CN103979587A - Device and method for preparing nano aluminium oxide powder by adopting argon-oxygen plasma - Google Patents
Device and method for preparing nano aluminium oxide powder by adopting argon-oxygen plasma Download PDFInfo
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- CN103979587A CN103979587A CN201410220743.XA CN201410220743A CN103979587A CN 103979587 A CN103979587 A CN 103979587A CN 201410220743 A CN201410220743 A CN 201410220743A CN 103979587 A CN103979587 A CN 103979587A
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Abstract
The invention discloses a device and a method for preparing nano aluminium oxide powder by adopting argon-oxygen plasma and aims at providing a device and a method for preparing nano aluminium oxide powder as the nano aluminium oxide powder has the excellent characteristics of high strength, high hardness and abrasion resistance and has a broad application prospect and a great commercial value. The device for preparing the nano aluminium oxide powder by adopting the argon-oxygen plasma comprises a reaction body, a vacuum machine set connected with the interior of the reaction body, a quartz tube arranged on the reaction body, a high frequency plasma generator arranged outside the quartz tube, a protective gas supply device, a working gas supply device, a feeding device, a cyclone dust catcher, a collection chamber connected with the cyclone dust catcher, a solid-gas separation dust removal chamber connected with the cyclone dust catcher and a tail gas treatment and discharge system. The prepared nano aluminium oxide powder has the characteristics that particle size is not more than 50nm and alpha-Al2O3 content is high, so that the nano aluminium oxide powder is obviously better than the prior art; the nano aluminium oxide powder can be widely applied to each filed and has a broad application prospect and a great commercial value.
Description
Technical field
The present invention relates to functional materials preparation and manufacture field, especially superfine powder preparation field, be specially a kind of argon-oxygen plasma and prepare nano alumina powder jointed devices and methods therefor.
Background technology
Materials science and technology are one of three large pillars of contemporary civilization, are also one of three marks of global new technology revolution, and it,, in the high speed development of current science and technology, plays basis and leading role.Therefore, be the needs of social development for the research of novel material, be also the guarantee of development in science and technology.
Along with high-tech development, society also more and more payes attention to novel material, and worker has given great concern to the exploitation of novel material and application both at home and abroad, and the especially various materials with specific function become the emphasis of people's research.Wherein, the super-refinement of various materials be it is believed that it is the basis of developing material research.Corresponding with material super-refinement is superfine powder, and so-called superfine powder typically refers to: yardstick is between molecule, between atom and macro object, and the micro mist of granularity within the scope of (1-100) nm.
And nano alumina powder jointed as the one in superfine powder, it is in 21st century novel material, one of output maximum, the output value is the highest, purposes is the widest tip materials.Nano alumina powder jointed have small-size effect, surface-interface effect, quantum size effect and a macroscopic quantum channel effect, optical, electrical, the magnetic, heat and the mechanical characteristics that have demonstrated that conventional material do not have.Therefore, a kind of new function material of nano alumina powder jointed conduct, is widely used in multiple fields such as optics, chemical industry and special cermacis.
Nano alumina powder jointed is the indispensable raw material of high-pressure sodium fluorescent tube, fluorescent material and support of the catalyst, utilizes its less primary particle characteristic, can reduce ceramic body sintering temperature.In some occasion, nano alumina powder jointedly also can be made into senior crucible, in order to replace expensive platinum crucible.Nano alumina powder jointed as one of special type function material, it accounts for 1/3rd left and right, particularly α-Al of whole superfine powders
2o
3powder owing to thering is high strength, high rigidity, resistance to wear, the excellent characteristic such as wear-resistant, corrosion-resistant, high temperature resistant, anti-oxidant, good insulating, surface-area are large, so nano aluminium oxide has special purposes at aspects such as catalysis, fire-retardant, sound insulation, insulation, fine ceramics, have broad application prospects and huge commercial value.
Based on this, the object of the present invention is to provide a kind of new argon-oxygen plasma to prepare nano alumina powder jointed devices and methods therefor.
Summary of the invention
Goal of the invention of the present invention is: for the excellent characteristic such as nano alumina powder jointedly have high strength, high rigidity, resistance to wear, have broad application prospects and huge commercial value, provide a kind of argon-oxygen plasma to prepare nano alumina powder jointed devices and methods therefor.The present invention relates to the preparation of nano aluminium oxide, belong to the technical field of preparation and the processing of advanced ceramics material.The prepared Nano-sized Alumina Powder of the present invention has particle diameter and is not more than 50nm, α-Al
2o
3content, compared with high, is significantly better than prior art.It can widespread use every field, has broad application prospects and huge commercial value.
To achieve these goals, the present invention adopts following technical scheme:
A kind of argon-oxygen plasma is prepared nano alumina powder jointed device, comprise reactant, with the inner vacuum unit being connected of reactant, be located at the silica tube in reactant, be positioned at the Radio-frequency plasma torch in silica tube outside, shielding gas feeding mechanism, working gas feeding mechanism, feeding device, cyclone, the collecting chamber being connected with cyclone, the solid and gas connected with cyclone separates dust settling chamber, vent gas treatment and blowdown system, described reactant comprises the reaction chamber for carrying out plasma reaction, shock chamber, described reaction chamber is fixedly connected with shock chamber, described silica tube is communicated with reaction chamber, described shielding gas feeding mechanism is communicated with the inwall of silica tube, the interface end of described working gas feeding mechanism is positioned at the interface end inner side of shielding gas feeding mechanism, the interface end of described feeding device is communicated with the interface end of working gas feeding mechanism, described cyclone is connected with shock chamber, described collecting chamber is positioned at the bottom of cyclone, described solid and gas separation dust settling chamber is positioned at the top of cyclone, described solid and gas separates dust settling chamber and is connected with blowdown system with vent gas treatment.
Shielding gas in described shielding gas feeding mechanism is oxygen, and the gas in described working gas feeding mechanism is argon oxygen gas mixture.
Described feeding device is induction heating device.
Described feeding device is temp. controllable resistance induction heating device.
Described solid and gas separates that dust settling chamber comprises housing, several are arranged on the polypropylene filter core in housing, and described polypropylene filter core is tangled and made by polypropylene superfine fiber hot melt.
Described shock chamber adopts water cooled double-layered cold-drawing seamless pipe to make.
Described shock chamber adopts the cold-drawing seamless pipe of water cooled double-layered Ti-0.8Ni-0.3Mo alloy to make.
Described cyclone adopts Ti-0.8Ni-0.3Mo alloy to make.
Also comprise the back-blowing device that is arranged on solid and gas separation dust settling chamber top, the blowback air that described back-blowing device adopts is argon gas.
Described back-blowing device is blow-back low pressure bubble.
Also comprise the blowback Controlling System being connected with back-blowing device.
Adopt aforementioned means to prepare nano alumina powder jointed method, comprise the steps:
(1) by AlCl
3pack in feeding device, open shielding gas feeding mechanism, working gas feeding mechanism simultaneously, in silica tube, pass into shielding gas, working gas, wherein shielding gas is between working gas and silica tube inwall;
(2) again by after the radio tube heating 20min-200min in Radio-frequency plasma torch power supply, open vacuum unit, making the vacuum tightness in reaction chamber is 10
3pa ~ 8*10
4pa, starts Radio-frequency plasma torch, makes one end near silica tube in reaction chamber form stable argon-oxygen plasma torch, and opens feeding device, makes the AlCl in feeding device
3be sublimed into rapidly gaseous state AlCl
3, gaseous state AlCl
3pass in argon-oxygen plasma torch, carry out replacement(metathesis)reaction, obtain reaction product;
(3) reaction product falls into shock chamber, and cooling fast, then enter and in cyclone, carry out flash liberation, flash liberation obtains alumina particle and gaseous mixture, alumina particle deposits in collecting chamber, and gaseous mixture enters solid and gas separation dust settling chamber and carries out secondary separation filtration, and the alumina particle that secondary separation obtains also enters in collecting chamber, tail gas enters in vent gas treatment and blowdown system and processes, and the alumina particle obtaining in collecting chamber is product;
In described step 2, the equation of replacement(metathesis)reaction is as follows: 4AlCl
3(gaseous state)+3O
2(plasma state)=2Al
2o
3(solid-state)+6Cl
2(gaseous state).
Reaction product falls into shock chamber, and cooling fast, then enter and in cyclone, carry out flash liberation, flash liberation obtains alumina particle and gaseous mixture, alumina particle deposits in collecting chamber, gaseous mixture enters solid and gas separation dust settling chamber and carries out secondary separation filtration, back-blowing device passes into argon gas to carrying out blowback in solid and gas separation dust settling chamber simultaneously, the alumina particle that secondary separation obtains also enters in collecting chamber, tail gas enters in vent gas treatment and blowdown system and processes, and the alumina particle obtaining in collecting chamber is product.
For foregoing problems, the present invention adopts argon-oxygen plasma precursor reactant to prepare nanometer Al
2o
3, and successfully develop preparation nanometer Al
2o
3equipment, its preparation method is provided simultaneously.The present invention is as the important step of preparing Nano-sized Alumina Powder, prepared nanometer Al
2o
3granularity be about about 50nm, and there is α-Al
2o
3content high, has industrialization throughput, can meet the nano alumina powder jointed needs of industrialized mass production, utilizes significant for the deep development of aluminum oxide.
Feeding device in the present invention is used for making powder or granular AlCl
3at 178 DEG C of AlCl that are sublimed into gaseous state
3thereby, realize replacement(metathesis)reaction.Feeding device can adopt the resistance induction heating of temperature-controlled.Reaction chamber in the present invention, for realizing 4AlCl
3(gaseous state)+3O
2(plasma state)=2Al
2o
3(solid-state)+6Cl
2(gaseous state) replacement(metathesis)reaction.While adopting device of the present invention, in reaction, oxygen mainly participates in replacement(metathesis)reaction with plasma state, can greatly improve reaction process, improves the turnover ratio of nano aluminium oxide.In the present invention, the gas in working gas feeding mechanism is argon oxygen gas mixture, and it,, in argon-oxygen plasma torch, not only can be used as AlCl
3→ Al
2o
3the thermal source of replacement(metathesis)reaction, and the oxonium ion of different valence state is provided, fully participate in the short period of time replacement(metathesis)reaction, further improve turnover ratio.Meanwhile, the shielding gas in shielding gas feeding mechanism is oxygen, by using oxygen as protection gas, can ensure the carrying out of replacement(metathesis)reaction, can pass through again oxygen cooling protection high purity quartz pipe, plays the object of killing two birds with one stone.
The optional cold-drawing seamless pipe with water cooled double-layered Ti-0.8Ni-0.3Mo alloy in shock chamber in the present invention is made, thereby have, intensity is high, solidity to corrosion good, thermotolerance high.Cyclone also can adopt Ti-0.8Ni-0.3Mo alloy material to make.Wherein, the major impetus of cyclone derives from vacuum unit exhausting, coordinates its internal structure to realize cyclone collection.In order to promote filter effect, solid and gas of the present invention separates dust settling chamber and comprises housing, several polypropylene filter cores, and polypropylene filter core is arranged in housing.Polypropylene filter core is tangled and is made by polypropylene superfine fiber hot melt, wherein polypropylene superfine fiber forms three-dimensional micropore structure at random in space, dimension aperture, hole, along filtrate flow to distribution gradient, integrates surface, deep layer, smart filtration, can hold back the impurity of different-grain diameter.
Separate the separating effect of dust settling chamber in order further to improve solid and gas, the present invention separates dust settling chamber top at solid and gas back-blowing device is set, and adopts argon gas as blowback air, carries out blowback.By which, can remove in proper order in time the nano alumina particles being attached on solid and gas separation dust settling chamber inner filter core, thereby ensure solid-gas separating power and dust collection effect, improve the purity of nano aluminium oxide.Meanwhile, blowback air separates dust settling chamber by solid and gas and enters in cyclone, forms convection current, thereby form the effect of similar screening with the gas from shock chamber, further improves the purity of nano aluminium oxide.
In conjunction with Figure of description 3, the present invention is further described.
First by the AlCl of solid or powdery
3pack in feeding device, whether other utility appliance of corresponding inspection is intact, prepares to start start.Open shielding gas feeding mechanism, working gas feeding mechanism simultaneously, in silica tube, pass into shielding gas, working gas, wherein shielding gas is between working gas and silica tube inwall.
By after the radio tube heating 20min-200min in Radio-frequency plasma torch power supply, open vacuum unit again, make the vacuum tightness in reaction chamber reach 10
3pa ~ 8*10
4pa, starts Radio-frequency plasma torch, makes one end near silica tube in reaction chamber form stable argon-oxygen plasma torch, and opens feeding device, makes the AlCl in feeding device
3be sublimed into rapidly gaseous state AlCl
3, gaseous state AlCl
3pass in argon-oxygen plasma torch, carry out replacement(metathesis)reaction, obtain reaction product.
The chlorine producing in replacement(metathesis)reaction and nano level aluminum oxide (being reaction product) are cooling fast in shock chamber, then enter and in cyclone, carry out flash liberation, most nano alumina particles is realized and being separated with chlorine, and deposit at collecting chamber, be that flash liberation obtains alumina particle and gaseous mixture, alumina particle deposits in collecting chamber, and gaseous mixture enters solid and gas separation dust settling chamber and carries out secondary separation filtration.The gaseous mixture that contains a small amount of nano alumina particles carries out secondary separation filtration, the alumina particle that secondary separation obtains also enters in collecting chamber, tail gas enters in vent gas treatment and blowdown system and processes, and the alumina particle obtaining in collecting chamber is product.
In vent gas treatment and blowdown system, can adopt the NaOH solution of titanium pump pump 15% to spray processing to the chlorine overflowing, tail gas reaches discharging standards, subsequently discharge.Wherein, vent gas treatment and blowdown system are mainly used in removing chlorine, and the present invention adopts titanium pump, the chlorine overflowing are sprayed to processing with 15% the NaOH aqueous solution.Tail gas must not exceed the regulation 0.50mg/m of State Environmental Protection Administration
3, otherwise forbid discharge.In addition, vacuum unit all adopts Polymer Structure, so that acidproof, alkaline-resisting and corrosion.
The present invention, as the important step of preparing nano aluminium oxide, uses argon-oxygen plasma, realizes 4AlCl
3(gaseous state)+3O
2(plasma state)=2Al
2o
3(solid-state)+6Cl
2(gaseous state) replacement(metathesis)reaction.Argon-oxygen plasma torch is used for providing AlCl
3→ Al
2o
3the thermal source of replacement(metathesis)reaction, also provided the oxonium ion of different valence state, thereby complete chemical reaction within the indoor shorter time of reaction, improved the productive rate of nano aluminium oxide, had significant progressive meaning; Working gas adopts argon gas and oxygen mixed gas, can maintain high-temperature plasma arc; Protection gas adopts oxygen, can not only reduce the impact of impurity on replacement(metathesis)reaction, by gas cooling, effectively protects silica tube simultaneously, extends the work-ing life of silica tube; The optional cold-drawing seamless pipe with water cooled double-layered Ti-0.8Ni-0.3Mo alloy in shock chamber is made, and has that intensity is high, solidity to corrosion good, thermotolerance high, thereby reaches cooling object fast; Solid and gas separates dust settling chamber and preferably adopts the entanglement of polypropylene superfine fiber hot melt to make PP filter core and configuration back-blowing device, reach the object that improves filtering accuracy, remove in proper order in time the nano alumina particles adhering on filter element, to ensure solid-gas separating power and dust collection effect simultaneously.Fig. 2 adopts the present invention to prepare the scanning electron microscope microgram (SEM) of nano aluminium oxide, and as shown in the figure, the size of nano aluminium oxide does not exceed 50nm, and has obvious agglomeration.
The present invention is as the important step of preparing nano aluminium oxide, prepared nano aluminium oxide not only has small-size effect, surface-interface effect, quantum size effect and macroscopic quantum channel effect, and have that true density is large, Mohs' hardness is high, the feature such as corrosion-resistant, easy-sintering and high-strength, the high-ductility at high temperature still having, good stability, can be used in the aspects such as electronic industry, biochemical ceramic, structural ceramics, function ceramics, is in the high-tech areas such as electronics, machinery, aviation, chemical industry, building materials.Meanwhile, experiment shows, the prepared Nano-sized Alumina Powder of the present invention has particle diameter and is not more than 50nm, α-Al
2o
3content, compared with high, is significantly better than prior art.
To sum up, the present invention prepares nano aluminium oxide industrialization to have established solid previous work basis, is a technology that using value is high, technology is perfect, easy to implement and invention, has wide market application foreground.
Brief description of the drawings
Examples of the present invention will be described by way of reference to the accompanying drawings, wherein:
Fig. 1 is the structural representation of apparatus of the present invention.
Fig. 2 adopts the present invention to prepare the scanning electron microscope microgram (SEM) of nano aluminium oxide.
Fig. 3 is process flow sheet of the present invention.
Mark in figure: 1, silica tube; 2, Radio-frequency plasma torch; 3, shielding gas feeding mechanism, 4, working gas feeding mechanism, 5, feeding device; 6, cyclone; 7, collecting chamber, 8, solid and gas separates dust settling chamber, 9, vent gas treatment and blowdown system; 10, reaction chamber, 11, shock chamber.
Embodiment
Disclosed all features in this specification sheets, or step in disclosed all methods or process, except mutually exclusive feature and/or step, all can combine by any way.
Disclosed arbitrary feature in this specification sheets, unless narration especially all can be replaced by other equivalences or the alternative features with similar object.,, unless narration especially, each feature is an example in a series of equivalences or similar characteristics.
Embodiment 1
This device comprises reactant, with the inner vacuum unit being connected of reactant, be located at the silica tube in reactant, be positioned at the Radio-frequency plasma torch in silica tube outside, shielding gas feeding mechanism, working gas feeding mechanism, feeding device, cyclone, the collecting chamber being connected with cyclone, the solid and gas connected with cyclone separates dust settling chamber, vent gas treatment and blowdown system, be arranged on the back-blowing device that solid and gas separates dust settling chamber top, the blowback Controlling System being connected with back-blowing device.Wherein, reactant comprises reaction chamber, shock chamber, and reaction chamber is fixedly connected with shock chamber, and silica tube is communicated with reaction chamber.Shielding gas feeding mechanism is communicated with the inwall of silica tube; the interface end of working gas feeding mechanism is positioned at the interface end inner side of shielding gas feeding mechanism; the interface end of feeding device is communicated with the interface end of working gas feeding mechanism; shielding gas in shielding gas feeding mechanism is oxygen; gas in working gas feeding mechanism is argon oxygen gas mixture; adopt this structure, silica tube inside is followed successively by silica tube, oxygen, argon oxygen gas mixture, gaseous state aluminum chloride from outside to inside.Cyclone is connected with shock chamber, and the reaction product in shock chamber can enter in cyclone, carries out flash liberation.Collecting chamber is positioned at the bottom of cyclone, solid and gas separation dust settling chamber is positioned at the top of cyclone, the nano alumina particles that flash liberation obtains deposits in collecting chamber, and the gaseous mixture that separation obtains enters in solid and gas separation dust settling chamber and carries out secondary separation.Solid and gas separates dust settling chamber and comprises housing, is arranged on the polypropylene filter core in housing, and polypropylene filter core is tangled and made by polypropylene superfine fiber hot melt, and in the present embodiment, polypropylene filter core adopts four.Separate dust settling chamber secondary separation through solid and gas, separate the alumina particle obtaining and also enter in collecting chamber, tail gas enters in vent gas treatment and blowdown system and processes, and after question response, the alumina particle obtaining in collecting chamber is product.In the process of secondary separation, blowback Controlling System can be controlled back-blowing device and carry out blowback, remove in proper order in time the alumina particle being attached on solid and gas separation dust settling chamber inner filter core, ensure that solid and gas separates solid and gas separating power and the dust collection effect of dust settling chamber, make long-time continuous prepare nano aluminium oxide becomes possibility simultaneously.In the present embodiment, feeding device is temp. controllable resistance induction heating device, solid-state or powder aluminum chloride can be heated into gaseous state, shock chamber adopts the cold-drawing seamless pipe of water cooled double-layered Ti-0.8Ni-0.3Mo alloy to make, and cyclone adopts Ti-0.8Ni-0.3Mo alloy to make.
Flow process of the present invention as shown in Figure 3.
1. first the AlCl3 of solid or powdery is packed in feeding device.Whether other utility appliance of corresponding inspection is intact, prepares to start start.Open shielding gas feeding mechanism, working gas feeding mechanism simultaneously, in silica tube, pass into oxygen, argon oxygen gas mixture.
2. again by after the radio tube heating 30min in Radio-frequency plasma torch power supply, open vacuum unit, make the vacuum tightness in reaction chamber reach 10
4pa left and right; Start Radio-frequency plasma torch, form argon-oxygen plasma torch stable and normal operation, and open feeding device, make the temperature rise to 300 DEG C in feeding device, the AlCl in feeding device
3be sublimed into rapidly gaseous state AlCl
3, gaseous state AlCl
3pass in argon-oxygen plasma torch, (replacement(metathesis)reaction formula is as follows: 4AlCl to carry out replacement(metathesis)reaction
3(gaseous state)+3O
2(plasma state)=2Al
2o
3(solid-state)+6Cl
2(gaseous state)), obtain reaction product, i.e. nano alumina particles.
3. the chlorine producing in replacement(metathesis)reaction and nano level aluminum oxide are cooling fast in shock chamber, and after cyclone, most nano alumina particles is realized and being separated with chlorine, and deposits at collecting chamber subsequently.Small part nano alumina particles by chlorine carry enter solid and gas separate dust settling chamber carry out secondary separation filtration, to guarantee maximum yield.Tail gas after solid and gas separates dust settling chamber enters in vent gas treatment and blowdown system to be processed, and the alumina particle obtaining in collecting chamber is product.
In vent gas treatment and blowdown system, adopt the NaOH solution of titanium pump pump 15% to spray processing to the chlorine overflowing, tail gas reaches discharging standards, subsequently discharge.
The present invention is not limited to aforesaid embodiment.The present invention expands to any new feature or any new combination disclosing in this manual, and the arbitrary new method disclosing or step or any new combination of process.
Claims (10)
1. an argon-oxygen plasma is prepared nano alumina powder jointed device, it is characterized in that, comprise reactant, with the inner vacuum unit being connected of reactant, be located at the silica tube in reactant, be positioned at the Radio-frequency plasma torch in silica tube outside, shielding gas feeding mechanism, working gas feeding mechanism, feeding device, cyclone, the collecting chamber being connected with cyclone, the solid and gas connected with cyclone separates dust settling chamber, vent gas treatment and blowdown system, described reactant comprises the reaction chamber for carrying out plasma reaction, shock chamber, described reaction chamber is fixedly connected with shock chamber, described silica tube is communicated with reaction chamber, described shielding gas feeding mechanism is communicated with the inwall of silica tube, the interface end of described working gas feeding mechanism is positioned at the interface end inner side of shielding gas feeding mechanism, the interface end of described feeding device is communicated with the interface end of working gas feeding mechanism, described cyclone is connected with shock chamber, described collecting chamber is positioned at the bottom of cyclone, described solid and gas separation dust settling chamber is positioned at the top of cyclone, described solid and gas separates dust settling chamber and is connected with blowdown system with vent gas treatment.
2. argon-oxygen plasma is prepared nano alumina powder jointed device according to claim 1, it is characterized in that, the shielding gas in described shielding gas feeding mechanism is oxygen, and the gas in described working gas feeding mechanism is argon oxygen gas mixture.
3. argon-oxygen plasma is prepared nano alumina powder jointed device according to claim 1, it is characterized in that, described feeding device is induction heating device.
4. prepare nano alumina powder jointed device according to argon-oxygen plasma described in claim 1-3 any one, it is characterized in that, described solid and gas separates that dust settling chamber comprises housing, several are arranged on the polypropylene filter core in housing, and described polypropylene filter core is tangled and made by polypropylene superfine fiber hot melt.
5. argon-oxygen plasma is prepared nano alumina powder jointed device according to claim 1, it is characterized in that, described shock chamber adopts water cooled double-layered cold-drawing seamless pipe to make.
6. prepare nano alumina powder jointed device according to argon-oxygen plasma described in claim 1-5 any one, it is characterized in that, also comprise the back-blowing device that is arranged on solid and gas separation dust settling chamber top, the blowback air that described back-blowing device adopts is argon gas.
7. argon-oxygen plasma is prepared nano alumina powder jointed device according to claim 6, it is characterized in that, described back-blowing device is blow-back low pressure bubble.
8. argon-oxygen plasma is prepared nano alumina powder jointed device according to claim 6, it is characterized in that, also comprises the blowback Controlling System being connected with back-blowing device.
9. the nano alumina powder jointed method of device preparation described in employing claim 1-5 any one, is characterized in that, comprises the steps:
(1) by AlCl
3pack in feeding device, open shielding gas feeding mechanism, working gas feeding mechanism simultaneously, in silica tube, pass into shielding gas, working gas, wherein shielding gas is between working gas and silica tube inwall;
(2) again by after the radio tube heating 20min-200min in Radio-frequency plasma torch power supply, open vacuum unit, making the vacuum tightness in reaction chamber is 10
3pa ~ 8*10
4pa, starts Radio-frequency plasma torch, makes one end near silica tube in reaction chamber form stable argon-oxygen plasma torch, and opens feeding device, makes the AlCl in feeding device
3be sublimed into rapidly gaseous state AlCl
3, gaseous state AlCl
3pass in argon-oxygen plasma torch, carry out replacement(metathesis)reaction, obtain reaction product;
(3) reaction product falls into shock chamber, and cooling fast, then enter and in cyclone, carry out flash liberation, flash liberation obtains alumina particle and gaseous mixture, alumina particle deposits in collecting chamber, and gaseous mixture enters solid and gas separation dust settling chamber and carries out secondary separation filtration, and the alumina particle that secondary separation obtains also enters in collecting chamber, tail gas enters in vent gas treatment and blowdown system and processes, and the alumina particle obtaining in collecting chamber is product;
In described step 2, the equation of replacement(metathesis)reaction is as follows: 4AlCl
3(gaseous state)+3O
2(plasma state)=2Al
2o
3(solid-state)+6Cl
2(gaseous state).
10. the nano alumina powder jointed method of device preparation described in employing claim 6-8 any one, is characterized in that, comprises the steps:
(1) by AlCl
3pack in feeding device, open shielding gas feeding mechanism, working gas feeding mechanism simultaneously, in silica tube, pass into shielding gas, working gas, wherein shielding gas is between working gas and silica tube inwall;
(2) again by after the radio tube heating 20min-200min in Radio-frequency plasma torch power supply, open vacuum unit, making the vacuum tightness in reaction chamber is 10
3pa ~ 8*10
4pa, starts Radio-frequency plasma torch, makes one end near silica tube in reaction chamber form stable argon-oxygen plasma torch, and opens feeding device, makes the AlCl in feeding device
3be sublimed into rapidly gaseous state AlCl
3, gaseous state AlCl
3pass in argon-oxygen plasma torch, carry out replacement(metathesis)reaction, obtain reaction product;
Reaction product falls into shock chamber, and cooling fast, then enter and in cyclone, carry out flash liberation, flash liberation obtains alumina particle and gaseous mixture, alumina particle deposits in collecting chamber, gaseous mixture enters solid and gas separation dust settling chamber and carries out secondary separation filtration, back-blowing device passes into argon gas to carrying out blowback in solid and gas separation dust settling chamber simultaneously, the alumina particle that secondary separation obtains also enters in collecting chamber, tail gas enters in vent gas treatment and blowdown system and processes, and the alumina particle obtaining in collecting chamber is product;
In described step 2, the equation of replacement(metathesis)reaction is as follows: 4AlCl
3(gaseous state)+3O
2(plasma state)=2Al
2o
3(solid-state)+6Cl
2(gaseous state).
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| CN112939038A (en) * | 2021-02-09 | 2021-06-11 | 东北大学 | Method for preparing aluminum oxide by using high-alumina fly ash based on chlorination-oxygen pressure conversion |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1381304A (en) * | 2002-01-08 | 2002-11-27 | 纪崇甲 | DC arc plasma equipment and process for preparing micron-class and nano-class powder material |
| CN2678760Y (en) * | 2004-02-25 | 2005-02-16 | 孙陶 | Prodn. appts. for synthetizing multi-kind of nano powders by utilizing plasma |
| CN101391306A (en) * | 2008-11-20 | 2009-03-25 | 核工业西南物理研究院 | Globular titanium micro-powder or ultra-micro powder preparation device and method |
| CN102464323A (en) * | 2010-11-04 | 2012-05-23 | 中国科学院过程工程研究所 | Method for preparing high-purity superfine zirconium boride powder by high-frequency plasma |
| CN102515233A (en) * | 2011-12-29 | 2012-06-27 | 中国科学院过程工程研究所 | Method and product for preparing aluminum oxide with hot plasma |
-
2014
- 2014-05-23 CN CN201410220743.XA patent/CN103979587B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1381304A (en) * | 2002-01-08 | 2002-11-27 | 纪崇甲 | DC arc plasma equipment and process for preparing micron-class and nano-class powder material |
| CN2678760Y (en) * | 2004-02-25 | 2005-02-16 | 孙陶 | Prodn. appts. for synthetizing multi-kind of nano powders by utilizing plasma |
| CN101391306A (en) * | 2008-11-20 | 2009-03-25 | 核工业西南物理研究院 | Globular titanium micro-powder or ultra-micro powder preparation device and method |
| CN102464323A (en) * | 2010-11-04 | 2012-05-23 | 中国科学院过程工程研究所 | Method for preparing high-purity superfine zirconium boride powder by high-frequency plasma |
| CN102515233A (en) * | 2011-12-29 | 2012-06-27 | 中国科学院过程工程研究所 | Method and product for preparing aluminum oxide with hot plasma |
Non-Patent Citations (3)
| Title |
|---|
| 王俊文等: ""RF-PCVD法制备纳米Al2O3粉体动力学模型的建立"", 《第五届全国材料与热加工物理模拟及数值模拟学术会议论文集》, 23 October 2006 (2006-10-23) * |
| 白杨柳等: ""高频感应热等离子体在微细球形粉体材料制备中的应用"", 《高压电技术》, vol. 39, no. 7, 31 July 2013 (2013-07-31), pages 1577 - 1583 * |
| 马兵等: ""等离子体法制备特种超细氧化铝"", 《化工进展》, no. 2, 31 December 1996 (1996-12-31), pages 28 - 31 * |
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| CN106693853A (en) * | 2015-11-12 | 2017-05-24 | 松下知识产权经营株式会社 | Fine particle production apparatus and fine particle production method |
| CN111777076A (en) * | 2020-08-18 | 2020-10-16 | 苏州英纳特纳米科技有限公司 | Equipment for preparing amorphous nano spherical silicon dioxide |
| CN112723399A (en) * | 2020-12-10 | 2021-04-30 | 合肥中航纳米技术发展有限公司 | Plasma arc flame combustion reaction system and method for preparing high-purity gamma-Al by using same2O3Method (2) |
| CN112939038A (en) * | 2021-02-09 | 2021-06-11 | 东北大学 | Method for preparing aluminum oxide by using high-alumina fly ash based on chlorination-oxygen pressure conversion |
| CN113373597A (en) * | 2021-06-02 | 2021-09-10 | 四川亿耐特新材料有限公司 | Method for manufacturing non-woven felt by pure PET composite long fiber |
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