CN1721328A - Method and apparatus for preparing fumed nano oxide - Google Patents
Method and apparatus for preparing fumed nano oxide Download PDFInfo
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- CN1721328A CN1721328A CN200510010829.0A CN200510010829A CN1721328A CN 1721328 A CN1721328 A CN 1721328A CN 200510010829 A CN200510010829 A CN 200510010829A CN 1721328 A CN1721328 A CN 1721328A
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- 239000007789 gas Substances 0.000 claims abstract description 107
- 239000000843 powder Substances 0.000 claims abstract description 66
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- 239000001257 hydrogen Substances 0.000 claims abstract description 20
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 17
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- 238000006460 hydrolysis reaction Methods 0.000 claims description 49
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- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 36
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- 150000001875 compounds Chemical class 0.000 claims description 8
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- 150000004820 halides Chemical class 0.000 claims description 2
- 238000009434 installation Methods 0.000 claims description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 2
- 230000001737 promoting effect Effects 0.000 claims description 2
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 2
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- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 4
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- OEYOHULQRFXULB-UHFFFAOYSA-N arsenic trichloride Chemical compound Cl[As](Cl)Cl OEYOHULQRFXULB-UHFFFAOYSA-N 0.000 description 2
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- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 2
- 239000012808 vapor phase Substances 0.000 description 2
- 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 description 1
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- Oxygen, Ozone, And Oxides In General (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The present invention is gas phase process and apparatus of preparing nanometer oxide. Pre-treated hydrogen containing fuel, oxygen containing oxidant, inert gas and metal or non-metal halogen salt are mixed and sprayed into flame hydrolyzing furnace for burning, so that the gaseous halogen salt is hydrolyzed with the produced gaseous water to produce oxide, which is first agglomerated in the cooling gas flow to form primary nanometer oxide particle and flocculated in the flocculating unit into oxide flock. Through gas-solid separation to separate out oxide powder and elimination of hydrogen halide in the surface of the powder inside a deacidification furnace, nanometer oxide powder is obtained. The burning nozzle of the hydrolyzing furnace is provided with mixing chamber and star vane for homogeneous mixing of gas flows. The product has purity higher than 99.9 %, particle size of 5-40 nm and specific surface area of 100-400 sq m/g.
Description
One. technical field: the present invention relates to a kind of method and apparatus for preparing fumed nano oxide, belong to chemical engineering technology preparation field.
Two. background technology: nano oxide powder is the important foundation raw material of current growing nano material industry, and nano oxide powder itself is exactly a principal item in the nano material.High-quality nano oxide powder is produced in mass-producing, serialization, is the foundation works in nano material technology and its industrialization process.As the white carbon black of vapor phase process, promptly particle diameter is 5～55nm, specific surface area 100～360m
2/ g, flocculus shape SiO
2Nano-powder has unique, irreplaceable strengthening action in fields such as rubber industry, organosilicon industry and coatings industries, has worldwide formed nearly 200,000 tons/year selling market at present; High-temperature nano TiO
2Powder (＜50nm is as the P25 powder) because of its significant photochemical catalysis, uv absorption property, is just progressively realized industrialization in fields such as environmental pollutant degradation treatment, household electrical appliance automatically cleaning (antibiotic) functional development, uvioresistant, sterilizing function fabrics.In addition; Such as Al
2O
3, ZnO, Fe
2O
3, SnO
2, Sb
2O
3Etc. numerous nano oxide powders, in plastics, rubber, coating, slurry and all kinds of field of compound material, the traditional performance of these materials produced significantly promoted, and the function of a lot of novelties occurred.Thereby the nano oxide powder technology of preparing with superfine granularity, excellent dispersiveness, abundant function of surface is showed its importance day by day.
The preparation method of known nm-class oxide powder is very many, mainly can be divided into physics method and chemical method, and the method that wherein has the technical scale meaning is also few.The one, evaporation one condensation method.Under high vacuum condition, make the evaporation of metal gasification, generate oxide compound, be gathered into high-quality nano-powder at cold zone with gas reaction with electrically heated (or electron beam heating system).The powder quality that this method is produced is very high, but productive rate lower, need high vacuum environment, batch production, the powder small scale, production cost is very high; The 2nd, plasma method.Under plasma ambient, gasified and reactant gases generates nano oxide powder as the metal of electrode.This method productive rate is higher, but the atmosphere temperature difficulty is controlled, powder is crossed over nanometer to submicron-scale, and broad particle distribution is of low quality, and is big to its technique controlling difficulty of multicomponent composite oxide powder (as the semi-conductor powder that need mix up, ITO, ATO, ZTO etc.); The 3rd, the wet-chemical precipitator method, this method are to allow metal ion in chemical solution under alkali or Acid precipitation agent effect, with oxyhydroxide or acidulants precipitation, after filtration, link acquisition oxide powders such as cleanings, drying, calcining, pulverizing.This method can obtain the powder of ten thousand tons of/year scales on the wall scroll production line, but the powder quality is too low, in solution, there is the tendency of inevitably reuniting between micelle, in thermal treatment link subsequently, form very strong bridging oxygen (hydroxyl) bonding between powder, make the serious deterioration of powder dispersity, thereby the powder of liquid-phase precipitation method preparation can not use generally as nano-powder.
1958, in the document of US2990249, disclose Degussa company and prepared the white carbon black (SiO of ultra tiny vapor phase process with the gas phase flame hydrolysis
2Particle) technology and hydrolysis stove nozzle arrangements, nozzle system has tentatively improved the stability of flame, substantially avoided the spray nozzle front end problem that scabs with the mechanical curettage method, but come the speed of controlled temperature and reaction with water spray at flame front, owing to add a large amount of water at home and abroad at the air-flow raw material, greatly reduce the technological advantage of flame hydrolysis as anhydrous dry method, it is even to be difficult to obtain particle diameter, the uniform single SiO of shape
2Particle; Degussa company is in disclosed US3954945 document in 1976 and in the Cabot company disclosed US4292290 document in 1981, on nozzle arrangements, improve, optimization on the combined process, solved the problem that scabs of flame-thrower nozzle front end, overcome the unstable of flame, but nozzle arrangements is too complicated, working accuracy is high, under flame high temperature, fragile, the manufacturing cost costliness.In Degussa company the document US in 1988 5762914, prepare TiO with the gas phase flame hydrolysis
2, SiO
2, Al
2O
3Ultra tiny composite particles should be admitted TiO
2Specific surface be easy to control, but SiO
2, Al
2O
3At TiO
2In shared proportion restive, do not solve raw material TiCl
4, SiCl
4, AlCl
3Gasification (evaporation) transportation problem.In the US6242373B1 document, prepare B with the gas phase flame hydrolysis
2O
3-SiO
2(TiO
2, Al
2O
3, ZrO) composite particles mixed powder, composite particles B
2O
3, SiO
2Specific surface and other powder proportion therein control easily, but the collection effciency of composite granule is lower, the gathering that does not have thoroughly to solve the composite particles problem of growing up.
Three. summary of the invention:
The purpose of this invention is to provide a kind of method and apparatus for preparing fumed nano oxide, the molecular water generation hydrolysis reaction that the volatile metal-salt raw material that pre-treatment is good generates with flame in the hot environment that oxyhydrogen flame produces, generate the oxide compound primary particle, separate the nano oxide powder that obtains 4-40nm through flocculation-solid and gas.
Technical scheme of the present invention is:
(1) technical process: Fig. 1 is a process flow sheet of the present invention, and Fig. 2 is a device connection diagram:
With hydrogen-containing fuel, oxygenated fuel, rare gas element, air carries out udst separation, dry, preheating, after the supercharging, be transported in the flame hydrolysis stove burner noz(zle) gas hybrid chamber, simultaneously volatile salt raw material is evaporated, and with rare gas element as carrier gas, be transported in the flame hydrolysis stove burner noz(zle) gas hybrid chamber and each road gas uniform mixing, and under promoting, pressurized air stream in the stove hall, burns, hydrolysis, the mixture that comes out from the burner hearth afterbody imports the one-level flocculator, separate in primary cyclone the flocculation back, tail gas imports the secondary flocculator, flocculation once more, in secondary cyclone, separate once more then,, after the powder device for filtering and collecting is collected for the third time, import device for absorbing tail gas and absorb the back emptying from the secondary cyclone tail gas discharged.After the depickling, collect in the depickling stove from the product oxide compound that primary cyclone, secondary cyclone, powder device for filtering and collecting obtain, obtain nano oxide powder through the product hopper.
(2) invention is finished according to the following steps:
1. raw material, fuel, rare gas element and pre-treatment thereof
With flow is 1.5～5m
3/ h hydrogen-containing fuel, flow are 0.8～15m
3The oxygenated fuel of/h, flow are 0.4～6m
3The rare gas element of/h, air carry out udst separation remove moisture, oil content under 99.0% unbound state, be dried to dew point and be lower than-12 ℃, be preheated to 75-400 ℃, be pressurized to 2～3 normal atmosphere after, being transported in the flame hydrolysis stove burner noz(zle) gas hybrid chamber, is 2.5～120kg/h.m with volatile salt raw material with temperature 80-400 ℃, rate of evaporation simultaneously
2Evaporate, and with rare gas element as carrier gas, be transported in the burner noz(zle) gas hybrid chamber and each road gas uniform mixing, hydrogen-containing fuel is H
2, CH
4, NH
3In one or more mixture; Oxygenated fuel is oxygen, airborne one or both mixture, and rare gas element is N
2, airborne one or both mixture, volatile salt raw material comprises one or more in metal or non-metallic halide, metal or the nonmetal carboxylate; Oxygenated fuel be fuel also be oxygenant,
Purity requirement as the fruit product oxide compound reaches more than 99.9%, can increase the rectifying tower of cover scale coupling in the vaporizer front, and the metal liquid salt of technical purity is purified in advance;
2. flame hydrolysis: the flame hydrolysis furnace structure as shown in Figure 3.
Pretreated three road air-flows are sent into the flame hydrolysis stove after supercharging, after mixing in the gas hybrid chamber of hydrolysis stove nozzle, from ejection of burner noz(zle) conduit and ignition, be 1-12m to combustion flame district feed flow simultaneously
3/ h, temperature be 25-300 ℃ around air, around between nozzle duct and nozzle housing, spraying, prevent to scab because of the nano particle that generates when the nozzle duct mouth burns is sintered in conduit mouth, be unfavorable for the continuous production of technology.Hydrogen-containing fuel and oxygenated fuel burn at the nozzle duct mouth, provide hydrolysis reaction required heat, supply with the needed gaseous molecular water of hydrolysis reaction simultaneously, make the reaction of gaseous state salt and water, nozzle mixed airflow total flux 6.O-20m is finished in flame high-temperature zone reaction at 600-1500 ℃
3/ h, flow velocity is 15-45m/s, it is that aggegation becomes the metal oxide primary particle of 4-40nm in the gradually black furnace thorax of 1500-500 ℃/m in thermograde that the gaseous metal salt finished of reaction is formed aerosol flow with the rare gas element of not participating in reaction, and imports flocculator after flame hydrolysis outlet of still place is cooled to 100-200 ℃;
3. flocculation is collected: the flocculator structure as shown in Figure 7.
Metal oxide primary particle aerosol flow enters the one-level flocculator from the outer tube gas feed, imports 2-3 normal atmosphere simultaneously in the one-level flocculator, and flow is 1-15m
3The forced air of/h, make aerosol flow in flocculator, form turbulent flow and make oxide compound primary particle sharp impacts, derive from interior pipe pneumatic outlet after flocculating into flocculus shape oxide powder, subsequently, the aerosol of flake oxide powder of flocculation is sent in the primary cyclone with the induction air flow ratio of 15-30 meter per second, in primary cyclone, realize 70% powder collection rate, what come out from primary cyclone is that the aerosol that contains primary particle is constant down at forced air and flow equally, advance again in the secondary flocculator, make primary particle flocculate into flocculus shape oxide powder, send in the secondary cyclone with the induction air flow ratio of 15-30 meter per second again and separate, can reach the collection rate more than 90% this moment, (oxide powder that tail gas discharged contains from secondary cyclone can not be collected with flocculator, mainly is the restriction that is subjected to aerosol load to collect for the third time less than the speed importing powder device for filtering and collecting of 10 meter per seconds with the tail gas aerosol again.Can only collect with the powder device for filtering and collecting).Realize that collection rate reaches more than 98%;
4. depickling is handled
The flocculus shape oxide powder of collecting for three times is sent into the depickling stove, slough the sour gas (as hydrogen halide) of powder granule surface adsorption, flaky oxide powder obtains wadding a quilt with cotton.The depickling burner hearth feeds can decompose the liquefied ammonia, (NH that contains ammonia attitude material
4)
2CO
3, NH
4HCO
3, fire box temperature remains on 600～700 ℃, contains ammonia flow and is made progress by furnace bottom, and the flocculus shape oxide powder that is loaded with sour gas down lands from furnace roof portion, sloughs the sour gas layer on surface in containing ammonia flow, obtains the finished product nano oxide powder;
Contain 1/3 the hydrogen halide of having an appointment from solid and gas tripping device tail gas discharged, the purifying treatment that must carry out hydrogen halide reclaims, and produces haloid acid.
5. flame hydrolysis furnace structure
Fig. 3 is the composition structure iron of flame hydrolysis stove, its composition comprises heat-eliminating medium loop head 17-1, furnace outlet 17-2, feet 17-3, burner hearth 17-4, furnace shell internal cooling torus 17-5, the loop exit 17-6 of heat-eliminating medium, metallic high temperature heat transfer layer 17-7, high-temperature-resistant layer 17-8 in the heat transfer layer, burner noz(zle) 17-9, anti-corrosion layer 17-10, furnace shell 17-11, burner noz(zle) is installed in the flame hydrolysis furnace roof, and furnace outlet is at burner hearth bottom, the central lines of both medullary rays and hydrolysis stove, H1 and H2 are respectively heat-eliminating medium loop head and outlet from the distance of furnace bottom and furnace roof, and it is respectively 1/15 and 1/20 high (the stove height does not comprise the furnace bottom conical part) of burner hearth.High-temperature-resistant layer can be used graphite, stainless steel, and anti-corrosion layer can be used aluminum oxide, carborundum, graphite.
Fig. 4,5, the 6th, the burner noz(zle) structure iron, it comprises portfire 17-12, flame temperature measurer 17-13, around air export mouth 17-14, nozzle duct 17-15 is around air introducing port 17-16, star blade 17-17, gas hybrid chamber 17-18, hydrogen fuel introducing port 17-19, oxygenated fuel introducing port 17-20, gasifiable metal-salt material-guiding inlet 17-21, nozzle housing 17-22,17-23 uses as standby introducing port, when general gas flow at 10m
3When/h is above, need import oxygenated fuel from 17-23, import air from 17-20 and promote the conveying of mixed gas in nozzle duct.The air-flow introducing port is installed around nozzle centerline, and the star blade is installed in the nozzle duct of bottom of gas hybrid chamber, and its medullary ray overlaps installation with nozzle centerline.Be enclosed in the periphery of star blade pipe around air chamber, portfire, flame temperature measurer, be arranged on nozzle exit around the air export mouth.
6, Fig. 7, the 8th, the flocculator structure iron, comprise gas feed 12-1, pneumatic outlet 12-2, outer tube 2-3, interior pipe 12-4, gas feed is arranged on the outer tube, the pneumatic outlet setting on inner pipe, outward, interior pipe is by the spiral way coiled by a long pipe for 20-60m, its internal diameter is 15-40mm, distance between outer tube and the interior pipe is 20-30mm, metal oxide primary particle aerosol flow enters the flocculator from the outer tube gas feed, flows back into pneumatic outlet from interior pipe to opposite direction again, and flocculator is made with Glass tubing.
Advantage of comparing with known technology and positively effect:
Among the present invention, air both came transferring metal salt unstripped gas as inert carrier gas, again as oxygen containing oxidant, adopted industrial liquefied ammonia gasification that hydrogen-containing fuel is provided simultaneously, had replaced pure N substantially
2With pure H
2, significantly reduced the production cost of powder product; Burner noz(zle) is provided with mixing section and star blade construction, makes each road air-flow energy uniform mixing and enters flame zone with layer flow mode, and the outside sprays into secondary air and is looped around around the flame, realizes steady spray combustion, avoids the appearance that scabs of flame-thrower nozzle front end; The flame hydrolysis stove adopts the resistant to elevated temperatures burner hearth inner lining material of the burn into of anti-the hydrogen halide, basically eliminate the hydrolysising by-product air-flow in the furnace high-temperature district, middle sour gas is to the strong corrosion effect of burner hearth, makes that explained hereafter can long continuous production; The two-stage flocculator separates arrangement with three grades of solid and gases, makes the primary particle flocculation fully, the separation efficiency height.Product purity is more than 99.9%, crystal with controllable crystal forms, and particle diameter is 5～40nm, specific surface is 100～400m
2/ g, volume density is 0.03～0.06g/cm
3
Four. description of drawings:
Fig. 1 is a process route chart;
Fig. 2 is a device connection diagram, wherein the 1,5, the 15th, and gas blower, the 2nd, strainer, the 3rd, water-and-oil separator, the 4th, moisture eliminator, the 6th, ammonia decomposer, the 7th, the product hopper, the 8th, depickling stove, the 9th, powder device for filtering and collecting, the 10th, secondary cyclone, the 11st, device for absorbing tail gas, the 12nd, secondary flocculator, the 13rd, one-level flocculator, the 14th, primary cyclone, the 16th, process furnace, the 17th, flame hydrolysis stove, the 18th, vaporizer, the 19th, condenser, the 20th, drimeter, the 21st, rectifying tower, A-fuel inlet, the import of B-ammonia;
Fig. 3 is a flame hydrolysis furnace accretion composition, 17-1 is the loop head of heat-eliminating medium, and 17-2 is a furnace outlet, and 17-3 is a feet, 17-4 is a burner hearth, 17-5 is a furnace shell internal cooling torus, and 17-6 is the loop exit of heat-eliminating medium, and 17-7 is the metallic high temperature heat transfer layer, 17-8 is a high-temperature-resistant layer in the heat transfer layer, 17-9 is a burner noz(zle), and 17-10 is an anti-corrosion layer, and 17-11 is a furnace shell;
Fig. 4 is the burner noz(zle) structure iron, and 17-12 is a portfire, and 17-13 is the flame temperature measurer, 17-14 is around the air export mouth, 17-15 is a nozzle duct, and 17-16 is around the air introducing port, and 17-17 is the star blade, 17-18 is the gas hybrid chamber, 17-19 is the hydrogen-containing fuel introducing port, and 17-20 is the oxygenated fuel introducing port, and 17-21 is gasifiable metal-salt material-guiding inlet, 17-22 is a nozzle housing, standby introducing port 17-23;
Fig. 5 burner noz(zle) A view;
Fig. 6 burner noz(zle) B view;
Fig. 7 is the flocculator structural front view, and 12-1 is gas feed, and 12-2 pneumatic outlet, 12-3 are outer tubes, and 12-4 is interior pipe; Fig. 8 is the flocculator side-view, and B is the distance between the inner and outer pipe.
Five. embodiment:
Embodiment 1:
1. the pretreatment technology of raw material, fuel, rare gas element: with technical pure liquid titanium tetrachloride (TiCl
4) under 80 ℃, with 30kg/hm
2Rate of evaporation evaporation, be pressurized to 2 normal atmosphere; Hydrogen, air, N
2Through purifying, being dried to dew point and being lower than-12 ℃, be pressurized to 2 normal atmosphere, be preheated to 180 ℃; Hydrogen, oxygen and be loaded with TiCl
4N
2Respectively with 1.5m3/h, 3.2m
3/ h and 0.6m
3The tolerance of/h is sent in the orifice gas hybrid chamber together.
2. three strands of gas mixtures of blended spray from nozzle duct in hybrid chamber, and total flux is 6.0Nm
3/ h, the speed that sprays from nozzle duct is 15m/s, in this ignition, carries 2.0m to flame zone simultaneously
3/ h, temperature be 200 ℃ around air, reaction zone temperature reaches 1200 ℃, burns at reaction zone, hydrolysis reaction, the nanometer oxide particle that reaction generates is with the rare gas element N that does not participate in reaction
2And the gas composition aerosol that generates of reaction, the temperature of flowing through tonsure is the gradually black furnace thorax of 500-1200 ℃/m,, and grow up into the primary particle of 25-35nm, derive the flame hydrolysis stove with 130 ℃ temperature, enter flocculator.
3. import 2 normal atmosphere in one-level flocculator gas, flow is 10m
3The forced air of/h flocculates, after flocculation is finished, tail gas is input in the primary cyclone with 15-20 meter per second speed and separates, separating the aerosol still contain primary particle from primary cyclone enters in the secondary flocculator with the forced air of pressure identical with the one-level flocculator and flow and continues flocculation, after tail gas is gone into the secondary cyclone separation with 15-20 meter per second speed Lose again, aerosol tail gas to import the powder device for filtering and collecting less than 10 meter per second speed, can be realized the collection rate more than 98% again.20 meters of flocculator pipe ranges, 40 millimeters of bores, 20 millimeters of the distances between the inner and outer pipes.
4, the flocculus shape oxide powder of collecting for three times is sent into the depickling stove, feeding liquefied ammonia, fire box temperature remain on 600～700 ℃, containing ammonia flow is made progress by furnace bottom, the flocculus shape oxide powder that is loaded with sour gas down lands from furnace roof portion, in containing ammonia flow, slough the sour gas layer on surface, obtain the finished product nano-titanium oxide powder.
5. flame hydrolysis stove throughput is 2.0kg/h.
Embodiment 2:
1. the pre-treatment of raw material, fuel, rare gas element: with the liquid metatitanic acid four tincture fat (Ti (OC of technical pure
4H
9)
4Under 190 ℃, with 85kg/hm
2Rate of evaporation evaporation, be pressurized to 2 normal atmosphere; Hydrogen-containing fuel CH
4, oxygenated fuel is 1: 4 oxygen of ratio and AIR MIXTURES, N
2Through purifying, being dried to dew point and being lower than-12 ℃, be pressurized to 2.5 normal atmosphere, be preheated to 220 ℃; Hydrogen, oxygen and be loaded with SiCl
4N
2Respectively with 3.0m
3/ h, 4m
3/ h and 3.5m
3The flow of/h is sent in the orifice gas hybrid chamber.
2. three strands of gas mixtures of blended spray from nozzle duct in hybrid chamber, and total flux is 12.0m
3/ h, the speed that sprays from nozzle duct is 30m/s, in this ignition, carries 8.0m to flame zone simultaneously
3/ h, temperature be 200 ℃ around air, reaction zone temperature reaches 900 ℃, burns at reaction zone, hydrolysis reaction, the nanometer oxide particle that reaction generates is with the rare gas element N that does not participate in reaction
2And the gas composition aerosol of reaction generation, the temperature of flowing through tonsure is the gradually black furnace thorax of 500-900 ℃/m, and grows up into the primary particle of 5-15nm, derives the flame hydrolysis stove with 100 ℃ temperature, enters flocculator.
3. import 2 normal atmosphere in one-level flocculator gas, flow is 10m
3The forced air of/h flocculates, after flocculation is finished, tail gas is input in the primary cyclone with 20-30 meter per second speed and separates, separating the aerosol still contain primary particle from primary cyclone enters in the secondary flocculator with the forced air of pressure identical with the one-level flocculator and flow and continues flocculation, tail gas separates through secondary cyclone with 20-30 meter per second speed, aerosol tail gas can be realized the collection rate more than 98% to import the powder device for filtering and collecting less than 10 meter per second speed.40 meters of flocculator pipe ranges, 25 millimeters of bores, 35 millimeters of the distances between the inner and outer pipes.
4, the flocculus shape oxide powder of collecting for three times is sent into the depickling stove, feed liquefied ammonia, fire box temperature remains on 600～700 ℃, sloughs the sour gas layer on surface in containing ammonia flow, obtains the finished product nano-titanium oxide powder.
5. flame hydrolysis stove throughput is 5.0kg/h.
Embodiment 3:
1. the pre-treatment of raw material, fuel, rare gas element: with the liquid arsenic trichloride (AsCl of technical pure
3Under 270 ℃, with 110kg/hm
2Rate of evaporation evaporation, be pressurized to 2.5 normal atmosphere; The hydrogen-containing fuel ratio is 1: 1 hydrogen and CH
4Mixture, oxygen, as the air of rare gas element through purifying, being dried to dew point and being lower than-12 ℃, be pressurized to 3 normal atmosphere, be preheated to 180 ℃; Hydrogen-containing fuel, oxygen and the air that is loaded with arsenic trichloride are respectively with 4.8m
3/ h, 10m
3/ h and 2.0m
3The flow of/h is sent in the orifice gas hybrid chamber.
2. three strands of gas mixtures of blended spray from nozzle duct in hybrid chamber, and total flux is 11.5m
3/ h, the speed that sprays from nozzle duct is 29m/s, in this ignition, carries 8.0Nm to flame zone simultaneously
3/ h, temperature be 200 ℃ around air, reaction zone temperature reaches 1200 ℃, burn at reaction zone, hydrolysis reaction, the gas composition aerosol that the nanometer oxide particle that reaction generates generates with the rare gas element of not participating in reaction and reaction, the temperature of flowing through tonsure is the gradually black furnace thorax of 700-1200 ℃/m, and grows up into the primary particle of 10-20nm, derive the flame hydrolysis stove with 160 ℃ temperature, enter flocculator.
3. import 3 normal atmosphere in one-level flocculator gas, flow is 10m
3The forced air of/h flocculates, after flocculation is finished, tail gas is input in the primary cyclone with 20-30 meter per second speed and separates, separating the aerosol still contain primary particle from primary cyclone enters in the secondary flocculator with the forced air of pressure identical with the one-level flocculator and flow and after continuing flocculation, tail gas separates through secondary cyclone with 20-30 meter per second speed again, aerosol tail gas to import the powder device for filtering and collecting less than 10 meter per second speed, can be realized the collection rate more than 98% again.50 meters of flocculator pipe ranges, 35 millimeters of bores, 35 millimeters of the distances between the inner and outer pipes.
4, the flocculus shape oxide powder of collecting for three times is sent into the depickling stove, feed (NH
4)
2CO
3, fire box temperature remains on 600～700 ℃, sloughs the sour gas layer on surface in containing ammonia flow, obtains the nano oxidized arsenic powder body of the finished product.
5. flame hydrolysis stove throughput is 5.0kg/h.
Embodiment 4:
1. the pre-treatment of raw material, fuel, rare gas element: with technical pure liquid titanium tetrachloride (TiCl
4) and silicon tetrachloride (SiCl
4Ratio is that 3: 1 mixture is under 350 ℃, with 116kg/hm
2Rate of evaporation evaporation, be pressurized to 3 normal atmosphere; Liquefied ammonia, oxygen, ratio be 2: 1 as the gas mixture of the air of rare gas element and nitrogen through purifying, being dried to dew point and being lower than-12 ℃, be pressurized to 3 normal atmosphere, be preheated to 400 ℃; Liquefied ammonia, oxygen and the inert mixed gas that is loaded with gaseous feed be not with 5.0m
3/ h, 13.0m
3/ h and 6.0m
3The flow of/h is sent in the orifice gas hybrid chamber.
2. three strands of gas mixtures of blended spray from nozzle duct in hybrid chamber, and total flux is 20m
3/ h, the speed that sprays from nozzle duct is 45m/s, in this ignition, carries 12.0m to flame zone simultaneously
3/ h, temperature be 300 ℃ around air, reaction zone temperature reaches 1500 ℃, burns at reaction zone, hydrolysis reaction, the nanometer oxide particle that reaction generates is with the rare gas element N that does not participate in reaction
2And the gas composition aerosol of reaction generation, the temperature of flowing through tonsure is the gradually black furnace thorax of 1500-600 ℃/m, and grows up into the primary particle of 5-35nm, derives the flame hydrolysis stove with 200 ℃ temperature, enters flocculator.
3. import 3 normal atmosphere in one-level flocculator gas, flow is 15m
3The forced air of/h flocculates, after flocculation is finished, tail gas is input in the primary cyclone with 20-30 meter per second speed and separates, separating the aerosol still contain primary particle from primary cyclone enters in the secondary flocculator with the forced air of pressure identical with the one-level flocculator and flow and continues flocculation, tail gas separates through secondary cyclone with 20-30 meter per second speed, and aerosol tail gas is again to import the powder device for filtering and collecting less than 10 meter per second speed.60 meters of flocculator pipe ranges, 40 millimeters of bores, 30 millimeters of the distances between the inner and outer pipes.
4, the flocculus shape oxide powder of collecting for three times is sent into the depickling stove, feed NH
4HCO
3, fire box temperature remains on 600～700 ℃, sloughs the sour gas layer on surface in containing ammonia flow, obtains the finished product nano-titanium oxide silicon oxide mixed powder.
5. flame hydrolysis stove throughput is 10.0kg/h.
Claims (7)
1, a kind of method for preparing fumed nano oxide, with hydrogen-containing fuel, oxygenated fuel, rare gas element, air carries out udst separation, dry, preheating, after the supercharging, be transported in the flame hydrolysis stove burner noz(zle) gas hybrid chamber, simultaneously volatile salt raw material is evaporated, and with rare gas element as carrier gas, be transported in the flame hydrolysis stove burner noz(zle) gas hybrid chamber and each road gas uniform mixing, and under promoting, pressurized air stream in the stove hall, burns, hydrolysis, the mixture that comes out from the burner hearth afterbody imports the one-level flocculator, separate in primary cyclone the flocculation back, tail gas imports the secondary flocculator, flocculation once more, in secondary cyclone, separate once more then, from the secondary cyclone tail gas discharged after the powder device for filtering and collecting is collected for the third time, import device for absorbing tail gas and absorb the back emptying, from primary cyclone, secondary cyclone, the product oxide compound that the powder device for filtering and collecting obtains is in the depickling stove after the depickling, collect through the product hopper, obtain nano oxide powder, it is characterized in that:
1), hydrogen-containing fuel is H
2, CH
4, NH
3In one or more mixture, oxygenated fuel is oxygen, airborne one or both mixture, rare gas element is N
2, airborne one or both mixture, volatile salt raw material comprises one or more in metal or non-metallic halide, metal or the nonmetal carboxylate;
2) be 1.5～5m with flow
3/ h hydrogen-containing fuel, flow are 0.8～15m
3The oxygenated fuel of/h, flow are 0.4～6m
3The rare gas element of/h, air carry out udst separation remove moisture, oil content under 99.0% unbound state, be dried to dew point and be lower than-12 ℃, be preheated to 75-400 ℃, be pressurized to 2～3 normal atmosphere after, being transported in the flame hydrolysis stove burner noz(zle) gas hybrid chamber, is 2.5～120kg/h.m with volatile salt raw material with temperature 80-400 ℃, rate of evaporation simultaneously
2Evaporate, and with rare gas element as carrier gas, be transported in the burner noz(zle) gas hybrid chamber and each road gas uniform mixing;
3) in the gas hybrid chamber of hydrolysis stove nozzle, mix after, from burner noz(zle) conduit ejection and ignition, be 1-12m to combustion flame district feed flow simultaneously
3/ h, temperature be 25-300 ℃ around air, around between nozzle duct and nozzle housing, spraying, hydrogen-containing fuel and oxygenated fuel burn at the nozzle duct mouth, provide hydrolysis reaction required heat, supply with the needed gaseous molecular water of hydrolysis reaction simultaneously, make the reaction of gaseous state salt and water, nozzle mixed airflow total flux 6.0-20m is finished in flame high-temperature zone reaction at 600-1400 ℃
3/ h, flow velocity is 15-45m/s, it is that aggegation becomes the metal oxide primary particle of 4-40nm in the gradually black furnace thorax of 1500-500 ℃/m in thermograde that the gaseous metal salt finished of reaction is formed aerosol flow with the rare gas element of not participating in reaction, and imports flocculator after flame hydrolysis outlet of still place is cooled to 100-200 ℃;
4), metal oxide primary particle aerosol flow enters the one-level flocculator from the outer tube gas feed, 2-3 normal atmosphere of input in the one-level flocculator simultaneously, flow is 1-15m
3The forced air of/h, make aerosol flow in flocculator, form turbulent flow and make oxide compound primary particle sharp impacts, derive from interior pipe pneumatic outlet after flocculating into flocculus shape oxide powder, subsequently, the aerosol of flake oxide powder of flocculation is sent in the primary cyclone with the induction air flow ratio of 15-30 meter per second, in primary cyclone, realize 70% powder collection rate, what come out from primary cyclone is that the aerosol that contains primary particle is constant down at forced air and flow equally, advance again in the secondary flocculator, make primary particle continue to flocculate into flocculus shape oxide powder, send in the secondary cyclone with the induction air flow ratio of 15-30 meter per second again and separate, again the tail gas aerosol is imported the powder device for filtering and collecting with the speed less than 10 meter per seconds at last and collect for the third time;
5), the flocculus shape oxide powder of collecting for three times is sent into the depickling stove, slough the sour gas of powder granule surface adsorption, the flaky oxide powder that obtains wadding a quilt with cotton, the depickling burner hearth feeds liquefied ammonia, (NH
4)
2CO
3Or NH
4HCO
3, fire box temperature remains on 600～700 ℃, contains ammonia flow and is made progress by furnace bottom, and the flocculus shape oxide powder that is loaded with sour gas down lands from furnace roof portion, sloughs the sour gas layer on surface in containing ammonia flow, obtains the finished product nano oxide powder.
2, the method for preparing fumed nano oxide according to claim 1 is characterized in that: increase the rectifying tower of cover scale coupling in the vaporizer front, the metal liquid salt of technical purity is purified in advance.
3, a kind of device for preparing fumed nano oxide is characterized in that: in accordance with the method for claim 1, the device that hydrolysis reaction is provided is the flame hydrolysis stove, and what flocculation usefulness was provided is flocculator.
4, the device of preparation fumed nano oxide according to claim 3, it is characterized in that: the composition structure of flame hydrolysis stove comprises heat-eliminating medium loop head (17-1), furnace outlet (17-2), feet (17-3), burner hearth (17-4), furnace shell internal cooling torus (17-5), the loop exit of heat-eliminating medium (17-6), metallic high temperature heat transfer layer (17-7), high-temperature-resistant layer (17-8) in the heat transfer layer, burner noz(zle) (17-9), anti-corrosion layer (17-10), furnace shell (17-11), burner noz(zle) is installed in the flame hydrolysis furnace roof, furnace outlet is arranged on burner hearth bottom, the central lines of both medullary rays and hydrolysis stove, H1 and H2 are respectively heat-eliminating medium loop head and outlet from the distance of furnace bottom and furnace roof, its be respectively burner hearth high 1/15 and 1/20, high-temperature-resistant layer is with graphite or stainless steel, anti-corrosion layer aluminum oxide, carborundum or graphite.
5, device according to claim 3 or 4 described preparation fumed nano oxides, it is characterized in that: described burner noz(zle) comprises portfire (17-12), flame temperature measurer (17-13), around air export mouth (17-14), nozzle duct (17-15), around air introducing port (17-16), star blade (17-17), gas hybrid chamber (17-18), hydrogen fuel introducing port (17-19), oxygenated fuel introducing port (17-20), gasifiable metal-salt material-guiding inlet (17-21), nozzle housing (17-22), the air-flow introducing port is installed around nozzle centerline, and the star blade is installed in the nozzle duct of bottom of gas hybrid chamber, and its medullary ray overlaps installation with nozzle centerline, be enclosed in the periphery of star blade pipe, portfire around air chamber, the flame temperature measurer, be arranged on nozzle exit around the air export mouth.
6, the device of preparation fumed nano oxide according to claim 5 is characterized in that: (17-23) use as standby introducing port, when general gas flow at 10m
3When/h is above, need import oxygenated fuel from (17-23), import air from (17-20) and promote the conveying of mixed gas in nozzle duct.
7, the device of preparation fumed nano oxide according to claim 3, it is characterized in that: described flocculator structure comprises gas feed (12-1), pneumatic outlet (12-2), outer tube (2-3), interior pipe (12-4), gas feed is arranged on the outer tube, the pneumatic outlet setting on inner pipe, outward, interior pipe is by the spiral way coiled by a long pipe for 20-60m, its internal diameter is 15-40mm, and the distance between outer tube and the interior pipe is 20-50mm, and flocculator is made with Glass tubing.
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|---|---|---|---|
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| DE3611449A1 (en) * | 1986-04-05 | 1987-10-15 | Degussa | BASIC MATERIAL FOR THE PRODUCTION OF CERAMIC MATERIALS |
| DE4235996A1 (en) * | 1992-10-24 | 1994-04-28 | Degussa | Titanium dioxide mixed oxide produced by flame hydrolysis, process for its preparation and use |
| DE19919635A1 (en) * | 1999-04-30 | 2000-11-23 | Degussa | Silicon-aluminum mixed oxide |
| DE10326049A1 (en) * | 2003-06-10 | 2004-12-30 | Degussa Ag | Flame hydrolytically produced silicon dioxide, process for its production and use |
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