CN101372317B - Method for producing high quality nanometer oxide by gas phase method - Google Patents
Method for producing high quality nanometer oxide by gas phase method Download PDFInfo
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- CN101372317B CN101372317B CN2008102334035A CN200810233403A CN101372317B CN 101372317 B CN101372317 B CN 101372317B CN 2008102334035 A CN2008102334035 A CN 2008102334035A CN 200810233403 A CN200810233403 A CN 200810233403A CN 101372317 B CN101372317 B CN 101372317B
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- 238000004519 manufacturing process Methods 0.000 title claims description 14
- 239000007789 gas Substances 0.000 claims abstract description 41
- 239000000843 powder Substances 0.000 claims abstract description 32
- 239000002245 particle Substances 0.000 claims abstract description 25
- 238000002485 combustion reaction Methods 0.000 claims abstract description 22
- 238000000926 separation method Methods 0.000 claims abstract description 14
- 238000005189 flocculation Methods 0.000 claims abstract description 13
- 230000016615 flocculation Effects 0.000 claims abstract description 13
- 239000007787 solid Substances 0.000 claims abstract description 13
- 230000000694 effects Effects 0.000 claims abstract description 9
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 8
- 239000001257 hydrogen Substances 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims description 18
- 239000000463 material Substances 0.000 claims description 17
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 14
- 239000008246 gaseous mixture Substances 0.000 claims description 11
- 239000000443 aerosol Substances 0.000 claims description 10
- 239000007795 chemical reaction product Substances 0.000 claims description 10
- 239000011164 primary particle Substances 0.000 claims description 10
- DUNKXUFBGCUVQW-UHFFFAOYSA-J zirconium tetrachloride Chemical compound Cl[Zr](Cl)(Cl)Cl DUNKXUFBGCUVQW-UHFFFAOYSA-J 0.000 claims description 10
- 238000006460 hydrolysis reaction Methods 0.000 claims description 9
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 8
- 239000005049 silicon tetrachloride Substances 0.000 claims description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 239000012159 carrier gas Substances 0.000 claims description 6
- 239000004744 fabric Substances 0.000 claims description 6
- 239000002737 fuel gas Substances 0.000 claims description 6
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims description 6
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 6
- 239000006096 absorbing agent Substances 0.000 claims description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 239000011552 falling film Substances 0.000 claims description 5
- 230000005484 gravity Effects 0.000 claims description 5
- 230000007062 hydrolysis Effects 0.000 claims description 5
- 229910052760 oxygen Inorganic materials 0.000 claims description 5
- 239000001301 oxygen Substances 0.000 claims description 5
- 239000007921 spray Substances 0.000 claims description 5
- 238000010521 absorption reaction Methods 0.000 claims description 4
- 230000001133 acceleration Effects 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 4
- 229910052810 boron oxide Inorganic materials 0.000 claims description 4
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 claims description 4
- 230000003301 hydrolyzing effect Effects 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 239000004482 other powder Substances 0.000 claims description 4
- 238000010926 purge Methods 0.000 claims description 4
- 238000004062 sedimentation Methods 0.000 claims description 4
- 239000006200 vaporizer Substances 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000003570 air Substances 0.000 claims description 2
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 2
- 239000000292 calcium oxide Substances 0.000 claims description 2
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 2
- 239000000446 fuel Substances 0.000 claims description 2
- 229910052736 halogen Inorganic materials 0.000 claims description 2
- 150000002367 halogens Chemical class 0.000 claims description 2
- 239000000413 hydrolysate Substances 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 2
- 239000002105 nanoparticle Substances 0.000 abstract description 9
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- 238000005054 agglomeration Methods 0.000 abstract 1
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- 239000013078 crystal Substances 0.000 abstract 1
- -1 halide salt Chemical class 0.000 abstract 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 abstract 1
- 238000011031 large-scale manufacturing process Methods 0.000 abstract 1
- 238000000746 purification Methods 0.000 abstract 1
- 239000003381 stabilizer Substances 0.000 abstract 1
- 239000012071 phase Substances 0.000 description 12
- 239000012808 vapor phase Substances 0.000 description 11
- 239000000047 product Substances 0.000 description 6
- 239000000567 combustion gas Substances 0.000 description 4
- 239000011858 nanopowder Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
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- 238000010079 rubber tapping Methods 0.000 description 2
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- 229910052796 boron Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000004581 coalescence Methods 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- TXKMVPPZCYKFAC-UHFFFAOYSA-N disulfur monoxide Inorganic materials O=S=S TXKMVPPZCYKFAC-UHFFFAOYSA-N 0.000 description 1
- 239000012065 filter cake Substances 0.000 description 1
- 230000003311 flocculating effect Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- FDNAPBUWERUEDA-UHFFFAOYSA-N silicon tetrachloride Chemical class Cl[Si](Cl)(Cl)Cl FDNAPBUWERUEDA-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- XTQHKBHJIVJGKJ-UHFFFAOYSA-N sulfur monoxide Chemical compound S=O XTQHKBHJIVJGKJ-UHFFFAOYSA-N 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
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Abstract
The invention provides a new technique for producing high-quality nano oxide powder by using a gas phase method; the main process flow is as follows: metallic halide salt and a crystal stabilizing agent are vaporized at high temperature, premixed with hydrogen, air, and the like, and then undergo combustion reaction at a nozzle to generate nano particles; and the nano particles are treated by three-stage flocculation, three-stage gas-solid separation, surface deacidification, tail gas purification, and the like, to prepare the oxide powder. The technique has the advantages of high degree of serialization, advanced technology, low energy consumption, no pollution, high working reliability, good stability and small investment scale, and the produced nano oxide particles are characterized by high purity, high specific surface, high activity, no agglomeration, good dispersivity, narrow particle size distribution, and the like, thus fundamentally solving the difficult problem of large-scale production of high-purity nano oxides in industry.
Description
Technical field
The present invention relates to a kind of method of method for producing high quality nanometer oxide by gas phase, belong to technical field of nano material.
Background technology
Vapor phase process is a kind of chemical technology for preparing various high-quality nano particles, since superfine powder after particularly the potentiality of nano particle aspect performance application are excavated, its science and commercial value increase greatly, and vapor phase process has become very important technology in the nano oxide powder preparation.Although there is many difference in various vapor phase process synthesis techniques, but nano particle all has a common generting machanism when generating, and the quality product of nano particle and application performance mainly are by its size distribution and accumulation shape, i.e. granular size and determined jointly by the reunion degree institute of elementary nanoparticle subnumber definition.Producing with vapor phase process in the process of nano-oxide, the final performance of nanometer product is determined by hydromeehanics and particle dynamics in several milliseconds of time in synthesis technique early stage, in case primary particle is after flame zone forms, its cardinal trait has just been determined.In general, nanoparticle and gaseous mixture that flame zone forms have formed the aerosol material jointly, and how to control effectively the nanometer primary granule with nano-powder is effectively separated is that present vapor phase process is produced the hot issue that nano-powder is comparatively paid close attention to.
When using vapor phase process to produce nano-powder at present, filtering technique is mainly adopted in the separation of gas-solid, and existing filtering technique exists following point: (1) filter cloth easily stops up; (2) particle escapes was too much before filter cake formed; (3) because of the unstable product quality problem that brings in reaction zone pressure field; (4) need to clean continually and blowback.In addition, because nozzle is the single hole structure, combustion flame sprays from nozzle center, but because flame is generally " fusiform ", there is bigger thermograde in flame zone, must cause the track difference of nanometer primary particle experience; These problems cause existing fumed nano oxide diameter of particle distribute wide, technology is discontinuous, energy consumption is big, filter plant overload and unstable product quality.Therefore, be necessary fully prior art is improved.
Summary of the invention
For overcoming the prior art above shortcomings, the invention provides a kind of method of method for producing high quality nanometer oxide by gas phase, enable continuous production, the product purity height of producing, active high, size distribution is even, specific surface area is big, reunite less, the high quality nanometer oxide powder of good dispersity, the production of especially suitable nano zirconium oxide powder.
Second purpose of the present invention is to provide a kind of vapor phase process combustion reactions nozzle that uses in method for producing high quality nanometer oxide by gas phase, this nozzle is premixed, make flame present stratiform by this nozzle, the thermograde of this flame zone is very little, can make the track of primary particle process roughly suitable, can reach the effect of control nanoparticle growth by the ratio of pilot-gas flow velocity and unstripped gas.
The 3rd purpose of the present invention is to provide a kind of aerosol flocculation plant that uses in method for producing high quality nanometer oxide by gas phase.
First purpose of the present invention is finished by following technical proposal: a kind of method of method for producing high quality nanometer oxide by gas phase is characterized in that through the following step:
A, raw material are carried: utilize nitrogen or air as carrier gas, stablizer and zirconium tetrachloride or silicon tetrachloride are heated to 50-400 ℃ become raw material steam in vaporizer, with pressure is the carrier gas of 0.1-0.3Mpa, with the raw material delivery of steam to combustion reactions nozzle premix chamber, wherein the mol ratio of load volume and raw material quantity of steam is 1～3: 1, and the molar ratio of stablizer and zirconium tetrachloride or silicon tetrachloride is 1: 20-100;
The mixing of B, raw material and fuel: with temperature is that 350～500 ℃ hydrogen and oxygen or air are delivered to the premix chamber of combustion reactions nozzle as fuel gas, wherein the mol ratio of amounts of hydrogen and zirconium tetrachloride or silicon tetrachloride is controlled at 3～10: 1, the mol ratio of amount of oxygen and zirconium tetrachloride or silicon tetrachloride is controlled at 1～10: 1, the mixture of raw material steam and fuel gas is the high speed premix in combustion reactions nozzle premix chamber, and burning produces hydrolysis reaction;
Primary particle after C, the combustion reactions and mixed gas are through the combustion reactions nozzle, speed with 20～40m/s sprays in the hydrolysis stove burner hearth, combustion hydrolytic forms the aerosol material, and emit a large amount of heat, make the burner hearth reaction zone temperature reach 1400-2000 ℃, hydrolysate is primary particle, and all between the 4-20 nanometer, primary particle is calcined naturally through the furnace flame district and obtained stable crystalline phase reaction product and gaseous mixture;
D, with the crystalline phase reaction product and the gaseous mixture of C step, speed with 20～40m/s, deliver in the flocculator by burner hearth, the pilot-gas temperature is 105-150 ℃, allow reaction product successively through after the acceleration zone in the flocculator, the turbulent area flocculation, rely on the gravity sedimentation effect to be deposited to the negative area, to collect most of powder particle, all the other powder particles flow out with air-flow;
E, with the effusive residue powder particle of air-flow more successively after cyclonic separator, cloth bag collector filter, promptly get the powder after the gas solid separation;
F, the powder particle that D step and E step are obtained, send into the fluidized-bed extracting tower in the mode of gas delivery after, be 100 ℃～350 ℃ with temperature, absolute humidity is 30-100g/m
3Damp-heat air the depickling that powder carried out 0.5～2 hour is handled, obtain the deacidified prod that pH value is 4-6;
G, from D step flocculator, E step gas-solid filtering separation device, F step extracting tower come out contain acid gas and collect after, send into exhaust treatment system in the lump, behind falling-film absorber efficient absorption hydrogenchloride wherein, with routine techniques of the prior art and equipment hydrogenchloride is prepared into industrial hydrochloric acid, then emptying of Purge gas up to standard.
Described stablizer is one or more the mixing in sulfur oxide, boron oxide, titanium oxide or the calcium oxide, and its add-on is 1/20～1/100 of a metal halogen mol ratio.
The vaporizer of described A step is a conventional equipment of the prior art.
The hydrolysis stove of described C step, the cyclonic separator of E step, cloth bag collector, the fluidized-bed extracting tower of F step, the falling-film absorber of G step is conventional equipment of the prior art.
Second purpose of the present invention realizes by following technical proposal: a kind of vapor phase process combustion reactions nozzle, it is characterized in that comprising the cavity of carrying raw material inlet, fuel gas inlet on it, the nozzle of cavity bottom is by outer wall, be located at the plug at outer wall middle part, the annular channel between plug and outer wall is formed.So that gaseous mixture such as raw material, combustion gas, oxygenant outwards spray from the annular channel of nozzle.
The annular channel of described nozzle distance is between the 1mm-5mm, and the gas flow rate by nozzle is at 15m/s-50m/s.
The 3rd purpose of the present invention realizes by following technical proposal: a kind of aerosol flocculation plant, it is characterized in that being provided with in the housing of opening for feed, air outlet, discharge port thereon, be interval with staggered dividing plate group, the below, space between the dividing plate group is provided with discharge port.
Described housing is made as right cylinder, perhaps pros or rectangular parallelepiped, perhaps polygonal cylinder, the best is a rectangular parallelepiped, opening for feed on the housing and air outlet are arranged on the top of housing, and opening for feed and air outlet branch be arranged, and are advisable at the intravital passage length of shell to prolong material.
Staggered dividing plate group is made up of two dividing plates at least in the described housing, wherein an end of one is fixed on housing top, the other end is suspended from the housing, and an end of another piece is fixed on lower housing portion, the other end then is suspended from the housing, thereby forms staggered dividing plate group, makes material channel form long crooked road, make material between dividing plate, form long distance, high-speed turbulent flow, so that flocculation.
Clearance distance in the described housing between the staggered dividing plate group is made as equidistantly or is not equidistant, and to reduce the material flow by this interstitial area, the granule materials of being convenient to grow up is at this regional subsidence.
Each discharge port below of described lower housing portion is respectively equipped with the casing by band opening for feed, discharge port, inlet mouth on it, and is located at the material conveyer that rotating paddle constituted in the casing, and the discharge port of material conveyer is communicated with the mass transport road.
The casing of described material conveyer is a right cylinder, opening for feed on it is communicated with the housing discharge port that is positioned at the top, the casing upside is provided with the balance air flow inlet, discharge port on the casing is located at the right cylinder bottom, link to each other with the mass transport person in charge by the tapping channel that is obliquely installed, the end that mass transport is responsible for is communicated with the delivery air inlet, so that the material behind the flocculating settling is sent by delivery air after material conveyer enters the person in charge.
Rotating paddle in the described material conveyer casing is arranged on the axle on the case axis line, blade quantity is at least 2, so that from the material on top under the combined action of upper and lower two strands of air-flows, promote blade movement, be sent to by the rotation of blade in the person in charge of bottom, thereby realize the serialization convey materials.
Technology of the present invention compared with prior art has following advantage and effect: technology serialization degree height of the present invention; advanced technology, energy consumption is low, and is pollution-free; scale of investment is little; be suitable for large-scale industrial production, the nanometer oxide particle of production has the purity height, and specific surface area is big; active high; do not have and reunite good dispersity, characteristics such as narrow diameter distribution.Especially the setting of aerosol flocculation plant, the nanometer primary particle that vapor phase process is produced is finished coalescence and is grown up in this device, make most powder particle equivalent dimensions greater than 50 microns, thereby easily realize gravity separation, alleviate postorder filter plant working load greatly, guarantee constant product quality, reduce production costs.Technical process of the present invention is short, equipment used simple in structure, and the working reliability height, good stability has fundamentally solved the problem of the gas solid separation difficulty that industrial scale operation high quality nanometer oxide exists.
Description of drawings
Fig. 1 is a process flow sheet of the present invention;
Fig. 2 is an aerosol flocculation plant structural representation provided by the invention;
Fig. 3 is a vapor phase process combustion reactions nozzle arrangements synoptic diagram provided by the invention.
Embodiment
Below in conjunction with accompanying drawing apparatus of the present invention are described further.
As Fig. 2, the housing of aerosol flocculation plant provided by the invention is a rectangular parallelepiped 9, housing 9 is provided with opening for feed 1, air outlet 8 and three discharge ports 19,10,11, opening for feed 1 is arranged on housing 9 tops one side, air outlet 8 is arranged on housing 9 top opposite sides, discharge port 19,10,11 are made as taper, cone angle is 20 degree, the top of each discharge port corresponds to the space between the dividing plate group, promptly there is not baffle region (yet being the negative area) 3,5,7, rectangle housing 9 internal intervals are provided with staggered dividing plate group 2,4 and 6, the spacing between the dividing plate group 2 and 4,4 and 6 is made as not equidistant, wherein an end of several is fixed on housing 9 tops, the other end is suspended from the housing, and an end of several is fixed on housing 9 bottoms in addition, and the other end then is suspended from the housing, thereby form staggered dividing plate group, spacing between every dividing plate is 10cm, each discharge port 19,11,10 belows are respectively equipped with a spiral device for transporting objects, and the powder conveying that is used for will not having continuously baffle region is gone out.Wherein the spiral device for transporting objects comprises a cylindrical shell 17, cylindrical shell 17 inside are provided with one group of screw-blade 16, blade 16 activities are fixed in the rotating shaft of casing 17 centers, above the side of cylindrical shell 17, be provided with a balance air flow inlet 18, below cylindrical shell 17, be provided with the tapping channel 15 of inclination, this passage is responsible for 12 with feeding and is linked to each other, an end of the feeding person in charge 12 links to each other with a delivery air inlet 14, so that coming self-equilibrating airflow orifice 18 and delivery air to enter the mouth under the effect of 14 two strands of air-flows, promote blade 16 motions, thereby the feeding that will be sent to the bottom by the rotation of blade 16 from the material of upper part discharge port 19 is responsible in 12, thereby realizes the serialization mass transport.The below of same discharge port 11,10 is connected with identical spiral device for transporting objects, in this omission.
As Fig. 3, vapor phase process combustion reactions nozzle provided by the invention, the cavity 102 that comprises carrying raw material steam on it, stablizer inlet 103, fuel gas inlet 101, gas inlet 104, be the premix chamber in the cavity 102, the nozzle of cavity 102 bottoms is by outer wall 105, be located at the plug 106 at outer wall 105 middle parts, the annular channel 107 between plug 106 and outer wall 105 is formed, and the distance of annular channel 107 is 2mm.So that gaseous mixture such as raw material, combustion gas, oxygenant outwards spray from the annular channel of nozzle.
Below in conjunction with embodiment the present invention's processing method is described further.
The method of method for producing high quality nanometer oxide by gas phase provided by the invention, process the following step:
A, evaporator temperature is heated to 400 ℃, be 99.6% zirconium tetrachloride with purity with 10 moles/hour, purity be that 99% boron oxide is sent in the vaporizer with 0.03 mole/hour flow, when sending into zirconium tetrachloride and boron oxide, be as carrier gas with industrial nitrogen, load volume is 25 moles/hour, and delivers in the premix chamber 102 from the inlet 103 of combustion reactions nozzle under the pressure of 0.15Mpa;
B, be that 450 ℃ hydrogen is with 60 moles/hour with temperature simultaneously, the oxygen that with temperature is 450 ℃ is with 80 moles/hour flow, under the pressure of 0.15Mpa, enter in the nozzle premix chamber 102 from combustion reactions nozzle entrance 101 and 104 by utilidor respectively;
C, above-mentioned raw materials gas and combustion gas 102 mix after nozzle ring-type path 10 7 laminar flows are lighted to jet exit through nozzle premix chamber, and in hydrolysis stove burner hearth combustion hydrolytic, this hydrolysis reaction is emitted a large amount of heat, reaction zone temperature is reached about 1500 ℃, naturally calcine through flame zone and promptly to get stable crystalline phase reaction product and gaseous mixture, form aerosol;
D, with the reaction product and the gaseous mixture of C step, deliver in the flocculator through burner hearth, the pilot-gas temperature is 120 ℃, allow particle successively through after the acceleration zone in the flocculator, the turbulent area flocculation, rely on the gravity sedimentation effect to be deposited to the negative area, to collect most of powder particle, all the other powder particles flow out with air-flow;
E, with the effusive residue powder particle of air-flow more successively through cyclonic separator, cloth bag collector, promptly get the powder after the gas solid separation; Can reach more than 96% by powder collection rate after flocculation, the gas-solid filtering separation;
F, the powder particle that D step and E step are obtained, after sending into the fluidized-bed extracting tower in the gas delivery mode, be 300 ℃ with temperature, absolute humidity is that the hot damp-heat air of 50g/ cubic meter carries out clock time depickling in 50 fens to powder, getting purity is 99.4%, and specific surface area is less than 150m
2The high-quality fumed nano oxide powder of/g;
G, from D step flocculator, E step gas-solid filtering separation device, F step extracting tower come out contain acid gas and collect after, send into exhaust treatment system in the lump, with being prepared into industrial hydrochloric acid behind the falling-film absorber efficient absorption hydrogenchloride wherein, Purge gas emptying up to standard.
The method of method for producing high quality nanometer oxide by gas phase provided by the invention comprises:
A, carburettor temperature are heated to 100 ℃, with purity is 100 moles/hour of 99.6% silicon tetrachlorides, as carrier gas (dry air dew point-20 ℃), load volume is 150 moles/hour, delivers in the premix chamber 102 from the inlet 103 of combustion reactions nozzle under the pressure of 0.2Mpa with dry air;
B, it is 500 moles/hour with amounts of hydrogen simultaneously, flow with 1000 moles/hour of dry airs, hydrogen and dry air are heated to 400 ℃ respectively, under the pressure of 0.2Mpa, enter in the nozzle premix chamber 102 from combustion reactions nozzle entrance 101 and 104 by utilidor respectively;
C, above-mentioned raw materials gas and combustion gas 102 mix after nozzle ring-type path 10 7 laminar flows are lighted to jet exit through nozzle premix chamber, and in hydrolysis stove burner hearth combustion hydrolytic, this hydrolysis reaction is emitted a large amount of heat, the burner hearth reaction zone temperature is reached about 1450 ℃, naturally calcine through flame zone and to obtain stable crystalline phase reaction product and gaseous mixture, form aerosol;
D, with the reaction product and the gaseous mixture of C step, be delivered in the flocculator through burner hearth, the pilot-gas temperature is 130 ℃, allow particle successively through after the acceleration zone in the flocculator, the turbulent area flocculation, rely on the gravity sedimentation effect to be deposited to the negative area, to collect most of powder particle, all the other powder particles flow out with air-flow;
E, with the effusive residue powder particle of air-flow more successively through cyclonic separator, cloth bag collector, promptly get the powder after the gas solid separation; Can reach more than 98% by powder collection rate after flocculation, the gas-solid filtering separation;
F, the powder particle that D step and E step are obtained, after sending into the fluidized-bed extracting tower in the gas delivery mode, be 400 ℃ with temperature, absolute humidity is that the hot damp-heat air of 80g/ cubic meter carries out clock time depickling in 100 fens to powder, getting purity is 99.8%, and specific surface area is not less than 380m
2The high-quality fumed nano silica powder of/g;
G, from D step flocculator, E step gas-solid filtering separation device, F step extracting tower come out contain acid gas and collect after, send into exhaust treatment system in the lump, with being prepared into industrial hydrochloric acid behind the falling-film absorber efficient absorption hydrogenchloride wherein, Purge gas emptying up to standard.
Claims (2)
1. the method for a method for producing high quality nanometer oxide by gas phase is characterized in that through the following step:
A, raw material are carried: utilize nitrogen or air as carrier gas, stablizer and zirconium tetrachloride or silicon tetrachloride are heated to 50-400 ℃ become raw material steam in vaporizer, with pressure is the carrier gas of 0.1-0.3MPa, with the raw material delivery of steam to combustion reactions nozzle premix chamber, wherein the mol ratio of load volume and raw material quantity of steam is 1～3: 1, and the molar ratio of stablizer and zirconium tetrachloride or silicon tetrachloride is 1: 20-100;
The mixing of B, raw material and fuel: with temperature is that 350～500 ℃ hydrogen and oxygen or air are delivered to the premix chamber of combustion reactions nozzle as fuel gas, wherein the mol ratio of amounts of hydrogen and zirconium tetrachloride or silicon tetrachloride is controlled at 3～10: 1, the mol ratio of amount of oxygen and zirconium tetrachloride or silicon tetrachloride is controlled at 1～10: 1, the mixture of raw material steam and fuel gas is the high speed premix in nozzle premix chamber, and burning produces hydrolysis reaction;
Primary particle after C, the combustion reactions and mixed gas are through nozzle, speed with 20～40m/s sprays in the hydrolysis stove burner hearth, combustion hydrolytic forms the aerosol material, and emit a large amount of heat, make the burner hearth reaction zone temperature reach 1400 ℃-2000 ℃, hydrolysate is primary particle, and all between the 4-20 nanometer, primary particle is calcined naturally through the furnace flame district and obtained stable crystalline phase reaction product and gaseous mixture;
D, with the crystalline phase reaction product and the gaseous mixture of C step, speed with 20～40m/s, deliver in the flocculator by burner hearth, the pilot-gas temperature is 105-150 ℃, make reaction product successively through after the acceleration zone in the flocculator, the turbulent area flocculation, rely on the gravity sedimentation effect to be deposited to the negative area, to collect most of powder particle, all the other powder particles flow out with air-flow;
E, with the effusive residue powder particle of air-flow more successively after cyclonic separator, cloth bag collector filter, promptly get the powder after the gas solid separation;
F, the powder particle that D step and E step are obtained, send into the fluidized-bed extracting tower in the mode of gas delivery after, be 100 ℃～350 ℃ with temperature, absolute humidity is 30-100g/m
3Damp-heat air the depickling that powder carried out 0.5～2 hour is handled, the pH value be the deacidified prod of 4-6;
G, from D step flocculator, E step gas-solid filtering separation device, F step extracting tower come out contain acid gas and collect after, send into exhaust treatment system in the lump, behind falling-film absorber efficient absorption hydrogenchloride wherein, with routine techniques of the prior art and equipment hydrogenchloride is prepared into industrial hydrochloric acid, then emptying of Purge gas up to standard.
2. the method for method for producing high quality nanometer oxide by gas phase according to claim 1 is characterized in that described stablizer is one or more the mixing in boron oxide, titanium oxide or the calcium oxide, and its add-on is 1/20～1/100 of a metal halogen mol ratio.
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| CN103739014A (en) * | 2013-12-04 | 2014-04-23 | 首都师范大学 | Vapor phase method for controllable synthesis of biocompatible zirconium dioxide nano powder |
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| CN102513031B (en) * | 2011-11-30 | 2014-04-16 | 广州吉必盛科技实业有限公司 | Deacidification process and equipment thereof |
| CN104609375A (en) * | 2014-12-03 | 2015-05-13 | 胡晞 | Nano oxide composite powder and preparation method |
| CN108190950B (en) * | 2018-02-06 | 2020-10-27 | 新疆晶硕新材料有限公司 | Preparation method of zirconium dioxide |
| CN108557880B (en) * | 2018-03-08 | 2019-07-26 | 新疆晶硕新材料有限公司 | The preparation process of zirconium chloride and zirconium dioxide |
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