CN100462137C - Method for preparing nanopowder - Google Patents
Method for preparing nanopowder Download PDFInfo
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- CN100462137C CN100462137C CNB2006100981281A CN200610098128A CN100462137C CN 100462137 C CN100462137 C CN 100462137C CN B2006100981281 A CNB2006100981281 A CN B2006100981281A CN 200610098128 A CN200610098128 A CN 200610098128A CN 100462137 C CN100462137 C CN 100462137C
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Abstract
The invention relates to a method for preparing nanometer power, which uses gas-phase method and ceramic film separating technique to prepare nanometer power, wherein it comprises gas-phase reaction and ceramic film separation; it uses gas-phase method to prepare nanometer power which via ceramic film separator is stopped on the ceramic film; then uses pulse ejection of compressed gas to blow down the nanometer powder on the ceramic film tube and collect. The invention has simple method, operation on high temperature and high separating efficiency. And the nanometer powder has small size and high purity.
Description
Technical field
The present invention relates to a kind of preparation method of nano-powder, relate in particular to a kind of vapor phase method and the integrated method for preparing nano-powder of ceramic membrane isolation technics.
Background technology
The preparation method of nano-powder is a lot, mainly can be divided into solid phase method, liquid phase method and vapor phase method from preparation method's phase.Solid phase method time consumption and energy consumption wherein, the particle diameter that obtains is difficult to less than 1 μ m, and is prone to and forms uneven phenomenon; For grain forming and the activation that makes generation a roasting process is often arranged all in the liquid phase method, be easy to cause the decline of final nano material specific area like this and introduce impurity easily, thereby finally influence the performance of nano material, the gas phase rule mainly is to utilize the steam of volatile compound, generate needed compound by chemical reaction, rapid condensation, thus prepare all kinds of nano particles.The powder that vapor phase method prepares has evenly, the purity height, granularity is little, and plurality of advantages such as good dispersion (Pratsinis S E.FlameAerosol Synthesis of Ceramic Powder.Prog.Energy Combust Sci..1998,24:197-219).Wherein vapor phase method can be divided into vapor condensation method (PVD) again, chemical vapour deposition technique (CVD), plasma method, the spray burning method that flame is assisted, spray heating decomposition, gas-phase combustion method or the like.
At present, vapor phase method is to prepare high quality nano material method commonly used, but it exists the problem that product is collected difficulty again.Although can be used for the equipment of gas solid separation has a lot, as cyclone dust collectors, electrostatic precipitator, sack cleaner or the like, when but handling nano-powder synthetic in vapor phase method with their turnover rate often reach percent a few to tens of, and these collection process majorities can only be 400 ℃ of operations down, and vapor phase method when preparing nano-powder in the gas-phase reaction zone major part all have higher temperature (Generation of silicananoparticles from tetraethylorthosilicate (teos) vapor in a diffusionflame, Hee Doog Jang, Aerosol science and technology 1999; Temperaturefield distribution in spark plasma sintering of BN, Wang Yucheng, Wuhan University of Technology's journal).Comparatively tradition and common collection method are by a cold-trap gas phase nano powder to be cooled off, the rotation cold-trap that does not stop, with fixing scraper the nano-powder on the cold-trap wall is collected, efficient is low, complex operation, and to guarantee that whole collection process is in negative pressure (Chinese patent CN1488444A); Also the someone adopts electrostatic precipitator to collect the nano-powder for preparing in the vapor phase method, but before entering electrostatic precipitator, nano-powder to its temperature be between 100～400 ℃ by heat exchanger earlier, and will be by in the air-flow that contains nano-powder, feeding water or the adjusting of ammonia steam than resistance (Chinese patent CN1488444A).
The appearing as of advanced porous ceramic film solves the gas-solid separation difficult problem that various vapor phase methods prepare under the high temperature that occurs in the nano-powder process a kind of practicable new technique route is provided.The ceramic membrane technology is a kind of new separation technology, can higher temperature (more than 800 ℃), bigger pressure (0.1～10MPa) and bigger pH value scope in use.Ceramic membrane separates that to have energy consumption low, the separative efficiency height, and design, preparation and operating process are simple, advantage such as can at high temperature operate, in food industry, biological industry, medical industry, all there have been a lot of application in fields such as paper industry.Nanjing University of Technology has applied for relevant patented technology, successful application inorganic ceramic membrane carries out isolated by filtration to the nano-powder in the liquid, average pore size is that the ceramic membrane of 0.2 μ m has been obtained filter efficiency preferably to nano-titanium oxide, is that the efficient of holding back of the metallic nickel superfine powder of 50nm reaches more than 99.9% and average pore size is the ceramic membrane of 0.05 μ m to average grain diameter.
The example that ceramic membrane is handled the gas success is the used in electronic industry gas cleaning, and the product that provides as U.S.Filter company reaches 99.9999% to 0.01 μ m grit removal efficiency.A kind of new membrane filter of Ceramem company exploitation, it reaches more than 99.9% the dust removal efficiency of high-temperature gas, its pressure drop can compare that (Xu Nan is the developing history and the trend of an ancient unit of weight ceramic membrane diffusion barrier at ordinary times, powder technology 1997,3 (3): 43-48) with sack cleaner.But above-mentioned employing ceramic membrane carries out the process of gas solid separation all also directly to be connected with course of reaction, and the present invention is intended to ceramic membrane separated and collected nano-powder technology is applied in the production of fumed nano powder, develops new integrating process.
Summary of the invention
Technical problem to be solved by this invention is to prepare the nano-powder complex process in order to overcome existing vapor phase method, deficiencies such as yield is low and a kind of vapor phase method and the integrated method for preparing the nano-powder technology of ceramic membrane isolation technics are provided, the present invention can be in high-temperature operation, have the separative efficiency advantages of higher.
Technical scheme of the present invention is:
A kind of preparation method of nano-powder, it is characterized in that separating two parts by gas-phase reaction with ceramic membrane forms, the nano-powder that is prepared by vapor phase method is trapped within on the ceramic membrane by the ceramic membrane separator, adopts the pulse jet of Compressed Gas that the nano-powder on the ceramic-film tube is blown down and collected then.
Wherein said vapor phase method is vapor condensation method (PVD), chemical vapour deposition technique (CVD), plasma method, auxiliary spray burning method, spray heating decomposition, gas-phase combustion method or the induced with laser gas-phase chemical reaction method of flame.Described ceramic membrane separator is made up of metal shell and tubular ceramic membrane; The average pore size of ceramic membrane is 2-200nm, and its material is aluminium oxide, zirconia, titanium oxide or is the compound of two kinds of materials.According to the size of output, can freely adjust the quantity of ceramic-film tube in the ceramic membrane separator.
For various vapor phase methods, directly with the nano-powder that generates together with carrier gas, also can be under the effect of vavuum pump ceramic membrane separator by forming by series of ceramic film pipe, the carrier gas that contains nano-powder before this need not through any heat transmission equipment, and the back adopts compressed-air actuated pulse jet that the nano-powder on the ceramic-film tube is blown down and collected.
The integrating process that this invention is adopted is seen shown in Figure 1.Whole process of preparation is mainly separated two parts by gas-phase reaction with ceramic membrane and is formed.According to the needs of practical problem, the ceramic membrane separator both can place the gas-phase reaction intra-zone, also can separate with the gas-phase reaction zone.The gas-phase reaction that relates in this invention includes many types, belong to known technology, innovation of the present invention is embodied in to be carried out gas phase reaction process and ceramic membrane isolation technics integrated, simplified the collection process of the powder among the vapor phase method preparation technology greatly, improved collection efficiency the powder for preparing.
Beneficial effect:
1, technology of the present invention is simple, and having can be in high-temperature operation, separative efficiency advantages of higher.
2, utilize the ceramic membrane separation to combine the nano-powder for preparing and have uniform particles with vapor phase method, the purity height, granularity is little, advantages such as good dispersion.
Description of drawings
Fig. 1 is an integrating process block diagram of the present invention.
Fig. 2 separates integrated experiment flow figure for the auxiliary spray burning method of flame with ceramic membrane.
Fig. 3 is the XRD spectra of yittrium oxide.
The TEM photo of Fig. 4 yittrium oxide.
Fig. 5 spray heating decomposition separates integrated experiment flow figure with ceramic membrane.
Fig. 6 separates the integrated XRD spectra that makes nano-cerium oxide for spray heating decomposition with ceramic membrane.
Fig. 7 separates integrated experiment flow figure for gas-phase combustion with ceramic membrane.
1-air compressor machine wherein, 2-presoma, 3-atomizer, 4-ceramic membrane separator, 5-vavuum pump, 6-gas-phase reaction zone, 7-evaporimeter, 8-fuel steel cylinder, 9-burner, 10-flowmeter, 11-tail gas absorption bottle.
The specific embodiment
The auxiliary spray burning method of flame is separated integrated with ceramic membrane:
The auxiliary spray burning method of flame is that presoma is incorporated in the combustion flame with steam or by the mode of an atomizer with spraying, steam or droplet have formed aerosol, aerosol reacts at the high-temperature area of flame and generates a mixed system of middle element and products molecule, these molecules are again by surface reaction or intermolecular coalescence, reunite and form nano particle, way in the past is to connect a cloth-bag type gathering-device in the back, the present invention adopts the ceramic membrane isolation technics, nano particle is trapped on the ceramic-film tube of reaction zone top, adopts compressed-air actuated pulse jet that the nano-powder on the ceramic-film tube is blown down and collected after a period of time.The experiment flow figure of integrating process for this reason shown in Figure 2:
Be prepared as the object description detailed process with yittrium oxide, yttrium nitrate aqueous solution with 20% concentration is a presoma, and the employing high-purity methane is a fuel, and air is an oxidant, and air is divided into two-way one tunnel directly and the methane blended burning, the drop that another road after atomizing as the carrier gas band enters flame.The thermal-flame face that the premixed gas of methane and air forms provides reaction zone for the yttrium nitrate droplet, the entire reaction time is in Millisecond, the yittrium oxide that reaction obtains leaves the high-temperature region (1350-1500 ℃) of flame fast, cooling rapidly, intergranular reunion and continued growth take place simultaneously, through the separator that the alumina ceramic membrane that is 10nm by 6 average pore sizes constitutes, hold back and obtain final objective product nano yttrium oxide.Fig. 3 and Fig. 4 are the XRD spectra and the TEM photos of the nano yttrium oxide that synthesizes with this method.Can find out that the yittrium oxide for preparing by this method has good degree of crystallinity from XRD spectra, the size of the nano-powder that synthesizes as can be seen from the TEM photo is little, more even, basically between 20-30nm.The ceramic membrane separator reaches more than 99% for the yield of the product of preparation.
Spray heating decomposition separates integrated with ceramic membrane:
The spray burning method auxiliary with the flame of the foregoing description 1 has the spray heating decomposition of similarity to be meant: material liquid is dispersed into atomizer sprays into the high-temperature region thermal decomposition behind the droplet and produce corresponding nano-powder.The experiment flow figure of integrating process for this reason shown in Figure 5:
Be prepared as the object description detailed process with cerium oxide, with the cerous nitrate aqueous solution of 15% concentration is that presoma and air are together through an atomizer, be atomized into behind the drop in the pyroreaction boiler tube, through pervaporation and decomposition, it is the ceramic membrane separator that 200nm zirconia ceramics film constitutes by 6 average pore sizes that waste gas process under the booster action of vavuum pump that the nano-powder logotype that a series of reaction such as crystallization back produces produces places one of the high-temperature reactor bottom, thereby nano-powder is retained down.Fig. 6 is the XRD spectra of the nano-cerium oxide for preparing in this way, can find out that the cerium oxide purity for preparing by this method is high and have good degree of crystallinity from XRD spectra.Prepared nano-powder average grain diameter is 60nm, and the ceramic membrane separator reaches more than 99% the yield of product.
Gas-phase combustion separates integrated with ceramic membrane:
Organic precursor volatilization back oxidizing fire in flame forms oxide particle, holds back through ceramic membrane, separates with reacting gas, obtains required product.The experiment flow schematic diagram of integrating process for this reason shown in Figure 7:
Be prepared as the object description detailed process with the commercially available white carbon black of gas phase, presoma organosilicon (tetraethyl orthosilicate TEOS) is 170 ℃ of volatilizations down, and be introduced in the flame of acetylene and air formation, the organosilicon combustion decomposition becomes silica, steam, carbon dioxide, through a ceramic membrane separator that constitutes for the 30nm alumina ceramic membrane by 19 average pore sizes, collection obtains silica, i.e. the white carbon black of gas phase.The primary particle size of resulting silica is less than 15nm.The ceramic membrane separator reaches more than 99% the yield of product.
Claims (4)
1. the preparation method of a nano-powder, it is characterized in that separating two parts by gas-phase reaction with ceramic membrane forms, the nano-powder that is prepared by vapor phase method is trapped within on the ceramic membrane by the ceramic membrane separator, adopts the pulse jet of Compressed Gas that the nano-powder on the ceramic-film tube is blown down and collected then.
2. preparation method according to claim 1 is characterized in that described vapor phase method is vapor condensation method, chemical vapour deposition technique, plasma method, auxiliary spray burning method, spray heating decomposition, gas-phase combustion method or the induced with laser gas-phase chemical reaction method of flame.
3. preparation method according to claim 1 is characterized in that the ceramic membrane separator is made up of metal shell and tubular ceramic membrane.
4. preparation method according to claim 3, the average pore size that it is characterized in that ceramic membrane is the 2-200 nanometer, its material is aluminium oxide, zirconia, titanium oxide or is aforementioned any two kinds compound.
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| CNB2006100981281A CN100462137C (en) | 2006-12-06 | 2006-12-06 | Method for preparing nanopowder |
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| CNB2006100981281A CN100462137C (en) | 2006-12-06 | 2006-12-06 | Method for preparing nanopowder |
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| CN1994549A CN1994549A (en) | 2007-07-11 |
| CN100462137C true CN100462137C (en) | 2009-02-18 |
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| CN110526709B (en) * | 2019-09-12 | 2022-06-17 | 广东东方锆业科技股份有限公司 | Method for preparing composite zirconium oxide precursor by spray thermal decomposition method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5618475A (en) * | 1994-10-27 | 1997-04-08 | Northwestern University | Evaporator apparatus and method for making nanoparticles |
| CN1239010A (en) * | 1998-06-11 | 1999-12-22 | 中国科学院金属研究所 | Method and system for collecting nm-class powder |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5618475A (en) * | 1994-10-27 | 1997-04-08 | Northwestern University | Evaporator apparatus and method for making nanoparticles |
| CN1239010A (en) * | 1998-06-11 | 1999-12-22 | 中国科学院金属研究所 | Method and system for collecting nm-class powder |
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