CN106698509A - Composite nano zirconium oxide with uniform particle size distribution, and continuous preparation method and equipment thereof - Google Patents
Composite nano zirconium oxide with uniform particle size distribution, and continuous preparation method and equipment thereof Download PDFInfo
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- CN106698509A CN106698509A CN201510788627.2A CN201510788627A CN106698509A CN 106698509 A CN106698509 A CN 106698509A CN 201510788627 A CN201510788627 A CN 201510788627A CN 106698509 A CN106698509 A CN 106698509A
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- C01—INORGANIC CHEMISTRY
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- C01G25/00—Compounds of zirconium
- C01G25/02—Oxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G25/00—Compounds of zirconium
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- C—CHEMISTRY; METALLURGY
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention discloses composite nano zirconium oxide with uniform particle size distribution, and a continuous preparation method and equipment thereof. The continuous preparation method comprises following steps: a zirconium oxide precursor and a stabilizing agent precursor are uniformly mixed, are delivered into a reactor by a carrier gas, are reacted with water vapor at a high temperature, and are subjected to rapid decomposition at the high temperature so as to obtain a composite nano zirconium oxide powder. The particle size of the obtained composite nano zirconium oxide ranges from 5 to 15nm, the stacking density is 0.2g/cm<3> or lower. The equipment comprises a feed system, a reaction system, and a product collecting system. The composite nano zirconium oxide prepared via the continuous preparation method is low in particle size and density, and exists in the form of aerosol. Multistage post-processing product collection and tail gas treatment are adopted in the equipment, so that a technical problem the effective collecting of composite nano zirconium oxide particles is difficult to realize is solved, product yield is increased, and air pollution caused by effusion of solid dust is prevented.
Description
Technical field
It is that one kind is received more specifically the present invention relates to a kind of nano level metal oxide powder level preparing technical field
The metal oxide powder of meter level, its continuous preparation method and its equipment.
Background technology
Zirconium oxide has the advantages that heat-resisting, wear-resisting and good chemical stability, chemical sensor, high-performance ceramic,
The fields such as catalysis material are of great interest.Research work in recent years shows that the zirconium oxide of fine grain has good breaking
Toughness and superplasticity are split, is one of study hotspot of current Material Field.Granularity is tiny and uniform, purity is high, reunion is weak
Powder be obtain high-performance zirconia product key.
Zirconium oxide has a three kinds of phases, i.e. monoclinic phase, Tetragonal and Emission in Cubic, each of which have different crystalline phase density and
Thermodynamically stable warm area.Under normal circumstances, zirconium oxide room temperature to 1170 DEG C be monoclinic phase, 1170-2370 DEG C for four directions
Phase, 2370-2680 DEG C is Emission in Cubic.The density ratio Tetragonal and Emission in Cubic of monoclinic phase are small.Pure zirconia powder metallurgy is (logical
Often>1200 DEG C) sintering after during room temperature is cooled to, due to high-temperature-phase (generally Tetragonal) can occur to low
The phase in version of warm phase (monoclinic phase), volume changes, and makes device cracking processed, crushes, and cannot get high intensity device.For
Overcome the limitation, add stabilizer, such as yittrium oxide, calcium oxide, magnesia in zirconia ceramics powder is prepared,
Composite oxide power is formed, by Zirconia-stabilized in Tetragonal, so that it is broken to be ftractureed in cooling procedure after roasting.
It is main at present that nanoscale zirconium powder is produced using liquid phase method.For example commercialized coprecipitation by containing
Add alkali co-precipitation in zirconates and dopant mixed solution, obtain hydroxide precipitation, then through filtering, washing, dry roasting
Burning obtains solid solution doped zirconia powder.The method is simple and easy to apply, and the easily controllable multicomponent nanocomposite of composition can be obtained
Powder, but the powder reunion degree of the product is big, and follow-up sintering step needs to carry out at a higher temperature, can not only
Consumption is high and crystal grain is grown up significantly, makes there is crackle or cavity in product, influences the mechanical property of ceramics.
In order to control the reunion of powder, liquid phase method is usually sheltered in powder process is prepared using organic solvent washing, addition
The means such as agent, supercritical drying, azeotropic distillation, addition organic surface active agent.Patent document CN1915836A is disclosed
A kind of method that the use precipitation method prepare nano zircite, the concentration of zirconium ion is controlled by screening agent, so as to control oxygen
Change the nucleation process of zirconium, obtain epigranular, purity nano-particle high.Patent document CN102442699A is provided
A kind of method that nano zircite is prepared by catalytic organism agent, the method in the aqueous solution of zirconium source by adding Ji Wusi
Alcohol, trimethylolpropane, 2 methyl valeric acid or 2 ethyl hexanoic acid are catalyst, carry out the oxygen that hydro-thermal reaction prepares Tetragonal
Change zirconium.However, these methods not only increased the complexity and cost of process, and the organic matter for introducing often to ring
Border and personnel health produce harm.By contrast, vapor phase method prepare oxide powder reunite due to having the advantages that to be difficult and
It is valued by people.
Current vapor phase method production oxide powder, is successfully obtained high-quality SiO2、TiO2、Al2O3Deng nanometer powder,
Products obtained therefrom purity is high, good dispersion, operation are continuous.But because vapor phase method prepares the composite oxides of multicomponent mixture in work
Control to require height in skill, the controllability of component is also relatively poor, limits the commercial Application of the technology.Although 1977
Year, Suyama (Ceramurgia Intern., 3 (4):141) just describe to be aoxidized by vapor-phase halides and prepare ZrO2Powder
End, but the method preparation temperature is very high, and it is obvious to there are problems that crystal grain is grown up.Japan Patent JP61-201604A leads to
The vapour-phase pyrolysis or hydrolysis for crossing organic zirconium prepare zirconium oxide, but the product that the technology is obtained is the loose structure of unformed shape,
And containing carbon residue.Patent document CN1259488A provides a kind of preparation side of the weakly agglomerated nano zircite of surface doping
Method, the technology passes through ZrCl4Vapor phase hydrolysis are obtained nano zircite, then again by impregnating introducing stabilizer ions.Should
Preparation flow is more long, and the stabilizer basic load introduced in dipping process is in zirconium surface, is not the solid solution of stabilization
Body.
The content of the invention
The purpose of the present invention is to solve the shortcomings of the prior art, there is provided a kind of even particle size distribution for being not easy to reunite is answered
Close nano zircite particle；
It is a further object of the present invention to provide a kind of preparation technology, the preparation technology can be used to prepare above-mentioned even particle size distribution
Nano zircite, the technique can continuously be run, high income；Further, the technique can also realize production process
Environmental protection；
It is yet another object of the invention to provide a kind of equipment, above-mentioned technique is used especially for.
The purpose of the present invention is implemented by the following technical programs：
A kind of composite Nano zirconium oxide of even particle size distribution, in the composite Nano zirconium oxide zirconia content be 90~
97wt%, stabiliser content is 3~10wt%, and particle diameter is 5nm-15nm, and bulk density is no more than 0.2g/cm3；It is preferred that
Ground, the zirconium oxide is Tetragonal, and stabilizer metals oxide enters zirconium oxide crystalline phase, i.e. η=0 in the form of solid solution,
η is the percentage of the crystal content of stabilizer metals oxide.
Preferably, the average grain diameter of the composite Nano zirconium oxide is 5nm, and bulk density is no more than 0.2g/cm3。
A kind of continuous preparation method of the composite Nano zirconium oxide of even particle size distribution,
Enter reactor after the precursor gasification of the precursor and stabilizer of uniform mixed zirconium oxide, at high temperature with water
Steam generation is reacted, and fast decoupled generates nano zirconium oxide powder to the hydroxide for being generated at high temperature；
Preferably, the mol ratio of the precursor of the precursor of the zirconium oxide and stabilizer is 1:0.02~0.10；
Preferably, the mol ratio of zirconium oxide precursor and vapor is 1：2.1~3.0；
Preferably, it is entrained into by carrier gas after the precursor gasification of the precursor and stabilizer of the uniform mixed zirconium oxide
Enter reactor.
Preferably, the water vapour is produced by hydrogeneous imflammable gas combustion process；
Preferably, the hydrogeneous imflammable gas refers to and can generate after burning the imflammable gas of water, including hydrogen, natural
Gas, oil refinery dry gas, liquefied gas, the alkane of C1-C6, the alkene of C1-C6；Preferably hydrogen or methane；
Preferably, refer to can be with steam reaction and chemical combination by that can generate zirconium oxide after high-temperature roasting for the precursor of zirconium oxide
Thing, including zirconium chloride, zirconium-n-propylate, zirconium iso-propoxide；
Preferably, stabilizer is metal oxide, preferably yittrium oxide, titanium oxide or magnesia one or more
Combination, more preferably yittrium oxide and/or titanium oxide；
Preferably, the precursor of the titanium oxide be can be with steam reaction and by titanium oxide can be generated after high-temperature roasting
One or more combination in compound, including titanium tetrachloride, butyl titanate or isopropyl titanate, more preferably
Titanium tetrachloride；
Preferably, the precursor of the yittrium oxide be can be with steam reaction and by yittrium oxide can be generated after high-temperature roasting
Compound, preferably yttrium isopropoxide, normal propyl alcohol yttrium.
Preferably, described carrier gas is Ar, N2, He or CO2In one or more of mixed gas；Preferably
Ar and/or N2。
Preferably, the reaction temperature in the reactor is controlled more than 600 DEG C, preferably 650~800 DEG C.
Preferably, the continuous preparation method of the nano zircite of above-mentioned even particle size distribution, specifically includes following steps：
1) to hydrogeneous imflammable gas and air and/or oxygen is passed through in reactor, mix entering in reactor
Burning generation water vapour；Or, enter reactor by the way of carrier gas carries water vapour；
2) enter using the well mixed zirconium oxide precursor of carrier gas carrying and as the precursor of the metal oxide of stabilizer
Enter reactor, and reacted generation hydroxide with aforementioned water vapor, fast decoupled generation is steady at high temperature for hydroxide
Nano zirconium oxide powder after fixed；Preferably, the carrier gas is heated to more than 650 DEG C；
3) air-flow for carrying nano zircite carries out product collection by product collection system；
Preferably, after gas is through product collection system, is post-processed and discharged with after meet the requirement of environmental protection.
Preferably, the step 1) in, when fuel gas is hydrogen, the oxygen in fuel gas and oxygen or air
Volume ratio be 2：1~1.2；When fuel gas is methane, the volume ratio of the oxygen in fuel gas and oxygen or air
It is 1：2~2.5.
Preferably, when the step 1) in, when reactor is entered by the way of carrying water vapour using carrier gas, into anti-
Mixed gas are heated to more than 650 DEG C before answering device；
Preferably, steam partial pressure is 1~100KPa, more preferably 10~50kPa；
Preferably, described carrier gas is Ar, N2, He or CO2In one or two and the above mixed gas, it is excellent
Elect Ar and/or N as2；
Preferably, the step 2) in, zirconium oxide precursor is 50 with the proportionate relationship of the vapour pressure of stabilizer precursor：
1~5, more preferably 30：1~1.5.
Further, product separation system is multistep treatment in the step (3), at least including cyclone separator and gas
Solid separator two parts, product collection is carried out in the reactor gas containing particulate matter out using cyclone separator first,
Then processed by gas-solid separator again, and collect product particle；
Preferably, the gas-solid separator uses sack cleaner, fiber or ceramic filter；
Preferably, in the step (3), carrying out post-processing approach to gas is：Tail gas after filtering is removed using wet method
Dirt and/or high-pressure electrostatic precipitation are processed, and the gas after treatment after alkali liquor absorption hydrogen chloride by emptying.
A kind of continuous equipment for preparing composite Nano zirconium oxide,
Including：Feed system, reaction system, product collection system, wherein,
The feed system includes two entrances, the respectively predecessor of the precursor of the zirconium oxide of volatile and stabilizer
The entrance of thing and the entrance of water vapour；
The reaction system is used for water vapour and hydrolysis occurs with the precursor of zirconium oxide and the precursor of stabilizer, including
Reactor, it is preferred that the reactor is externally provided with heater, the temperature for controlling reactor.
The equipment of the continuous preparation of the nano zircite of even particle size distribution of the present invention, particularly may be divided into two types, respectively
As depicted in figs. 1 and 2, the equipment of both types includes following three aspects：Feed system, reaction system, product
Collection system.Specifically two types area is illustrated separately below.
Device A：
When using hydrogeneous fuel gas to be burnt to provide water vapour in reactor top with air (and/or oxygen), using three
Bar gas circuit apparatus for feeding.Specifically, the continuous equipment for preparing nano zircite, the feed system includes three gas
Road,
First gas circuit is sequentially communicated by the first air inlet pipe, primary heater and blender and formed, and carrier gas is from the first air inlet pipe
Air inlet enter, the precursor of zirconium oxide and the precursor of stabilizer after uniform mixing in blender, by through first plus
Carrier gas after hot device heating is carried along into reactor head；
Article 2 gas circuit is directly connected by the second air inlet pipe with burner noz(zle)；
Article 3 gas circuit is directly connected by the 3rd air inlet pipe with burner noz(zle)；
Second air inlet pipe and the 3rd air inlet pipe are respectively used to be passed through hydrogeneous imflammable gas and for being passed through air and/or oxygen,
Hydrogeneous imflammable gas enters reactor head after there is oxidizing fire at burner noz(zle)；
Preferably, it is equipped with flowmeter at first air inlet pipe, the second air inlet pipe, the air inlet of the 3rd air inlet pipe.
Preferably, burner noz(zle) band flame detector, can immediately light a fire when flame surprisingly extinguishes.
Equipment B：
When steam is sent into reactor by the way of carrying vapor using carrier gas, the equipment for continuously preparing nano zircite,
Using two-way apparatus for feeding.Specifically, the continuous equipment for preparing nano zircite, the feed system is including two
Gas circuit,
First gas circuit is sequentially communicated by the first air inlet pipe, primary heater and blender and formed, and carrier gas is from the first air inlet pipe
Air inlet enter, the precursor of zirconium oxide and the precursor of stabilizer after uniform mixing in blender, by carrier gas through the
Reactor head is carried along into after the heating of one heater；
Article 2 gas circuit is provided with the second air inlet pipe and the 3rd air inlet pipe, is respectively used to be passed through carrier gas and water, the second air inlet pipe and
3rd air inlet pipe is converged for one is converged gas circuit and leads to reactor head, and secondary heater is provided with gas circuit in converging, and uses
The carrier gas of water vapour is carried in heating；
Preferably, it is equipped with flowmeter at first air inlet pipe, the second air inlet pipe, the air inlet of the 3rd air inlet pipe.
Below no matter which kind of equipment, it is preferred that described product collection system include cyclone separator and gas-solid separator,
The cyclone separator air inlet is connected with the product deposition portion of reactor by collecting pipe, the top of the cyclone separator
Portion gas outlet is connected with gas-solid separator air inlet, reactor bottom reaction after product under the carrying of carrier gas, from collecting pipe
Into cyclone separator, from cyclone separator bottom collection to portioned product, the gas taken out of by cyclone separator top is again
By further collecting product particle from gas-solid separator bottom after gas-solid separator；
Preferably, induced draught system is provided with after gas-solid separator, discharge tail gas is entered purification recovery device.
Beneficial effect of the present invention：
The inventive method, before the zirconium oxide and stabilizer metals oxide of well mixed volatile are carried using carrier gas
Body thing and water vapour react generation hydroxide, hydroxide nano oxygen at high temperature after fast decoupled generation stabilization
Change zirconium powder.Water vapour easily generates zirconium hydroxide, hydrolysis tool with volatile zirconates and stabilizer metals reactant salt
There is very big reaction equilibrium constant and reaction rate, in thermodynamics of reactions and kinetically to the preparation right and wrong of nano zircite
Chang Youli's.The temperature of reactor is kept more than 600 DEG C, preferably 650~800 DEG C, reaction at such a temperature is generated
Hydroxide can fast dewatering, the zirconium oxide aerosol after formation stabilizer doping.The zirconium oxide prepared using the method is received
Rice corpuscles is seldom reunited, average grain diameter can as little as 5nm, bulk density be no more than 0.2g/cm3。
It is small that the zirconium oxide prepared using the inventive method not only realizes fine size, density, can deposit in the form of an aerosol
.Meanwhile, present device is collected and vent gas treatment using the product of multistage post processing, is overcome small by force in preparation nanometer
There is the technology barrier for being difficult to effective collection in zirconia particles, product yield is improve, while also avoiding solid dust from escaping
Cause air pollution.
The zirconium oxide nano-particle prepared using the present invention has the advantages that particle diameter is small, uniformity is good, reunion is few, with wide
General application prospect.Because it has nanometer size effect, sintering temperature is low, without sky when craft articles or sintex
Gap, is difficult absorption pollutant dirty and not easy to break；The nano zircite also has good bionical performance, can be used as
It is the material of zirconia ceramics tooth.
Brief description of the drawings
Fig. 1 is the structural representation of present device 1 (embodiment 1)；
Fig. 2 is the structural representation of present device 2 (embodiment 2)；
Wherein, the air inlet pipe of 1- first, the air inlet pipe of 2- second, the air inlet pipe of 3- the 3rd, 4- burner noz(zle)s, 5- reactors, 51-
Product deposition portion, 52- reactor heaters, 6- collecting pipes, 7- cyclone separators, 8- gas-solid separators, 9- air inducing system
System, 10- flowmeters, 11- blenders, 12- primary heaters, 13- secondary heaters.
Specific embodiment
The preferred embodiments of the present invention are illustrated below in conjunction with accompanying drawing, it will be appreciated that described herein to be preferable to carry out
Example is merely to illustrate and explain the present invention, and is not intended to limit the present invention.
Embodiment 1：
A kind of equipment of the continuous preparation of composite Nano zirconium oxide, it includes that feed system, reaction system and product collect system
System, wherein, the feed system includes two entrances, the respectively precursor of the zirconium oxide of volatile and stabilizer
The entrance of precursor mixture and the entrance of water vapour；The reaction system is used for the predecessor of water vapour and volatile oxidation zirconium
There is hydrolysis, including reactor in the precursor of thing and stabilizer, it is preferred that the reactor is externally provided with heater,
Temperature for controlling reactor, the product collection system is used to complete to collect the nano zircite product for generating.Its
In, feed system can at least have two kinds of embodiments, and the first scheme is：
As shown in Figure 1：Feed system includes three road gas feeds, and first gas circuit is heated by the first air inlet pipe 1, first
Device 12 and blender 11 are sequentially communicated and form, and carrier gas enters from the air inlet of the first air inlet pipe 1, it is preferred to use flowmeter
The precursor of 10 precise controls its flows, zirconium oxide and stabilizer after uniform mixing in blender 11, into pipeline,
Carrier gas after by being heated through primary heater 12 is carried along into reactor 5.Imflammable gas and air containing hydrogen and/or
Oxygen each leads into the second air inlet pipe 2 and the 3rd air inlet pipe 3, preferably respectively through after flowmeter 10 through burner noz(zle) 4
Into reactor.Preferably, burner noz(zle) band flame detector, can immediately light a fire when flame surprisingly extinguishes.It is preferred that
, blender is provided with meter, the precursor for measuring zirconium oxide and stabilizer.
Reaction system：Including reactor 5, reactor 5 is made up of exotic material, and imflammable gas is at burner noz(zle)
Generation oxidizing fire, and ensure that the fuel gas in reactor is constantly in fired state, reaction system is maintained at 600 DEG C
More than, preferably 650~800 DEG C；Easily to there is hydrolysis in the water vapour of generation anti-with the precursor of volatile oxidation zirconium and stabilizer
Should, the doping type zirconium hydroxide of generation can quickly decompose generation zirconium oxide at high temperature, so as in reactor bottom,
I.e. reactant deposition portion 51 obtains nano zircite product.
Preferably, in order to preferably collect nano zircite product, the bottom of reactor 5 is in the tapered taper in bottom.
Product collection system：Including cyclone separator and gas-solid separator two parts.Due to what is obtained from reaction system
Product average grain diameter is less than 15nm, does not reunite substantially, exists with aerosol shape, and apparent bulk density is no more than
0.2g/cm3, in order to improve product yield, while also avoiding solid dust from escaping causes air pollution, multistage can be set
Collect.Product enters cyclone separator 7 from collecting pipe 6 after the reaction that carrier gas is carried, from the bottom collection of cyclone separator 7
To portioned product, the product taken out of by the gas on the top of cyclone separator 7 from bottom after gas-solid separator 8 again by entering one
Step collects product particle.
Preferably, in order to preferably collect nano zircite product, cyclone separator 7 and/or the bottom of gas-solid separator 8 are in
To the taper that bottom is tapered.
To improve the transfer efficiency of gas, it is preferable that increase induced draught system 9 after gas-solid separator 8.Preferably, arrange
Go out tail gas also need to by alkali cleaning removal hydrogen chloride after could discharge, specifically, tail gas can by use wet dedusting with
/ or high-pressure electrostatic precipitation processed, the gas after treatment by after alkali liquor absorption hydrogen chloride empty.
Nano zircite is prepared by the scheme of the embodiment, energy consumption is low, production is easy, and cost is relatively low, and obtained product
Product even particle size distribution, average grain diameter is not reunited in 5-15nm, and purity is high, and impurity content is less than 0.2%, is received
Rate is higher, and good dispersion, it is possible to achieve continuous to prepare.
Embodiment 2：
A kind of equipment of the continuous preparation of composite Nano zirconium oxide, the feed system of the present embodiment is unlisted in embodiment 1
Second scheme, specially：As shown in Figure 2：, by two-way gas feed composition, first article of gas circuit is by for feed system
One air inlet pipe 1, primary heater 12 and blender 11 are sequentially communicated and form, air inlet of the carrier gas from the first air inlet pipe 1
Into using its flow of the precise control of flowmeter 10, the precursor of zirconium oxide and stabilizer is uniformly mixed in blender 11
After conjunction, into pipeline, by being heated through primary heater 12 after carrier gas be carried along into the top of reactor 5, this gas circuit
Structure it is essentially identical with structure in the first scheme；Article 2 gas circuit is provided with the second air inlet pipe and the 3rd air inlet pipe, carries
After gas and water are converged by the second air inlet pipe 2 and the 3rd air inlet pipe 3 respectively, by entering reaction after secondary heater 13
The top of device 5, this method completes reaction by being directly added into vapor, and be only hydrolyzed reaction and hydrogen-oxygen in reactor
Change the decomposition reaction of zirconium, accessory substance is reduced.Preferably, blender is provided with meter, for measuring zirconium oxide and stabilization
The precursor of agent.
Reaction system：Reactor 5 is made up of exotic material, outside band heater 52, is maintained at reaction system
More than 600 DEG C, preferably 600~800 DEG C；Into the water vapour in reaction system easily with volatile oxidation zirconium and stabilizer before
There is hydrolysis in body thing, the doping type zirconium hydroxide of generation can quickly decompose generation zirconium oxide at high temperature, from
And obtain nano zircite product in reactor bottom, i.e. product deposition portion 51.
Product collection system is same as Example 1.
Although the device structure of the embodiment is different from embodiment 1, its obtained nano zirconium oxide powder equally has grain
Degree is evenly distributed, and average grain diameter is not reunited in 5-15nm, and purity is high, and yield is higher, and good dispersion,
Continuous preparation can be equally realized, while the scheme of the present embodiment also has control more accurate, and the product matter for obtaining
Measure more preferable advantage.
Embodiment 3：
Using the nano zircite continuous producing apparatus of Fig. 1, first gas circuit carries zirconium chloride and isopropyl using High Purity Nitrogen
The vapour pressure of the gas of alcohol yttrium, wherein zirconium chloride and yttrium isopropoxide is respectively 30kPa and 1kPa, and flow is 1.5m3/h。
The flow of air is 2.5m in Article 2 gas circuit3/ h, gas circuit 3 uses pentane, and its flow is 1.0m3/h.Article 2 gas
Road and Article 3 gas circuit enter reactor by sleeve pipe, and igniter is provided near mixer outlet, into after reactor
N-hexane burns, and the temperature in the reactor is 720 DEG C, and the doping type zirconium hydroxide of generation at high temperature can be fast
Speed is decomposed, the zirconium oxide after generation stabilization.
Product is white powder, is analyzed using dynamic laser light scattering experimental, zirconium dioxide after doped yttrium oxide it is average
Particle diameter is 4nm.The specific surface area (BET) of the product is 172m2/ g, yield is 93wt%.
Embodiment 4：
Using the nano zircite continuous producing apparatus of Fig. 1, first gas circuit carries zirconium chloride and isopropyl using High Purity Nitrogen
The vapour pressure of the gas of alcohol yttrium, wherein zirconium chloride and yttrium isopropoxide is respectively 30kPa and 1kPa, zirconium chloride and isopropyl
The mol ratio of alcohol yttrium is 1:0.02, flow is 1.5m3/h.The flow of air is 4.8m in Article 2 gas circuit3/ h, Article 3
Gas circuit uses methane, and its flow is 0.5m3/h.Zirconium chloride is 1 with the mol ratio of vapor：2.1, steam partial pressure
It is 10KPa, Article 2 gas circuit and Article 3 gas circuit enter reactor by sleeve pipe, and are provided with a little near mixer outlet
Firearm, into reactor after hydrogen burn, the temperature in the reactor be 650 DEG C.
Product is white powder, is analyzed using dynamic laser light scattering experimental, zirconium dioxide after doped yttrium oxide it is average
Particle diameter is 5nm.The specific surface area (BET) of the product is 198m2/ g, yield is 92wt%.
Embodiment 5：
Using the nano zircite continuous producing apparatus of Fig. 1, first gas circuit of charging using High Purity Nitrogen carry zirconium chloride and
The gas of yttrium isopropoxide mixing, the vapour pressure of wherein zirconium chloride and yttrium isopropoxide mixture is respectively 30kPa and 1.5kPa,
The mol ratio of zirconium chloride and yttrium isopropoxide is 1:0.10, flow is 1.5m3/h.The flow of air is in Article 2 gas circuit
2.50m3/ h, Article 3 gas circuit uses propylene, and its flow is 1.0m3/ h, zirconium chloride is 1 with the mol ratio of vapor：
3.0, steam partial pressure is 1KPa.Article 2 gas circuit and Article 3 gas circuit enter reactor by sleeve pipe, and in blender
Near exit is provided with igniter, into reactor after propylene burn, the temperature in the reactor be 720 DEG C.
Product is white powder, is analyzed using dynamic laser light scattering experimental, zirconium dioxide after doped yttrium oxide it is average
Particle diameter is 5nm.The specific surface area (BET) of the product is 175m2/ g, yield is 93wt%.
Embodiment 6：
Using the nano zircite continuous producing apparatus of Fig. 1, first gas circuit is using high-purity argon gas carrying zirconium chloride and just
The vapour pressure of the gas of propyl alcohol yttrium, wherein zirconium chloride and yttrium isopropoxide is respectively 15kPa and 1kPa, zirconium chloride and just
The mol ratio of propyl alcohol yttrium is 1:0.06, flow is 1.5m3/h.The flow of oxygen is 1.25m in Article 2 gas circuit3/ h, the
Three fuel gas of gas circuit are methane, and its flow is 0.5m3/ h, zirconium chloride is 1 with the mol ratio of vapor:2.5,
Steam partial pressure is 50KPa.Article 2 gas circuit and Article 3 gas circuit enter reactor by sleeve pipe, and in mixer outlet
Nearby be provided with igniter, into reactor after hydrogen burn, the temperature in the reactor be 780 DEG C.
Product is white powder, is analyzed using dynamic laser light scattering experimental, zirconium dioxide after doped yttrium oxide it is average
Particle diameter is 4nm.The specific surface area (BET) of the product is 138m2/ g, yield is 97wt%.
Embodiment 7：
Using the nano zircite continuous producing apparatus of Fig. 1, first gas circuit carries isopropyl using high-purity carbon dioxide gas
The vapour pressure of the gas of alcohol zirconium and yttrium isopropoxide, wherein zirconium iso-propoxide and yttrium isopropoxide is respectively 20kPa and 1kPa, flow
It is 1.5m3The mol ratio of/h, zirconium iso-propoxide and yttrium isopropoxide is 1：0.8.The flow of air is in Article 2 gas circuit
2.50m3/ h, Article 3 gas circuit uses liquefied gas, and its flow is 1.0m3/ h, zirconium iso-propoxide is with the mol ratio of vapor
1:2.8, steam partial pressure is 100KPa.Article 2 gas circuit and Article 3 gas circuit enter reactor by sleeve pipe, and mixed
Clutch near exit is provided with igniter, into reactor after liquefied gas burn, the temperature in the reactor be 720 DEG C.
Product is white powder, is analyzed using dynamic laser light scattering experimental, zirconium dioxide after doped yttrium oxide it is average
Particle diameter is 4nm.The specific surface area (BET) of the product is 163m2/ g, yield is 92wt%.
Embodiment 8：
Using the nano zircite continuous producing apparatus of Fig. 1, first gas circuit carries zirconium chloride and tetrachloro using High Purity Nitrogen
Change the gas of titanium, the vapour pressure of wherein zirconium chloride and titanium tetrachloride is respectively 20kPa and 0.95kPa, and flow is
2.0m3The mol ratio of/h, the precursor of zirconium oxide and the precursor of stabilizer is 1:0.03.The stream of oxygen in Article 2 gas circuit
It is 1.25m to measure3/ h, the fuel gas of Article 3 gas circuit is methane, and its flow is 0.5m3/ h, zirconium oxide precursor and water
The mol ratio of steam is 1：2.9, steam partial pressure is 30KPa.Article 2 gas circuit and Article 3 gas circuit enter by sleeve pipe
Reactor, and igniter is provided near mixer outlet, into reactor after methane burn, in the reactor
Temperature is 750 DEG C.
Product is white powder, is analyzed using dynamic laser light scattering experimental, it is titania-doped after zirconium dioxide it is flat
Equal particle diameter is 5nm.The specific surface area (BET) of the product is 159m2/ g, yield is 96wt%.
Embodiment 9：
Using the nano zircite continuous producing apparatus of Fig. 2, first gas circuit carries zirconium chloride and tetrachloro using High Purity Nitrogen
Change the gas of titanium, the vapour pressure of wherein zirconium chloride and titanium tetrachloride is respectively 20kPa and 0.95kPa, and flow is 2.0m3/ h,
The mol ratio of the precursor of zirconium oxide and the precursor of stabilizer is 1:0.05.Article 2 gas circuit is steamed using the water that argon gas is carried
Vapour, total flow is 2.50m3The mol ratio of/h, zirconium oxide precursor and vapor is 1：2.4, steam partial pressure is 42kPa.
This two-way gas enters reactor after needing to be heated to 600 DEG C, reactor needs further heating to maintain the temperature at
650℃。
Product is white powder, is analyzed using dynamic laser light scattering experimental, it is titania-doped after zirconium dioxide it is flat
Equal particle diameter is 5nm.The specific surface area (BET) of the product is 139m2/ g, yield is 94wt%.
Embodiment 10：
Using the nano zircite continuous producing apparatus of Fig. 2, first gas circuit carries zirconium chloride and tetrachloro using High Purity Nitrogen
Change the gas of titanium, the vapour pressure of wherein zirconium chloride and titanium tetrachloride is respectively 50kPa and 1kPa, and flow is 2.0m3/ h,
The mol ratio of the precursor of zirconium oxide and the precursor of stabilizer is 1:0.07.Article 2 gas circuit is steamed using the water that argon gas is carried
Vapour, total flow is 2.50m3The mol ratio of/h, zirconium oxide precursor and vapor is 1：2.6, steam partial pressure is 3kPa.
This two-way gas enters reactor after needing to be heated to 800 DEG C, reactor needs progressive heating to maintain the temperature at 800 DEG C.
Product is white powder, is analyzed using dynamic laser light scattering experimental, it is titania-doped after zirconium dioxide it is flat
Equal particle diameter is 3nm.The specific surface area (BET) of the product is 175m2/ g, yield is 97wt%.
Embodiment 11：
Using the nano zircite continuous producing apparatus of Fig. 2, first gas circuit carries zirconium chloride and tetrachloro using High Purity Nitrogen
Change the gas of titanium, the vapour pressure of wherein zirconium chloride and titanium tetrachloride is respectively 10kPa and 1kPa, and flow is 2.0m3/ h,
The mol ratio of the precursor of zirconium oxide and the precursor of stabilizer is 1:0.07.Article 2 gas circuit is steamed using the water that argon gas is carried
Vapour, total flow is 2.50m3The mol ratio of/h, zirconium oxide precursor and vapor is 1：2.4, steam partial pressure is 50kPa.
This two-way gas enters reactor after needing to be heated to 700 DEG C, reactor needs progressive heating to maintain the temperature at 700 DEG C.
Product is white powder, is analyzed using dynamic laser light scattering experimental, it is titania-doped after zirconium dioxide it is flat
Equal particle diameter is 5nm.The specific surface area (BET) of the product is 198m2/ g, yield is 93wt%.
Embodiment 12：
Using the nano zircite continuous producing apparatus of Fig. 1, first gas circuit carries zirconium-n-propylate and titanium using high-purity Ar
The gas of sour four butyl esters, the vapour pressure of wherein zirconium-n-propylate and butyl titanate is respectively 30kPa and 1kPa, and flow is
1.5m3The mol ratio of/h, the precursor of zirconium oxide and the precursor of stabilizer is 1:0.05.The stream of air in Article 2 gas circuit
It is 2m to measure3/ h, gas circuit 3 uses natural gas, and its flow is 1.0m3/ h, the precursor of zirconium oxide and the mol ratio of vapor
It is 1:2.4, steam partial pressure is 30KPa.Article 2 gas circuit and Article 3 gas circuit enter reactor by sleeve pipe, and mixed
Clutch near exit is provided with igniter, into reactor after natural gas burn, the temperature in the reactor be 600 DEG C.
Product is white powder, is analyzed using dynamic laser light scattering experimental, zirconium dioxide after doped yttrium oxide it is average
Particle diameter is 10nm.The specific surface area (BET) of the product is 162m2/ g, yield is 90wt%.
Embodiment 13：
Using the nano zircite continuous producing apparatus of Fig. 1, first gas circuit carries zirconium-n-propylate and different using high-purity He
The vapour pressure of the gas of propionic acid titanium, wherein zirconium-n-propylate and butyl titanate is respectively 30kPa and 1kPa, and flow is
1.5m3The mol ratio of/h, the precursor of zirconium oxide and the precursor of stabilizer is 1:0.08.The stream of air in Article 2 gas circuit
It is 2.2m to measure3/ h, gas circuit 3 uses oil refinery dry gas, and its flow is 1.0m3/ h, the precursor of zirconium oxide and rubbing for vapor
You are than being 1:2.8, steam partial pressure is 25KPa.Article 2 gas circuit and Article 3 gas circuit enter reactor by sleeve pipe, and
Igniter is provided near mixer outlet, into reactor after oil refinery dry gas burn, the temperature in the reactor is
800℃。
Product is white powder, is analyzed using dynamic laser light scattering experimental, zirconium dioxide after doped yttrium oxide it is average
Particle diameter is 13nm.The specific surface area (BET) of the product is 169m2/ g, yield is 94wt%.
Embodiment 14：
Using the nano zircite continuous producing apparatus of Fig. 2, first gas circuit is using High Purity Nitrogen and the gaseous mixture of carbon dioxide
Carry the gas of zirconium chloride and titanium tetrachloride, the vapour pressure of wherein zirconium chloride and titanium tetrachloride be respectively 20kPa and
0.95kPa, flow is 2.0m3The mol ratio of/h, the precursor of zirconium oxide and the precursor of stabilizer is 1:0.06.Second
The water vapour that bar gas circuit is carried using carbon dioxide, total flow is 2.50m3/ h, the precursor of zirconium oxide and rubbing for vapor
You are than being 1:2.3, steam partial pressure is 42kPa.This two-way gas enters reactor, reaction after needing to be heated to 600 DEG C
Device needs further heating to maintain the temperature at 680 DEG C.
Product is white powder, is analyzed using dynamic laser light scattering experimental, it is titania-doped after zirconium dioxide it is flat
Equal particle diameter is 15nm.The specific surface area (BET) of the product is 156m2/ g, yield is 97wt%.
Comparative example 1：
Using the nano zircite continuous producing apparatus of Fig. 1, the first air inlet pipe 1 carries zirconium chloride using High Purity Nitrogen, its
The vapour pressure of middle zirconium chloride is 30kPa, and flow is 1.5m3/h.The flow of air is 2.5m in second air inlet pipe 23/ h,
3rd air inlet pipe 3 uses hydrogen, and its flow is 1.0m3/h.Second air inlet pipe 2 and the 3rd air inlet pipe 3 are entered by sleeve pipe
Enter reactor, and igniter be provided near mixer outlet, into reactor after hydrogen burn, in the reactor
Temperature be 720 DEG C.Obtain Zirconium oxide powder.
Take 450 gram of five water yttrium nitrate (analyzing pure, traditional Chinese medicines chemical reagents corporation) to be dissolved in 8 kilograms of deionized waters, be made into
Yttrium nitrate aqueous solution, is then immersed in 3.7 kilograms of above-mentioned zirconium dioxides in the solution.Then heating evaporation while stirring
Solvent.After solvent is evaporated, 110 DEG C of oven drying 10h are put into.Sample B1 is obtained, using dynamic laser light scattering experimental point
Analysis, the average grain diameter of B1 is 20nm, illustrates that oxide particle part is reunited in dipping process.
Comparative example 2：
Using the nano zircite continuous producing apparatus of Fig. 1, the first air inlet pipe 1 carries zirconium chloride gas using High Purity Nitrogen,
Wherein the vapour pressure of zirconium chloride is 30kPa, and flow is 1.5m3/h.The flow of air is 4.8m in second air inlet pipe 23/ h,
3rd air inlet pipe 3 uses methane, and its flow is 0.5m3/h.Second air inlet pipe 2 and the 3rd air inlet pipe 3 are entered by sleeve pipe
Enter reactor, and igniter be provided near mixer outlet, into reactor after hydrogen burn, in the reactor
Temperature be 650 DEG C.Obtain Zirconium oxide powder.
Yttrium nitrate is introduced with reference to the method dipping of comparative example 1, sample B2 is obtained.Analyzed using dynamic laser light scattering experimental,
The average grain diameter of B2 is 18nm, illustrates that oxide particle part is reunited in dipping process.
Embodiment 15：
In order to further discriminate between the difference between different adsorbents, the crystalline phase composition to all samples is analyzed.Crystal phase analysis
Using X-ray diffraction and phase filtering (R.V.Siriwardane, J.A.Poston, G.Evans,
Jr.Ind.Eng.Chem.Res.33 (1994) 2810-2818), the Rietveld models (RIQASrietveld that is corrected
Analysis, operation manual, Material Data, Inc., Berkley, CA (1999)), different samples are analyzed, and use
The method of fitting calculates the crystalline phase composition of sample.Using be equipped with 40kV, 30mA drive fine focusing copper X- long
The Philips XRG3100 generators of radiographic source；Philips3020 digital goniometers and Philips3710MPD control meters
Calculation machine；All of X-ray diffraction measurement is carried out with Kevex PSI Peltier cooling silicon detectors.Using Kevex4601
Ion pump controller, Kevex4608Peltier power supplys, Kevex4621 detector bias, at Kevex4561A pulses
Reason device and Kevex4911-A single channel analyzers operation Kevex detectors.
Diffraction pattern is obtained using 4.1c editions softwares of Philips APD.Use Material Data, Inc.Riqas3.1c editions
Software (Outokumpu HSC Chemistry for Windows：User's manual, Outokumpo Resarch Oy, Pori,
Finland (1999)) carry out all of rietveld calculating.
The crystalline phase composition of the wherein sample of embodiment 1-14 only has zirconium oxide, and η=0, composite metal ion is stabilizer
Metal ion, in the form of amorphous phase enter zirconium oxide crystalline phase, i.e. η=0, η for composite metal ion oxide crystalline substance
The percentage of phase content.Zirconia content is that 95%, yittrium oxide crystal content is 5% in sample B1 crystalline phases composition, i.e.,
η=5；Zirconia content is that 95%, yittrium oxide crystal content is 5%, i.e. η=5 in sample B1 crystalline phases composition.
In sum, the zirconium oxide nano-particle that prepared by the present invention has the advantages that particle diameter is small, uniformity is good, reunion is few,
It is with a wide range of applications.There is nanometer size effect using the Zirconium oxide nano grain, sintering temperature is low, make work
Tight when skill product or sintex, pollutant is not adsorbed dirty and not easy to break；The nano zircite also has fine
Bionical performance, can be used for the material of zirconia ceramics tooth.
The preferred embodiments of the present invention are the foregoing is only, is not intended to limit the invention, although with reference to foregoing implementation
Example has been described in detail to the present invention, and for a person skilled in the art, it still can be to foregoing each implementation
Technical scheme described in example is modified, or carries out equivalent to which part technical characteristic.It is all of the invention
Within spirit and principle, any modification, equivalent substitution and improvements made etc. should be included in protection scope of the present invention
Within.
Claims (10)
1. the composite Nano zirconium oxide of a kind of even particle size distribution, it is characterised in that：Zirconium oxide in the composite Nano zirconium oxide
Content is 90~97wt%, and stabiliser content is 3~10wt%, and particle diameter is 5nm-15nm, and bulk density is no more than 0.2g/cm3；
Preferably, the zirconium oxide is Tetragonal, and stabilizer metals oxide enters zirconium oxide crystalline phase, i.e. η in the form of solid solution
=0, η are the percentage of the crystal content of stabilizer metals oxide.
Preferably, the average grain diameter of the composite Nano zirconium oxide is 5nm, and bulk density is no more than 0.2g/cm3。
2. the continuous preparation method of the composite Nano zirconium oxide of a kind of even particle size distribution, it is characterised in that：It is uniform mixed
The precursor of zirconium oxide and the precursor of stabilizer enter reactor, are reacted with water vapour at high temperature, the hydrogen for being generated
Fast decoupled generates nano zirconium oxide powder to oxide at high temperature；
Preferably, the mol ratio of the precursor of the precursor of the zirconium oxide and stabilizer is 1:0.02~0.10；
Preferably, the mol ratio of zirconium oxide precursor and vapor is 1：2.1~3.0；
Preferably, it is carried along into by carrier gas after the precursor gasification of the precursor and stabilizer of the uniform mixed zirconium oxide
Reactor.
3. the continuous preparation method of the composite Nano zirconium oxide of even particle size distribution according to claim 2, its feature exists
In：The water vapour is burnt by hydrogeneous imflammable gas and produced；Preferably, the hydrogeneous imflammable gas can after referring to burning
Generate water imflammable gas, including hydrogen, natural gas, oil refinery dry gas, liquefied gas, C1-C6 alkane, the alkene of C1-C6
Hydrocarbon；Preferably hydrogen or methane；
And/or, the precursor of zirconium oxide refer to can with steam reaction and compound by zirconium oxide can be generated after high-temperature roasting,
Including zirconium chloride, zirconium-n-propylate or zirconium iso-propoxide；
And/or, stabilizer is metal oxide, preferably the one kind or two in yittrium oxide, titanium oxide, magnesia, calcium oxide
The combination of kind and the above, more preferably yittrium oxide and/or titanium oxide；Preferably, the precursor of the titanium oxide is that can be steamed with water
Vapour reacts and by the compound of generation titanium oxide after high-temperature roasting, including in titanium tetrachloride, butyl titanate or isopropyl titanate
One or two and the above combination, more preferably titanium tetrachloride；Preferably, the precursor of the yittrium oxide is for can be with water
Steam reaction and the compound by generating yittrium oxide after high-temperature roasting, preferably yttrium isopropoxide, normal propyl alcohol yttrium；
And/or, the carrier gas is Ar, N2, He or CO2In one or two and the above mixed gas；Preferably Ar and/
Or N2。
4. the continuous preparation method of the composite Nano zirconium oxide of even particle size distribution according to claim 2, its feature exists
In：Temperature control in the reactor more than 600 DEG C, preferably 650~800 DEG C.
5. the continuous preparation method of the composite Nano zirconium oxide of the even particle size distribution according to claim any one of 2-4,
It is characterized in that：Specifically include following steps：
1) to hydrogeneous imflammable gas and air and/or oxygen is passed through in reactor, mixed combustion is generated in reactor
Water vapour；Or, enter reactor by the way of carrier gas carries water vapour；
2) enter anti-using the well mixed zirconium oxide precursor of carrier gas carrying and as the precursor of the metal oxide of stabilizer
Answer device, and reacted generation hydroxide with aforementioned water vapor, hydroxide at high temperature receive by fast decoupled generation stabilization
Rice Zirconium oxide powder；Preferably, the carrier gas is heated to more than 650 DEG C；
3) air-flow for carrying nano zircite carries out product collection by product collection system；
Preferably, after gas is through product collection system, is post-processed and discharged with after meet the requirement of environmental protection；
Preferably, the step 1) in, when imflammable gas is hydrogen, the oxygen in imflammable gas and oxygen or air
Volume ratio be 2：1~1.2；When fuel gas is methane, the volume ratio of the oxygen in fuel gas and oxygen or air is
1：2~2.5；
Preferably, when the step 1) in using carrier gas carry water vapour by the way of enter reactor when, into reactor before general
Mixed gas are heated to more than 650 DEG C；Preferably, steam partial pressure is 1~100KPa, more preferably 10~50kPa；It is preferred that
, described carrier gas is Ar, N2, He or CO2In one or more of mixed gas, preferably Ar and/or N2；
Preferably, the step 2) in, zirconium oxide precursor is 50 with the proportionate relationship of the vapour pressure of stabilizer precursor：1~
5, more preferably 30：1~1.5.
6. the continuous preparation method of the composite Nano zirconium oxide of even particle size distribution according to claim 5, its feature exists
In：The step 3) in piece-rate system be multistep treatment, including cyclone separator treatment and gas-solid separator process two parts,
The autoreactor gas containing particulate matter out carries out product collection using cyclone separator first, then again by gas solid separation
Device treatment, and collect product particle；Preferably, the gas-solid separator uses sack cleaner, fiber or ceramic filter
Device；
And/or, the step 3) in, carrying out post-processing approach to gas is：Tail gas after filtering using wet dedusting and/or
High-pressure electrostatic precipitation is processed, and the gas after treatment after alkali liquor absorption hydrogen chloride by emptying.
7. a kind of continuous equipment for preparing composite Nano zirconium oxide, it is characterised in that：Including：Feed system, reaction system
System, product collection system, wherein,
The feed system includes two entrances, the respectively precursor of the precursor of the zirconium oxide of volatile and stabilizer
The entrance of entrance and water vapour；
The reaction system is used for water vapour and hydrolysis occurs with the precursor of zirconium oxide and the precursor of stabilizer, including anti-
Answer device, it is preferred that the reactor is externally provided with heater, the temperature for controlling reactor.
8. the continuous equipment for preparing composite Nano zirconium oxide according to claim 7, it is characterised in that：The charging system
System includes three gas circuits,
First gas circuit is sequentially communicated by the first air inlet pipe, primary heater and blender and formed, and carrier gas is from the first air inlet pipe
After air inlet entrance, the precursor of zirconium oxide and the precursor of stabilizer uniformly mix in blender, by through primary heater
Carrier gas after heating is carried along into reactor head；
Article 2 gas circuit is directly connected by the second air inlet pipe with burner noz(zle)；
Article 3 gas circuit is directly connected by the 3rd air inlet pipe with burner noz(zle)；
Second air inlet pipe and the 3rd air inlet pipe are respectively used to be passed through hydrogeneous imflammable gas and for being passed through air and/or oxygen, contain
Hydrogen imflammable gas enters reactor head after there is oxidizing fire at burner noz(zle)；
Preferably, it is equipped with flowmeter at first air inlet pipe, the second air inlet pipe, the air inlet of the 3rd air inlet pipe.
9. the continuous equipment for preparing composite Nano zirconium oxide according to claim 7, it is characterised in that：The charging system
System includes two gas circuits,
First gas circuit is sequentially communicated by the first air inlet pipe, primary heater and blender and formed, and carrier gas is from the first air inlet pipe
After air inlet entrance, the precursor of zirconium oxide and the precursor of stabilizer uniformly mix in blender, by through primary heater
Carrier gas after heating is carried along into reactor head；
Article 2 gas circuit is provided with the second air inlet pipe and the 3rd air inlet pipe, is respectively used to be passed through carrier gas and water, the second air inlet pipe and
Three air inlet pipe are converged for one is converged gas circuit and leads to reactor head, and secondary heater is provided with gas circuit in converging, for plus
Heat carries the carrier gas of water vapour；
Preferably, it is equipped with flowmeter at first air inlet pipe, the second air inlet pipe, the air inlet of the 3rd air inlet pipe.
10. the continuous equipment for preparing composite Nano zirconium oxide according to claim any one of 7-9, it is characterised in that：Institute
The product collection system stated includes the product of cyclone separator and gas-solid separator, the cyclone separator air inlet and reactor
Deposition portion is connected by collecting pipe, and the top gas outlet of the cyclone separator is connected with gas-solid separator air inlet, reaction
Device bottom reaction after product under the carrying of carrier gas, enter cyclone separator from collecting pipe, from cyclone separator bottom collection to
Portioned product, the gas taken out of by cyclone separator top from gas-solid separator bottom after gas-solid separator again by further receiving
Collection product particle；
Preferably, induced draught system is provided with after gas-solid separator, discharge tail gas is entered reclaiming clean retracting device.
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| CN113198390A (en) * | 2021-05-28 | 2021-08-03 | 哈尔滨学院 | High-efficient processingequipment of nanometer titanium dioxide |
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