a kind of method preparing nano-sized molybdenum oxide for raw material with pure molybdenum trioxide, the method is with pure molybdenum trioxide as raw material, nano-sized molybdenum oxide is prepared by plasma distillation, pure molybdenum trioxide powder is sent in plasma subliming furnace by feeding device, plasma stream distils, operating time 10 ~ 100ms, the gaseous state molybdenum trioxide obtained uses quenching medium quenching, material collecting device is collected, obtain nano-sized molybdenum oxide, MoO3 > 99.80%.Using plasma sublimed method of the present invention prepares molybdenum trioxide, can obtain granularity high-purity nm molybdenum trioxide within 80nm, and be truly realized automatization, continuous prodution in ultra-short Time.The method by make molybdenum trioxide in plasma stream rapidly distillation and then the method that uses cold medium be quenched realize continuous prodution, but using plasma subliming furnace, whole tooling cost height, economic benefit is the highest；It addition, cold medium is only to be quenched molybdenum trioxide steam across pipeline, cooling effect is bad, and cool time is longer.
Summary of the invention
The present invention is to solve in prior art nanoscale molybdenum trioxide produce present in the problems referred to above, it is provided that a kind of structurally simple, economical high efficiency, the device preparing nanometer level high purity molybdenum trioxide of continuous prodution can be realized.
A kind of device preparing nanometer level high purity molybdenum trioxide, including raw material sublimation apparatus, water-soluble device, reducing mechanism and collection device；
Described raw material sublimation apparatus includes raw material cabin, feeding machine and subliming furnace, and described subliming furnace is provided with heating element heater and thermocouple；
Described water-soluble device includes VERTICAL TUBE, ejector, circulatory pool and circulation vacuum pump, described VERTICAL TUBE connects subliming furnace and ejector, circulation vacuum pump is positioned at circulatory pool side, conduit will connect circulatory pool, circulation vacuum pump and ejector and link together, and VERTICAL TUBE top is provided with normally opened electromagnetism flange, dispersant entrance and nozzle；
Described reducing mechanism includes that slush pump, flash vessel, air flow crushing device, described slush pump one end are connected with bottom circulatory pool, and the other end is connected with flash vessel；
Described collection device includes surge drum and finished product bin, is provided with filter element in described surge drum, is provided with automatic blowing element and air exhauster outside surge drum, and finished product bin is positioned at the lower section of surge drum.
Described subliming furnace side is provided with observation port.
Described ejector uses the heat-resistance stainless steel of 310S material.
The using method of a kind of device preparing nanometer level high purity molybdenum trioxide, comprises the following steps:
1) rendering on feeding machine by raw material molybdenum trioxide by raw material cabin, raw material molybdenum trioxide enters in subliming furnace, controls the temperature in subliming furnace at 900-1100 DEG C；
2) the molybdenum trioxide steam that step 1) obtains enters in ejector via VERTICAL TUBE, coolant in circulatory pool is extracted by circulation vacuum pump, by conduit from ejector top is drenched, completing the cooling to molybdenum trioxide steam, molybdenum trioxide particles falls to bottom circulatory pool；
3) open slush pump, the molybdenum trioxide particles in circulatory pool is drawn in flash vessel, slimy molybdenum trioxide is dried；
4) opening the air exhauster of surge drum side, molybdenum trioxide particles enters in air flow crushing device, after the crushed sub-sieve of granule, falls to finished product bin under the effect of filter element.
Described step 2) in coolant be deionized water or ethanol.
The method have the advantages that
1, employing prior art use universal subliming furnace to produce molybdenum trioxide steam, utilize circulatory pool and ejector (water-soluble device), molybdenum trioxide steam is sunk to bottom circulatory pool and forms muddy, cooling is rapidly, it is extracted in reducing mechanism by slush pump again, flash vessel is utilized to remove moisture, finally realized pulverizing by air flow crushing device, obtain nanoscale molybdenum trioxide particles and drop in finished product bin, structurally simple, economical high efficiency, utilizing circulatory pool to cool down, the time is short, can realize continuous prodution.
2, in the design, VERTICAL TUBE top is provided with normally opened electromagnetism flange, dispersant entrance and nozzle, add man-hour, dispersant enters from dispersant entrance, converge with molybdenum trioxide steam in being ejected into VERTICAL TUBE via nozzle, and then enter in water-soluble device, molybdenum trioxide particles gathering bottom circulatory pool can be prevented effectively from agglomerating, it is ensured that the quality of nanoscale molybdenum trioxide particles.
3, in the design, VERTICAL TUBE top is provided with normally opened electromagnetism flange, and during work, electromagnetism flange is closed so that the medium (preferably deionized water) in circulatory pool can be evacuated to ejector top by circulation vacuum pump, completes the cyclic process of a cooling；When after process finishing, owing to distillation furnace pressure is less, for preventing the deionized water in circulatory pool to be back in subliming furnace, now electromagnetism flange opens (because it is normally opened), keeping the pressure balance of pipe interior, deionized water will not reflux, it is ensured that the safe handling of whole device.
Accompanying drawing explanation
Fig. 1 is the structural representation of device in the present invention.
Wherein, raw material sublimation apparatus 1, raw material cabin 11, feeding machine 12, subliming furnace 13, heating element heater 14, electroheat pair 15, observation port 16, water-soluble device 2, VERTICAL TUBE 21, ejector 22, circulatory pool 23, circulation vacuum pump 24, conduit 25, electromagnetism flange 26, dispersant entrance 27, nozzle 28, reducing mechanism 3, slush pump 31, flash vessel 32, air flow crushing device 33, collection device 4, surge drum 41, finished product bin 42, filter element 43, automatic blowing element 44, air exhauster 45.
Detailed description of the invention
A kind of device preparing nanometer level high purity molybdenum trioxide, including raw material sublimation apparatus 1, water-soluble device 2, reducing mechanism 3 and collection device 4；
Described raw material sublimation apparatus includes raw material cabin 11, feeding machine 12 and subliming furnace 13, and described subliming furnace 13 is provided with heating element heater 14 and thermocouple 15；
Described water-soluble device 2 includes VERTICAL TUBE 21, ejector 22, circulatory pool 23 and circulation vacuum pump 24, described VERTICAL TUBE 21 connects subliming furnace 13 and ejector 22, circulation vacuum pump 24 is positioned at circulatory pool 23 side, conduit 25 will connect circulatory pool 23, circulation vacuum pump 24 and ejector 22 and link together, and VERTICAL TUBE 21 top is provided with normally opened electromagnetism flange 26, dispersant entrance 27 and nozzle 28；
Described reducing mechanism 3 includes that slush pump 31, flash vessel 32, air flow crushing device 33, described slush pump 31 one end are connected bottom circulatory pool 23, and the other end is connected with flash vessel 32；
Described collection device 4 includes surge drum 41 and finished product bin 42, is provided with filter element 43 in described surge drum 41, is provided with automatic blowing element 44 and air exhauster 45 outside surge drum 41, and finished product bin 42 is positioned at the lower section of surge drum 41.
Described subliming furnace 13 side is provided with observation port 16.
Described ejector 22 uses the heat-resistance stainless steel of 310S material.
The using method of a kind of device preparing nanometer level high purity molybdenum trioxide, comprises the following steps:
1) rendering on feeding machine 12 by raw material molybdenum trioxide by raw material cabin 11, raw material molybdenum trioxide enters in subliming furnace 13, controls the temperature in subliming furnace 13 at 900-1100 DEG C；
2) the molybdenum trioxide steam that step 1) obtains enters in ejector 22 via VERTICAL TUBE 21, coolant in circulatory pool 23 is extracted by circulation vacuum pump 24, by conduit 25 from ejector 22 top is drenched, completing the cooling to molybdenum trioxide steam, molybdenum trioxide particles falls to bottom circulatory pool 23；
3) open slush pump 31, the molybdenum trioxide particles in circulatory pool 23 is drawn in flash vessel 32, slimy molybdenum trioxide is dried；
4) opening the air exhauster 45 of surge drum 41 side, molybdenum trioxide particles enters in air flow crushing device 33, after the crushed sub-sieve of granule, falls to finished product bin 42 under the effect of filter element 43.
Described step 2) in coolant be deionized water or ethanol.
Dispersant is a kind of chemicals, is added to the water the ability increasing its degranulation, prevents the cohesion of solid particle.
310S is widely used in industrial transportation pipe line and the machine structural parts etc. such as oil, chemical industry, medical treatment, food, light industry, machinery instrument.310s has a much better creep strength, at high temperature can continuous operation, there is good heat-resisting quantity.
The design uses and uses universal subliming furnace 13 to produce molybdenum trioxide steam in prior art, utilize circulatory pool 23 and the water-soluble device of ejector 22(2), molybdenum trioxide steam is sunk to bottom circulatory pool 23 and forms muddy, cooling is rapidly, it is extracted in reducing mechanism 3 by slush pump 31 again, flash vessel 32 is utilized to remove moisture, finally realized pulverizing by air flow crushing device 33, obtain nanoscale molybdenum trioxide particles and drop in finished product bin 42, structurally simple, economical high efficiency, utilizing circulatory pool 23 to cool down, the time is short, can realize continuous prodution.In the design, VERTICAL TUBE 21 top is provided with normally opened electromagnetism flange 26, dispersant entrance 27 and nozzle 28, add man-hour, dispersant enters from dispersant entrance 27, converge with molybdenum trioxide steam in being ejected into VERTICAL TUBE 21 via nozzle 28, and then enter in water-soluble device 2, molybdenum trioxide particles gathering bottom circulatory pool 23 can be prevented effectively from agglomerating, it is ensured that the quality of nanoscale molybdenum trioxide particles.In the design, VERTICAL TUBE 21 top is provided with normally opened electromagnetism flange 26, and during work, electromagnetism flange 26 is closed so that the medium (preferably deionized water) in circulatory pool 23 can be evacuated to ejector 22 top by circulation vacuum pump 24, completes the cyclic process of a cooling；When after process finishing, owing in subliming furnace 13, pressure is less, for preventing the deionized water in circulatory pool 23 to be back in subliming furnace 13, now electromagnetism flange 26 opens (because it is normally opened), keeping the pressure balance of pipe interior, deionized water will not reflux, it is ensured that the safe handling of whole device.
The method that present invention employs water soluble method cooling, can realize quickly cooling, to realize large-tonnage production.Present configuration is simple, high financial profit, can realize continuous prodution.
Claims (5)
1. prepare a device for nanometer level high purity molybdenum trioxide, including raw material sublimation apparatus (1), water-soluble device (2), reducing mechanism (3) and collection device (4)；
Described raw material sublimation apparatus includes raw material cabin (11), feeding machine (12) and subliming furnace (13), and described subliming furnace (13) is provided with heating element heater (14) and thermocouple (15)；
Described water-soluble device (2) includes VERTICAL TUBE (21), ejector (22), circulatory pool (23) and circulation vacuum pump (24), described VERTICAL TUBE (21) connects subliming furnace (13) and ejector (22), circulation vacuum pump (24) is positioned at circulatory pool (23) side, conduit (25) will connect circulatory pool (23), circulation vacuum pump (24) and ejector (22) and link together, and VERTICAL TUBE (21) top is provided with normally opened electromagnetism flange (26), dispersant entrance (27) and nozzle (28)；
Described reducing mechanism (3) includes that slush pump (31), flash vessel (32), air flow crushing device (33), described slush pump (31) one end are connected with circulatory pool (23) bottom, and the other end is connected with flash vessel (32)；
Described collection device (4) includes surge drum (41) and finished product bin (42), filter element (43) it is provided with in described surge drum (41), surge drum (41) outside is provided with automatic blowing element (44) and air exhauster (45), and finished product bin (42) is positioned at the lower section of surge drum (41).
A kind of device preparing nanometer level high purity molybdenum trioxide the most according to claim 1, it is characterised in that: described subliming furnace (13) side is provided with observation port (16).
A kind of device preparing nanometer level high purity molybdenum trioxide the most according to claim 1, it is characterised in that: described ejector (22) uses the heat-resistance stainless steel of 310S material.
4. a using method for the device preparing nanometer level high purity molybdenum trioxide as described in Claims 1-4 is arbitrary, comprises the following steps:
1) rendering on feeding machine (12) by raw material molybdenum trioxide by raw material cabin (11), raw material molybdenum trioxide enters in subliming furnace (13), controls the temperature in subliming furnace (13) at 900-1100 DEG C；
2) the molybdenum trioxide steam that step 1) obtains enters in ejector (22) via VERTICAL TUBE (21), coolant in circulatory pool (23) is extracted by circulation vacuum pump (24), by conduit (25) from ejector (22) top is drenched, completing the cooling to molybdenum trioxide steam, molybdenum trioxide particles falls to circulatory pool (23) bottom；
3) open slush pump (31), the molybdenum trioxide particles in circulatory pool (23) is drawn in flash vessel (32), slimy molybdenum trioxide is dried；
4) opening the air exhauster (45) of surge drum (41) side, molybdenum trioxide particles enters in air flow crushing device (33), after the crushed sub-sieve of granule, falls to finished product bin (42) under the effect of filter element (43).
The using method of a kind of device preparing nanometer level high purity molybdenum trioxide the most according to claim 4, it is characterised in that: described step 2) in coolant be deionized water or ethanol.
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| CN113511680A (en) * | 2021-08-10 | 2021-10-19 | 郑州大学 | Preparation method of high-purity molybdenum trioxide |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113511680A (en) * | 2021-08-10 | 2021-10-19 | 郑州大学 | Preparation method of high-purity molybdenum trioxide |
| CN113511680B (en) * | 2021-08-10 | 2022-11-25 | 郑州大学 | Preparation method of high-purity molybdenum trioxide |
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