CN102126754A - Method and device for preparing nano bismuth trioxide by adopting high-frequency plasmas as heat source - Google Patents
Method and device for preparing nano bismuth trioxide by adopting high-frequency plasmas as heat source Download PDFInfo
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- CN102126754A CN102126754A CN 201110114239 CN201110114239A CN102126754A CN 102126754 A CN102126754 A CN 102126754A CN 201110114239 CN201110114239 CN 201110114239 CN 201110114239 A CN201110114239 A CN 201110114239A CN 102126754 A CN102126754 A CN 102126754A
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- bismuth trioxide
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Abstract
The invention discloses a method and device for preparing nano bismuth trioxide by adopting high-frequency plasmas as a heat source. The method comprises the steps of: putting metal bismuth or bismuth trioxide powder with particle size of not more than 0.1mm into a vertical reacting furnace through a composite feeding machine after being subjected to gas atomization to ensure that the powder is gasified in a high-temperature plasma arc region with a temperature of 6,000-10,000 DEG C, shock-chilling gaseous bismuth trioxide at an outlet of the reaction furnace by using compressed air to be below 120 DEG C, and collecting to obtain the nano bismuth trioxide. In the invention, the metal bismuth or bismuth trioxide powder is uniformly fed by adopting the composite feeding machine creatively, and thus particle size distribution uniformity is ensured; the nano bismuth trioxide is produced by adopting the high-frequency plasmas as the heat source and using the steps of instantly gasifying bismuth oxides into steam and rapidly chilling; and the produced nano bismuth trioxide product has high purity, an average particle size of 20-60nm and specific surface area of 48-75m<2>/g, is not easy to agglomerate, and can be continuously produced.
Description
Technical field
The present invention relates to the bismuthous oxide bismuth trioxide technical field, particularly relating to a kind of is method and the device that thermal source prepares the nanometer bismuthous oxide bismuth trioxide with the high frequency plasma.
Background technology
Bismuth oxide is a kind of important function powder body material, is widely used in fields such as inorganic synthetic, electronic ceramics, chemical reagent, is mainly used in the manufacturing ceramic capacitor, also can be used for making electronic ceramics elements such as piezoelectric ceramics, voltage dependent resistor.And nano bismuth oxide except character and purposes with common bismuth oxide powder, also can be used for electronic material, superconducting material, specific function stupalith, cathode tube inner-wall paint etc. have particular requirement to granularity occasion because granularity is thinner.
Application number is that 200410026454.2 Chinese patent discloses " a kind of electron grade bismuth oxide micropowder preparing process ", be to prepare bismuth oxide micro-powder with the precipitator method, precipitate Bismuth trinitrate, add tween or tripoly phosphate sodium STPP dispersion agent simultaneously with KOH, obtain the superfine bismuth oxide of 1.5 μ m; Application number is that 200310110558.7 Chinese patent disclosed " preparation technology of nano bismuth oxide " and application number are that 200310121804.9 Chinese patent disclosed " preparation method of bismuth oxide micro-powder " is the precipitator method and prepares the nanometer bismuthous oxide bismuth trioxide, the product cut size that obtains is micron order, though these methods have obtained some effects, but still have some limitations: the shortcoming of this method is the accurately control of processing condition needs, and use alkali lye in the production process, inevitably bring basic metal or alkaline-earth metal ions into, thereby influence the purity of bismuth oxide, and the selection of alkali lye, the composition of dispersion agent and concentration also are the difficult points of bismuth oxide particle diameter and size-grade distribution, also can bring environmental pollution simultaneously.
Application number is the Chinese patent of 200910043778.X, disclosed is that the employing DC arc plasma is that thermal source is the technology of the ultra-fine bismuthous oxide bismuth trioxide of raw material production with the bismuth metal, the purity of the product that obtains reaches more than 99.9%, median size is less than 100nm, but this method is difficult to realize the serialization of producing because electrode can serious be ablated in oxygen-enriched environment.
Summary of the invention
Technical problem to be solved by this invention is to overcome that existing bismuthous oxide bismuth trioxide grain size of micropowder is big, working condition is difficult to control, can bring defective such as environmental pollution, and providing a kind of is method and the device that thermal source prepares the nanometer bismuthous oxide bismuth trioxide with the high frequency plasma.
In order to solve the problems of the technologies described above, the present invention adopts following technical scheme:
The present invention is the method that thermal source prepares the nanometer bismuthous oxide bismuth trioxide with the high frequency plasma: the bismuth metal or the bismuthous oxide bismuth trioxide powder that granularity are no more than 0.1mm drop in the vertical response stove after gas atomization by compound feeding device, powder is gasified in 6000～10000 ℃ high-temperature plasma arc district, the gaseous state bismuthous oxide bismuth trioxide in the Reaktionsofen exit with below the pressurized air quick cooling to 120 ℃, collect, promptly.Because the viscosity of powder is bigger, also might be agglomerating even drop into the vertical response stove through compound feeding device, agglomerating powder can not fully gasify in Reaktionsofen, influence product yield and size-grade distribution, entering the vertical response stokehold,, with dispelling by agglomerating powder powder is fully atomized with gas, to improve the product yield.
In the preceding method, the gasification time of powder in Reaktionsofen is controlled at more than the 0.05s, the residence time is controlled at more than the 0.2s.
In the preceding method, the charging capacity of bismuth metal or bismuthous oxide bismuth trioxide powder is 0.08～0.15kg/kwh by the power calculation of plasma generator.
Further, the charging capacity of bismuth metal or bismuthous oxide bismuth trioxide powder is 0.08～0.10kg/kwh by the power calculation of plasma generator.
In the preceding method, when cooling bismuth oxide compound, compressed-air actuated input tolerance is 20～35 times of gaseous state bismuthous oxide bismuth trioxide vapor volume.
Aforementioned is that thermal source prepares in the method for nanometer bismuthous oxide bismuth trioxide with the high frequency plasma, and the temperature of the bismuthous oxide bismuth trioxide steam after the control gasification is higher than 2000 ℃.When being higher than 2000 ℃, Qi Hua bismuth metal or bismuthous oxide bismuth trioxide powder can further not gasify.
Aforementioned is that thermal source prepares in the method for nanometer bismuthous oxide bismuth trioxide with the high frequency plasma, and used compound feeding device is made of load hopper that has agitator and oscillating feeder.
The present invention also provides a kind of device that is exclusively used in aforementioned nanometer bismuthous oxide bismuth trioxide production method, comprise plasma generator, Reaktionsofen and quench gas port, Reaktionsofen is vertical Reaktionsofen, the feeding device of this production equipment comprises load hopper and oscillating feeder, agitator is housed in load hopper, the feed bin of oscillating feeder is stretched in the lower end of load hopper, oscillating feeder links to each other with filling tube, atomizing tracheae and filling tube are communicated with, filling tube links to each other with plasma generator, the lower end of plasma generator connects vertical Reaktionsofen, and vertical Reaktionsofen outside is surrounded by cooling layer, the quench gas port be positioned at vertical Reaktionsofen below.
Preferably, in the said apparatus, atomizing tracheae 5 and filling tube 6 tangentially are communicated with.Tangential connection can make air-flow form whirlpool in filling tube, can not blow to powder on the wall of filling tube.
Compared with prior art, because the viscosity of bismuth metal or bismuthous oxide bismuth trioxide powder is bigger, mobile relatively poor, adopt conventional feed-type to cause feed inhomogeneous and influence the size-grade distribution of product easily, the compound feeding device even feeding of the employing of novelty of the present invention and through gas atomization, guarantee even particle size distribution, the employing high frequency plasma is a thermal source, bismuth metal or bismuthous oxide bismuth trioxide moment gasification are come production nanometer bismuthous oxide bismuth trioxide for steam and fast quench, the purity height of gained finished product, adopt high frequency plasma method and vertical response stove, because adding powder, institute under action of gravity, passes through whole plasma flame, made full use of high temperature heat source, the median size of gained nanometer bismuthous oxide bismuth trioxide is 20～60nm, specific surface area is 48～75 ㎡/g, be difficult for reuniting, because high frequency plasma is an induction discharge, working medium is an air, without any pollution, there is not the loss of electric machine, can continuous production, it is simple that the inventive method has equipment, easy handling, characteristics such as the products obtained therefrom quality is good.
Description of drawings
Fig. 1 is a production equipment structural representation of the present invention.
Embodiment
The production equipment of nanometer bismuthous oxide bismuth trioxide as shown in Figure 1, this device adopts compound feeding device to feed in raw material, compound feeding device comprises load hopper 2 and oscillating feeder 4, agitator 1 is housed in load hopper 2, the feed bin 3 of oscillating feeder 4 is stretched in the lower end 21 of load hopper 2, oscillating feeder 4 links to each other with filling tube 6, atomizing tracheae 5 tangentially is communicated with filling tube 6, filling tube 6 links to each other with plasma generator 7, the lower end of plasma generator 7 connects vertical Reaktionsofen 11, vertical Reaktionsofen 11 outsides are surrounded by cooling layer 9, quench gas port one 2 be positioned at vertical Reaktionsofen 11 below.
Granularity is no more than the bismuthous oxide bismuth trioxide powder of 0.1mm, and (Chemical Composition is Bi
2O
399.63%, Cu 0.003%, Sb 0.02%, Al 0.005%, Fe 0.002%, surplus is other impurity) send in the arc district of plasma generator 7 by filling tube 6 after 5 atomizings of atomizing tracheae by compound feeding device, the power input of plasma generator 7 is that 100KW, work gas are that the air plasma temperature of air, generation is 6000～10000 ℃, and work tolerance is 25m
3/ h, the charging capacity of bismuthous oxide bismuth trioxide powder is 0.1kg/kwh by the power calculation of plasma generator, per hour drop into the 10kg powder, powder is gasified in 6000～10000 ℃ high-temperature plasma arc district, plasma generator 7 is vertically installed, the high-temperature plasma that produces enters vertical response stove 11 by the junction, the bismuthous oxide bismuth trioxide powder is the gaseous state bismuthous oxide bismuth trioxide by the high-temperature plasma gasification, the powder that is not in time gasified then enters in the Reaktionsofen 11 under the effect of gravity, by work tolerance, charging capacity and lamp torch volumetrical mate controls the gasification time of powder in the plasma arcs district more than 0.05s, the residence time in Reaktionsofen is controlled at more than the 0.2s, the first half at the vertical response stove adopts stainless steel water jacket or air cooling chuck to make cooling layer 9, the temperature of the bismuthous oxide bismuth trioxide steam after the control gasification is higher than 2000 ℃, the powder that is not in time gasified turns to bismuthous oxide bismuth trioxide in the temperature therapeutic method to keep the adverse qi flowing downward more than 2000 ℃, and the high-boiling-point impurity in the powder then falls to furnace bottom.In the outlet of vertical response stove 11, obtain the reaction product formed by plasma tail flame and gaseous state bismuthous oxide bismuth trioxide, the temperature of control reaction product is greater than 2000 ℃, is compressed air quenchedly in the exit, and the air supply that quench gas port one 2 feeds is 800m
3/ h, pressurized air stream sharply are cooled to product below 120 ℃, and cooled gas adopts traditional receipts powder technology, by induced draft fan through the nanometer collector filter finished product.
Finished product has following characteristic:
Specific surface area: adopt ST-A08 specific surface area and determinator, measurement result is 47.73 ㎡/g;
Granularity: adopt Japanese 3014X ray diffraction-spectrograph of science, measuring median size by ISO/TS13762 and GB/T13221 is that 58.5nm, middle particle diameter are 17.5nm; Adopt H-700 type TEM to amplify 70,000 times, the detected result size range is at 10～50nm;
Main chemical, Bi
2O
399.91%, Cu 0.001%, Sb 0.001%, Al 0.001%, Fe 0.002%.
Claims (9)
1. with the high frequency plasma method that thermal source prepares the nanometer bismuthous oxide bismuth trioxide, it is characterized in that: the bismuth metal or the bismuthous oxide bismuth trioxide powder that granularity are no more than 0.1mm drop in the vertical response stove after gas atomization by compound feeding device, powder is gasified in 6000～10000 ℃ high-temperature plasma arc district, the gaseous state bismuthous oxide bismuth trioxide in the Reaktionsofen exit with below the pressurized air quick cooling to 120 ℃, collect, promptly.
2. described according to claim 1 is the method that thermal source prepares the nanometer bismuthous oxide bismuth trioxide with the high frequency plasma, it is characterized in that: the residence time that the gasification time of powder in high-temperature plasma arc district is controlled at more than the 0.05s, in the vertical response stove is controlled at more than the 0.2s.
3. described according to claim 1 is the method that thermal source prepares the nanometer bismuthous oxide bismuth trioxide with the high frequency plasma, it is characterized in that: the charging capacity of bismuth metal or bismuthous oxide bismuth trioxide powder is 0.08～0.15kg/kwh by the power calculation of plasma generator.
4. described according to claim 3 is the method that thermal source prepares the nanometer bismuthous oxide bismuth trioxide with the high frequency plasma, it is characterized in that: described charging capacity is 0.08～0.10kg/kwh.
5. described according to claim 1 is the method that thermal source prepares the nanometer bismuthous oxide bismuth trioxide with the high frequency plasma, it is characterized in that: compressed-air actuated input tolerance is 20～35 times of gaseous state bismuthous oxide bismuth trioxide vapor volume.
According to described according to claim 1 be the method that thermal source prepares the nanometer bismuthous oxide bismuth trioxide with the high frequency plasma, it is characterized in that: the temperature of the bismuthous oxide bismuth trioxide steam after the control gasification is higher than 2000 ℃.
7. described according to claim 1 is the method that thermal source prepares the nanometer bismuthous oxide bismuth trioxide with the high frequency plasma, it is characterized in that: described compound feeding device is made of load hopper that has agitator and oscillating feeder.
8. the production equipment of nanometer bismuthous oxide bismuth trioxide, comprise plasma generator (7), Reaktionsofen (11) and quench gas port (12), it is characterized in that: described Reaktionsofen (11) is vertical Reaktionsofen, the feeding device of this production equipment comprises load hopper (2) and oscillating feeder (4), agitator (1) is housed in load hopper (2), the feed bin (3) of oscillating feeder (4) is stretched in the lower end (21) of load hopper (2), oscillating feeder (4) links to each other with filling tube (6), atomizing tracheae (5) is communicated with filling tube (6), filling tube (6) links to each other with plasma generator (7), the lower end of plasma generator (7) connects vertical Reaktionsofen (11), vertical Reaktionsofen (11) outside is surrounded by cooling layer (9), quench gas port (12) be positioned at vertical Reaktionsofen (11) below.
9. according to the production equipment of the described nanometer bismuthous oxide bismuth trioxide of claim 8, it is characterized in that: atomizing tracheae (5) tangentially is communicated with filling tube (6).
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1083538A (en) * | 1992-08-29 | 1994-03-09 | 中国科学院化工冶金研究所 | The preparing zinc-oxide by use of plasma method Processes and apparatus |
| CN1657421A (en) * | 2005-01-06 | 2005-08-24 | 贵州省冶金设计研究院 | Production method and device of nanmeter antimong trioxide |
| CN201372128Y (en) * | 2009-03-04 | 2009-12-30 | 中国石油天然气股份有限公司 | Delivery device for preventing bridging of powder |
| WO2010076632A2 (en) * | 2008-12-29 | 2010-07-08 | Vive Nano, Inc. | Nano-scale catalysts |
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2011
- 2011-05-05 CN CN 201110114239 patent/CN102126754A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1083538A (en) * | 1992-08-29 | 1994-03-09 | 中国科学院化工冶金研究所 | The preparing zinc-oxide by use of plasma method Processes and apparatus |
| CN1657421A (en) * | 2005-01-06 | 2005-08-24 | 贵州省冶金设计研究院 | Production method and device of nanmeter antimong trioxide |
| WO2010076632A2 (en) * | 2008-12-29 | 2010-07-08 | Vive Nano, Inc. | Nano-scale catalysts |
| CN201372128Y (en) * | 2009-03-04 | 2009-12-30 | 中国石油天然气股份有限公司 | Delivery device for preventing bridging of powder |
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Application publication date: 20110720 |