CN105819511B - A kind of device and its application method for preparing nanometer level high purity molybdenum trioxide - Google Patents
A kind of device and its application method for preparing nanometer level high purity molybdenum trioxide Download PDFInfo
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- CN105819511B CN105819511B CN201610291418.1A CN201610291418A CN105819511B CN 105819511 B CN105819511 B CN 105819511B CN 201610291418 A CN201610291418 A CN 201610291418A CN 105819511 B CN105819511 B CN 105819511B
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- molybdenum trioxide
- circulatory pool
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- high purity
- injector
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
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- C01G39/00—Compounds of molybdenum
- C01G39/02—Oxides; Hydroxides
Abstract
A kind of device for preparing nanometer level high purity molybdenum trioxide, including raw material sublimation apparatus, water-soluble device, reducing mechanism and collection device；The invention further relates to the application method of such a device for preparing nanometer level high purity molybdenum trioxide.
Description
Technical field
The present invention relates to non-ferrous metallurgy technology field, a kind of especially dress for preparing nanometer level high purity molybdenum trioxide
Put and its application method.
Background technology
Molybdenum trioxide is most important intermediate in molybdenum metallurgy, and the compound of most of molybdenums is all direct or indirect with it
Made from raw material, molybdenum trioxide is all widely used in fields such as catalyst, display device, sensor, camera batteries.By
There is more significant vapour pressure at a lower temperature in molybdenum trioxide, it is possible to molybdenum trioxide is carried out only with sublimed method
Change, under the operating condition of distillation, the usual magazine of symbiosis or without volatility therewith（Such as silicate）Or can not condense
And be removed.
US6468497 discloses a kind of production method of nano-sized molybdenum oxide, and industrial molybdenum oxide is used into distillation-quenching
Method produces nano-sized molybdenum oxide, and production technology is as follows:By about 24~260 μm of industrial molybdenum oxide powder of granularity（Generally by
Molybdenum trioxide and molybdenum dioxide composition）Through in controllable spiral conveyer feeding subliming furnace, blasting air through entrance makes molybdenum dioxide
Molybdenum trioxide is oxidized to, subliming furnace is heated with electric power, in-furnace temperature, when furnace temperature reaches 1100 DEG C, three oxygen are detected with thermocouple
Change molybdenum to start to distil and be deposited on like in membranaceous feed pipe；The nano-sized molybdenum oxide distilled is quenched with liquid nitrogen stream, enters material bin,
Then inflow filter, cold air is suctioned out through blower fan, and nano-sized molybdenum oxide product is discharged through funnel, and reaction sublimation temperature is 1093~
1260 DEG C, activity duration of subliming furnace is 120min, can the about long 100nm of output, wide 25nm, high 20nm be in strip nanoscale three
Molybdenum oxide.Such a method is quenched using liquid nitrogen stream, is not suitable for continuous production for a long time, and annual production is not high.
Chinese Authorization Notice No. CN102603005B, Patent No. CN201210057610.6, authorized announcement date is 2013
The patent of invention on December 04, in is related to non-ferrous metal metallurgical technology field, more particularly, to one kind using pure molybdenum trioxide as raw material
The method for preparing nano-sized molybdenum oxide, this method prepares the oxygen of nanometer three using pure molybdenum trioxide as raw material by plasma distillation
Change molybdenum, pure molybdenum trioxide powder sent into plasma subliming furnace by feeding device, distilled in plasma stream,
10 ~ 100ms of operating time, the gaseous state molybdenum trioxide of acquisition is quenched using quenching medium, and material collecting device is collected, and obtains the oxygen of nanometer three
Change molybdenum, MoO3>99.80%.Using plasma sublimed method of the present invention prepares molybdenum trioxide, and grain can be obtained in ultra-short Time
The high-purity nm molybdenum trioxide spent within 80nm, and it is truly realized automation, continuous production.This method is by making three
The method that molybdenum oxide is distilled rapidly in plasma stream and then is quenched using cold medium realizes continuous production, but uses
Plasma subliming furnace, whole tooling cost is high, and economic benefit is not high；In addition, cold medium is only to three across pipeline
Molybdenum oxide steam is quenched, and cooling effect is bad, and cool time is longer.
The content of the invention
There is provided one kind knot in order to solve above mentioned problem present in nanoscale molybdenum trioxide production in the prior art by the present invention
Structure is simple, high financial profit, can realize the device for preparing nanometer level high purity molybdenum trioxide of continuous production.
A kind of device for preparing nanometer level high purity molybdenum trioxide, including raw material sublimation apparatus, water-soluble device, reducing mechanism
And collection device；
The raw material sublimation apparatus includes being provided with heating element heater on raw material cabin, feeding machine and subliming furnace, the subliming furnace
And thermocouple；
The water-soluble device includes VERTICAL TUBE, injector, circulatory pool and circulation vacuum pump, and the VERTICAL TUBE connects subliming furnace
And injector, circulation vacuum pump is located at circulatory pool side, and conduit will connect circulatory pool, circulation vacuum pump and injector and be connected to one
Rise, normally opened electromagnetism flange, dispersant entrance and nozzle are provided with the top of VERTICAL TUBE；
The reducing mechanism includes slush pump, flash vessel, air flow crushing device, described slush pump one end and circulatory pool bottom
It is connected, the other end is connected with flash vessel；
The collection device includes being provided with outside filter element, surge drum in surge drum and finished product bin, the surge drum
Side is provided with automatic blowing element and air exhauster, and finished product bin is located at the lower section of surge drum.
The subliming furnace side is provided with peep hole.
The injector uses the heat-resistance stainless steel of 310S materials.
A kind of application method for the device for preparing nanometer level high purity molybdenum trioxide, comprises the following steps：
1）Raw material molybdenum trioxide is delivered onto feeding machine by raw material cabin, raw material molybdenum trioxide is entered in subliming furnace,
By the temperature control in subliming furnace at 900-1100 DEG C；
2）Step 1）Obtained molybdenum trioxide steam is entered in injector via VERTICAL TUBE, and circulation vacuum pump is by circulatory pool
Interior coolant is extracted, under being drenched by conduit at the top of injector, completes the cooling to molybdenum trioxide steam, molybdenum trioxide particles
Fall to circulatory pool bottom；
3）Slush pump is opened, the molybdenum trioxide particles in circulatory pool are drawn into flash vessel, is aoxidized to slimy three
Molybdenum is dried；
4）The air exhauster of surge drum side is opened, molybdenum trioxide particles are entered in air flow crushing device, particle is crushed
After sub-sieve, finished product bin is fallen in the presence of filter element.
The step 2）In coolant be deionized water or alcohol.
The invention has the advantages that：
1st, using molybdenum trioxide steam is produced using universal subliming furnace in the prior art, circulatory pool and injector are utilized
（Water-soluble device）So that molybdenum trioxide steam sinks to circulatory pool bottom and forms muddy, and cooling is rapid, then will by slush pump
It is extracted into reducing mechanism, and moisture is removed using flash vessel, is finally realized and crushed by air flow crushing device, obtains the oxygen of nanoscale three
Change molybdenum particle to drop into finished product bin, structurally simple, economical high efficiency is cooled down, the time is short using circulatory pool, can be realized
Continuous production.
2nd, normally opened electromagnetism flange, dispersant entrance and nozzle are provided with the top of VERTICAL TUBE in the design, during processing, disperseed
Agent enters from dispersant entrance, is ejected into VERTICAL TUBE and converges with molybdenum trioxide steam via nozzle, and then enters water-soluble dress
In putting, aggregation of the molybdenum trioxide particles in circulatory pool bottom can be prevented effectively from agglomerating, it is ensured that nanoscale molybdenum trioxide particles
Quality.
3rd, normally opened electromagnetism flange is provided with the top of VERTICAL TUBE in the design, during work, electromagnetism flange is closed so that circulation
Vavuum pump can be by the medium in circulatory pool（It is preferred that deionized water）It is evacuated at the top of injector, completes the cyclic process of a cooling；
After process finishing, because distillation furnace pressure is smaller, to prevent the deionized water in circulatory pool to be back in subliming furnace, now
Electromagnetism flange is opened（Because it is normally opened）, the pressure balance inside pipeline is kept, deionized water will not flow back, it is ensured that whole
The safe handling of device.
Brief description of the drawings
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 is seen
Hole 16 is examined, water-soluble device 2, VERTICAL TUBE 21, injector 22, circulatory pool 23, circulation vacuum pump 24, conduit 25, electromagnetism flange 26 divides
Powder 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.
Embodiment
A kind of device for preparing nanometer level high purity molybdenum trioxide, including raw material sublimation apparatus 1, water-soluble device 2, crushing dress
Put 3 and collection device 4；
The raw material sublimation apparatus includes being provided with raw material cabin 11, feeding machine 12 and subliming furnace 13, the subliming furnace 13
Heating element heater 14 and thermocouple 15；
The water-soluble device 2 includes VERTICAL TUBE 21, injector 22, circulatory pool 23 and circulation vacuum pump 24, the VERTICAL TUBE
21 connection subliming furnaces 13 and injector 22, circulation vacuum pump 24 are located at the side of circulatory pool 23, and conduit 25 will connect circulatory pool 23, circulation
Vavuum pump 24 and injector 22 link together, and the top of VERTICAL TUBE 21 is provided with normally opened electromagnetism flange 26, dispersant entrance 27
With nozzle 28；
The reducing mechanism 3 include slush pump 31, flash vessel 32, air flow crushing device 33, described one end of slush pump 31 with
The bottom of circulatory pool 23 is connected, and the other end is connected with flash vessel 32；
The collection device 4 includes being provided with filter element 43 in surge drum 41 and finished product bin 42, the surge drum 41,
The outside of surge drum 41 is provided with automatic blowing element 44 and air exhauster 45, and finished product bin 42 is located at the lower section of surge drum 41.
The side of subliming furnace 13 is provided with peep hole 16.
The injector 22 uses the heat-resistance stainless steel of 310S materials.
A kind of application method for the device for preparing nanometer level high purity molybdenum trioxide, comprises the following steps：
1）Raw material molybdenum trioxide is delivered on feeding machine 12 by raw material cabin 11, raw material molybdenum trioxide enters subliming furnace
In 13, by the temperature control in subliming furnace 13 at 900-1100 DEG C；
2）Step 1）Obtained molybdenum trioxide steam is entered in injector 22 via VERTICAL TUBE 21, and circulation vacuum pump 24 will
Coolant in circulatory pool 23 is extracted, and under being drenched by conduit 25 from the top of injector 22, completes the cooling to molybdenum trioxide steam,
Molybdenum trioxide particles fall to the bottom of circulatory pool 23；
3）Slush pump 31 is opened, the molybdenum trioxide particles in circulatory pool 23 are drawn into flash vessel 32, to slimy
Molybdenum trioxide is dried；
4）The air exhauster 45 of the side of surge drum 41 is opened, molybdenum trioxide particles are entered in air flow crushing device 33, particle
After pulverized sub-sieve, finished product bin 42 is fallen in the presence of filter element 43.
The step 2）In coolant be deionized water or alcohol.
Dispersant is a kind of chemicals, and being added to the water increases the ability of its degranulation, prevents the cohesion of solid particle.
310S is widely used in the industrial transportation pipe lines such as oil, chemical industry, medical treatment, food, light industry, machinery instrument and machinery knot
Structure part etc..310s possesses much better creep strength, at high temperature can continuous operation, with good heat-resisting quantity.
The design utilizes circulatory pool 23 using molybdenum trioxide steam is produced using universal subliming furnace 13 in the prior art
With injector 22（Water-soluble device 2）So that molybdenum trioxide steam sinks to the bottom of circulatory pool 23 and forms muddy, and cooling is rapid,
It is extracted into again by slush pump 31 in reducing mechanism 3, moisture is removed using flash vessel 32, it is finally real by air flow crushing device 33
Now crush, obtain nanoscale molybdenum trioxide particles and drop into finished product bin 42, structurally simple, economical high efficiency utilizes circulation
Pond 23 is cooled down, and the time is short, can realize continuous production.The top of VERTICAL TUBE 21 is provided with normally opened electromagnetism flange in the design
26th, dispersant entrance 27 and nozzle 28, during processing, dispersant enters from dispersant entrance 27, is ejected into vertically via nozzle 28
Converge in pipe 21 with molybdenum trioxide steam, and then enter in water-soluble device 2, molybdenum trioxide particles can be prevented effectively from circulatory pool
The aggregation of 23 bottoms is agglomerating, it is ensured that the quality of nanoscale molybdenum trioxide particles.The top of VERTICAL TUBE 21 is provided with often in the design
The electromagnetism flange 26 opened, during work, electromagnetism flange 26 is closed so that circulation vacuum pump 24 can be by the medium in circulatory pool 23（It is excellent
Select deionized water）The top of injector 22 is evacuated to, the cyclic process of a cooling is completed；After process finishing, due to subliming furnace 13
Interior pressure is smaller, to prevent the deionized water in circulatory pool 23 to be back in subliming furnace 13, and now electromagnetism flange 26 is opened（Because of it
It is normally opened）, the pressure balance inside pipeline is kept, deionized water will not flow back, it is ensured that the safe handling of whole device.
Present invention employs the method for water soluble method cooling, quick cooling can be realized, to realize large-tonnage production.The present invention
Structurally simple, economical high efficiency, continuous production can be realized.
Claims (5)
1. a kind of device for preparing nanometer level high purity molybdenum trioxide, including raw material sublimation apparatus（1）, water-soluble device（2）, crush
Device（3）And collection device（4）；
The raw material sublimation apparatus includes raw material cabin（11）, feeding machine（12）And subliming furnace（13）, the subliming furnace（13）On set
It is equipped with heating element heater（14）And thermocouple（15）；
The water-soluble device（2）Including VERTICAL TUBE（21）, injector（22）, circulatory pool（23）And circulation vacuum pump（24）, it is described
VERTICAL TUBE（21）Connect subliming furnace（13）And injector（22）, circulation vacuum pump（24）Positioned at circulatory pool（23）Side, conduit
（25）Circulatory pool will be connect（23）, circulation vacuum pump（24）And injector（22）Link together, VERTICAL TUBE（21）Top is provided with
Normally opened electromagnetism flange（26）, dispersant entrance（27）And nozzle（28）；
The reducing mechanism（3）Including slush pump（31）, flash vessel（32）, air flow crushing device（33）, the slush pump（31）
One end and circulatory pool（23）Bottom is connected, the other end and flash vessel（32）It is connected；
The collection device（4）Including surge drum（41）And finished product bin（42）, the surge drum（41）Inside it was provided with filtering element
Part（43）, surge drum（41）Outside is provided with automatic blowing element（44）And air exhauster（45）, finished product bin（42）Positioned at collection
Cylinder（41）Lower section.
2. a kind of device for preparing nanometer level high purity molybdenum trioxide according to claim 1, it is characterised in that：The liter
Magnificent stove（13）Side is provided with peep hole（16）.
3. a kind of device for preparing nanometer level high purity molybdenum trioxide according to claim 1, it is characterised in that：The spray
Emitter（22）Use the heat-resistance stainless steel of 310S materials.
4. a kind of application method of device for preparing nanometer level high purity molybdenum trioxide as described in claims 1 to 3 is any, bag
Include following steps：
1）Raw material molybdenum trioxide is passed through into raw material cabin（11）Deliver feeding machine（12）On, raw material molybdenum trioxide enters subliming furnace
（13）In, by subliming furnace（13）Interior temperature control is at 900-1100 DEG C；
2）Step 1）Obtained molybdenum trioxide steam is via VERTICAL TUBE（21）Enter injector（22）It is interior, circulation vacuum pump（24）
By circulatory pool（23）Interior coolant is extracted, and passes through conduit（25）From injector（22）Under top is drenched, complete to steam molybdenum trioxide
The cooling of vapour, molybdenum trioxide particles fall to circulatory pool（23）Bottom；
3）Open slush pump（31）, by circulatory pool（23）Interior molybdenum trioxide particles are drawn into flash vessel（32）In, to muddy
Molybdenum trioxide be dried；
4）Open surge drum（41）The air exhauster of side（45）, molybdenum trioxide particles enter air flow crushing device（33）In,
After the pulverized sub-sieve of grain, in filter element（43）In the presence of fall to finished product bin（42）.
5. a kind of application method of device for preparing nanometer level high purity molybdenum trioxide according to claim 4, its feature
It is：The step 2）In coolant be deionized water or alcohol.
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| US4551313A (en) * | 1984-02-27 | 1985-11-05 | Amax Inc. | Flash sublimation and purification of molybdenum oxide |
| US6468497B1 (en) * | 2000-11-09 | 2002-10-22 | Cyprus Amax Minerals Company | Method for producing nano-particles of molybdenum oxide |
| 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 |
| CN105347400B (en) * | 2015-12-04 | 2016-11-09 | 湖北中澳纳米材料技术有限公司 | A kind of device and method producing high-purity nm molybdenum trioxide |
| CN205575671U (en) * | 2016-05-05 | 2016-09-14 | 湖北中澳纳米材料技术有限公司 | Preparation nanometer high -purity molybdenum trioxide's device |
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