CN110255612A - A kind of device and method preparing high purity nano material - Google Patents
A kind of device and method preparing high purity nano material Download PDFInfo
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- CN110255612A CN110255612A CN201910665801.2A CN201910665801A CN110255612A CN 110255612 A CN110255612 A CN 110255612A CN 201910665801 A CN201910665801 A CN 201910665801A CN 110255612 A CN110255612 A CN 110255612A
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/003—Titanates
- C01G23/006—Alkaline earth titanates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
- C01G23/0532—Producing by wet processes, e.g. hydrolysing titanium salts by hydrolysing sulfate-containing salts
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
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- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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Abstract
The present invention relates to a kind of device and methods for preparing high purity nano material, it is characterised in that: a. dissolved salt raw material storage tank (1) is connected by first pipe (3) with hydrothermal reaction kettle (7)；B. additive storage tank (10) is connected by second pipe (14) with hydrothermal reaction kettle (7)；C. metal salt starting materials storage tank (15) is connected by third pipeline (17) with hydrothermal reaction kettle (7)；D. hydrothermal reaction kettle (7) bottom is connected at the top of hydrothermal reaction kettle (7) by the 4th pipeline (23)；E. the 5th pipeline (26) is connected on the 4th pipeline (23), the 5th pipeline (26) is successively connected with ceramic membrane cleaning machine, cold wind drier.It is high-efficient, have a wide range of application, shorten material homogenizer, emulsification times, yield rate and greatly improve the invention has the advantages that structure is simple, at low cost, easily operated, secondary pollution is prevented, ensure that purity.
Description
Technical field
The invention belongs to nano-powder material manufacturing fields, are related to a kind of device and method for preparing high purity nano material.
Background technique
In recent years, sonochemistry can have the advantages that uniqueness due to sound, and without secondary pollution, and equipment is simple, easy to operate,
There is highly important application in fields such as nano material, catalysis reaction, substance synthesis, sewage treatments.Simultaneously hydro-thermal reaction because
The special reaction and effect having the function of, it is also increasingly developed in ultra-fine and nanometer materials development and application at present,
Its principle is that pressure is greater than the aqueous medium condition of 0.1MPa in the closed system greater than 80 DEG C or more using hydro-thermal reaction equipment
The synthetic method of heterogeneous phase chemical reaction between lower generation reaction mass.
Currently, countries in the world (China, Japan, the U.S., Britain, Germany etc.) is although to the research of hydrothermal synthesis technology
Major progress is achieved, but sonochemistry is combined with hydrothermal synthesis reaction method and large-scale application in the industrial production
Research is not much.A kind of ultrasound such as used in 102350288 A of patent publication No. CN-hydrothermal reaction coupling prepares nano material
Device, device is by the fixed group such as electrothermic thermostatic control box, hydrothermal reaction kettle, ultrasonic variable amplitude bar and ultrasonic transducer
At only a kind of use for laboratory can be used for preparing TiO2Nano powder, TiO2Nanotube, PbO nano powder, PbO nanotube or GdS
The problems in the nano materials such as nanotube, production can not be applied to and be fully solved many hydrothermal synthesis system materials；For another example exist
A kind of ultrasonic/microwave hydro-thermal/meto-super-critical reaction kettle, is also experimental facilities disclosed in patent publication No. CN207769762U,
It is used in being difficult to produce；For another example one of patent publication No. CN206103910U can add the hydrothermal reaction kettle of ultrasonic field, be to use
A kind of microscale experiment assembling device that solution crystallization influences is carried out on hydro-thermal method in research ultrasonic field；Hydro-thermal reaction pressure-bearing
Device is made of stainless steel closing cap, stainless steel outer cylinder and gasket, and ultrasonic generator and hydro-thermal reaction container are respectively positioned on not
It becomes rusty in steel outer cylinder, gasket is placed on hydro-thermal reaction container, stainless steel closing cap is tightened with the cooperation of stainless steel outer cylinder, and ultrasound occurs
Device is located at hydro-thermal reaction container bottom, and is separated by rotary table piece, and the ultrasonic field that ultrasonic generator generates passes through rotary table piece
It is transmitted in hydro-thermal reaction container.However, the reaction mass that the device only is used to directly mix with experiment, using external stainless steel
After outer cylinder is heated conduction enter by polytetrafluoroethylene (PTFE) reaction cover again with bottom combination of ultrasound, without mixing, circulating emulsion and
Change presoma apparatus system, hydro-thermal reaction duration, energy consumption is big, is also difficult to be continued in subsequent wash and dry production
The disadvantages of volume production.
Summary of the invention
It is an object of the present invention to solve the deficiency of the existing technology and provide a kind of device for preparing high purity nano material and
Method, the present apparatus are by ultrasonic device and hydrothermal synthesis equipment in conjunction with high pure electronic ceramic nano material is prepared, especially with
The nano ceramics raw material of hydro-thermal method basic principle synthesis.
To achieve the goals above, The technical solution adopted by the invention is as follows:
A kind of device preparing high purity nano material, it is characterised in that including following equipment: dissolved salt raw material storage tank, additive storage
Tank, metal salt starting materials storage tank, hydrothermal reaction kettle, ultrasonic device, ceramic membrane cleaning machine, cold wind drier；
Specific connection relationship is as follows:
A. dissolved salt raw material storage tank inside first pipe and hydrothermal reaction kettle by being connected；Dissolved salt metering is installed in first pipe
Pump is respectively equipped with a valve on the pipeline of dissolved salt metering pump two sides, and the first pipe outlet in hydrothermal reaction kettle is connected with the
One atomizer, the first atomizer are loaded onto or are unloaded by the first sealing；
B. additive storage tank inside second pipe and hydrothermal reaction kettle by being connected；Additive metering is installed on second pipe
It pumps, a valve is respectively installed on the pipeline of additive metering pump two sides；
C. metal salt starting materials storage tank inside third pipeline and hydrothermal reaction kettle by being connected；Metal salt is installed on third pipeline
Metering pump is respectively equipped with a valve on the pipeline of metal salt metering pump two sides；
D. hydrothermal reaction kettle outlet at bottom is connected to hydrothermal reaction kettle top entry by the 4th pipeline；Appearance is installed on 4th pipeline
Product pump, positive displacement pump are equipped with a valve close to the side of hydrothermal reaction kettle outlet at bottom, and product formula is pumped close to hydro-thermal reaction kettle top
The side installation of portion's entrance is connected with the second atomizer there are two valve, the 4th pipe outlet in hydrothermal reaction kettle, and second
Atomizer is loaded onto or is unloaded by the second sealing；
E. positive displacement pump and its export between adjacent valve the 5th pipeline of connection, the 5th pipeline by valve successively with ceramic membrane
Cleaning machine, cold wind drier are connected, and ultrasonic device is equipped on hydrothermal reaction kettle.
Further, the dissolved salt raw material storage tank and metal salt starting materials storage tank liner are polyurethane, polytetrafluoro material, additive
Storage tank is plastic material or glass material；First pipe, third pipeline are polytetrafluoroethylene (PTFE), in polypropylene, 316 stainless steel materials
It is any, second pipe be polytetrafluoroethylene (PTFE) or polypropylene (PP) material, the 4th pipeline be inner liner polytetrafluoroethylene
(PTFE) carbon steel material is moulded outside, and the 5th pipeline is polypropylene (PP) or polyethylene (PE) material；First atomizer, the second mist
Change spray head is spiral nozzle, and material is aluminium oxide ceramics or polypropylene (PP) material.
Further, the ultrasonic device includes sound insulation shield, ultrasonic vibrator and its PLC controller, and wherein sound insulation is anti-
Shield is foamed aluminium or centrifugally glass-wool material.
A method of preparing high purity nano material, it is characterised in that the following steps are included:
1) dissolved salt raw material storage tank is equipped with soluble zirconates or barium salt or titanium salt solution, metal salt starting materials storage tank are equipped with rare earth metal
Solubility salt or transition metal solubility salt solution, additive storage tank are equipped with polyethylene glycols, ketone, esters, acrylic acid
The water soluble dispersing agent of any one or two kinds of compositions of class, amides, alkyls, alcohols, by needed for production nano-powder material
Raw material and its corresponding mol ratio (corresponding mol ratio of reaction is general knowledge known in this field) pass through dissolved salt metering pump, additive respectively
Metering pump, metal salt metering pump carry out charging into hydrothermal reaction kettle and hybrid reaction slurry are made, and adjust reaction kettle and stir linear speed
5-10m/s is spent, stirs 10-30 minutes, is sufficiently mixed hybrid reaction slurry；
2) the subsequent hybrid reaction slurry of is formed in hydrothermal reaction kettle under volume pumping action by second spray head uniformly mixed
Solution；
3) opens ultrasonic device, and control supersonic frequency takes out the first atomizer, the in 10-60KHZ after 10-60 minutes ultrasonic
Two atomizers close the first sealing, the second sealing, keep closed in hydrothermal reaction kettle；
4) carries out heat temperature raising to hydrothermal reaction kettle, controls temperature at 130-150 DEG C, improves agitating paddle linear velocity to 10-20m/
S, insulation reaction 0.5-8h, is then cooled to 40-60 DEG C；
5) the nano pulp solution obtained after reaction is carried out ceramic membrane cleaning machine (aperture 5-10nm) washing and cold wind drier by
(20-30 DEG C of vacuum degree -0.09-0.096MPa, temperature) is dry, obtains high purity nanometer powders material.
Ultrasonic wave is a kind of sound wave of the frequency higher than 20000HZ, and wavelength is short, is similar to straightline propagation, its good directionality,
Penetration capacity is strong, and being easily obtained the sound energy relatively concentrated can be by the liquid in liquid environment when ultrasonic wave acoustic energy acts on liquid
Molecule forms cavitation effect, and then plays the role of emulsification, the dispersion to liquid material, is a kind of very high dispersion hand of intensity
Section, reduction reunion can achieve for the dispersion of superfine powder suspension using ultrasonic cavitation effect and dispersing ultrafine is particle stabilized
The effect of change.
Before hydro-thermal reaction, each raw material is emulsified and dispersed by the mode of ultrasonic sound energy, ultrasonic sound is utilized
The hydraulic shock of dead angle acumulation, dispersion and emulsification in mechanical stirring are made liquid material in closed hydro-thermal by the effect of wave current body
Uniform distribution dispersity is formed in reaction kettle, uses ceramic membrane washing filtering and cold air drying after hydro-thermal reaction
Prepare high-purity, ultra-fine, the uniform nano-powder material of particle diameter distribution.
Advantages of the present invention: 1. combine ultrasonic device and hydrothermal synthesis equipment, and structure is simple, realize the two function
Effective collaboration；It is high-efficient, have a wide range of application 2. the present apparatus is at low cost, easily operated；3. shorten material homogenizer, emulsification times,
Avoid the preparation condition (high temperature and pressure) of hydrothermal reaction kettle harshness；4. yield rate greatly improves, secondary pollution is prevented, ensure that pure
Degree；5. high-purity out for preparation of industrialization, ultra-fine, the uniform nano material of particle diameter distribution provides reference.
Detailed description of the invention
The basic structure schematic diagram of Fig. 1 present apparatus；
The high-purity nm cubic phase barium titanate electron microscope that Fig. 2 is produced using apparatus of the present invention and method；
The high-purity nm cubic phase barium titanate XRD diagram that Fig. 3 is produced using apparatus of the present invention and method；
The high-purity nm anatase titanium dioxide electron microscope that Fig. 4 is produced using apparatus of the present invention and method；
The high-purity nm anatase titanium dioxide XRD diagram that Fig. 5 is produced using apparatus of the present invention and method.
Specific embodiment
In order to which the present invention is more clearly understood, below in conjunction with Fig. 1, the invention will be further described:
A kind of device preparing high purity nano material, including following equipment:
A. dissolved salt raw material storage tank 1(polyurethane material) pass through first pipe 3(polytetrafluoroethylene (PTFE) material) and 7 top of hydrothermal reaction kettle
The first sealing 7a entrance be connected, be sequentially connected in series regulation gate valve 2, dissolved salt metering pump 4 in first pipe 3, unidirectional stop valve 5,
The outlet of first pipe 3 in hydrothermal reaction kettle 7 is connected with the first atomizer 6(aluminium oxide ceramics material with spiral nozzle)；
B. additive storage tank 10(plastic material) pass through second pipe 14(polytetrafluoroethylene (PTFE) material) with 7 top phase of hydrothermal reaction kettle
It is connected to, is sequentially connected in series regulation gate valve 11, additive metering pump 12, unidirectional stop valve 13 on second pipe 14；
C. metal salt starting materials storage tank 15(polytetrafluoro material) pass through third pipeline 17(polypropylene material) and 7 top of hydrothermal reaction kettle
It is connected, regulation gate valve 16, metal salt metering pump 18, unidirectional stop valve 19 is sequentially connected in series on third pipeline 17；
D. 7 outlet at bottom of hydrothermal reaction kettle is by moulding carbon steel material outside the 4th pipeline 23(inner liner polytetrafluoroethylene) and hydro-thermal reaction
The second sealing 7b entrance at 7 top of kettle is connected, and regulation gate valve 20, positive displacement pump 21, unidirectional section are sequentially connected in series on the 4th pipeline 23
Only valve 22, unidirectional stop valve 24, the 4th pipeline 23 outlet in hydrothermal reaction kettle 7 are connected with the second atomization spray with spiral nozzle
Head 25(polypropylene material)；
E. the 5th pipeline 26(polypropylene material of connection between neighbouring unidirectional stop valve 22 is exported in positive displacement pump 21 and positive displacement pump 21
Matter), unidirectional stop valve 27, ceramic membrane cleaning machine, cold wind drier are sequentially connected in series on the 5th pipeline 26；Pacify on hydrothermal reaction kettle 7
Equipped with ultrasonic device 9, ultrasonic device 9 includes sound insulation shield 8(centrifugally glass-wool material), ultrasonic vibrator 28 and its PLC control
Device processed.
Embodiment 1
A method of high-purity barium titanate nano-powder material being prepared, specific implementation step is as follows:
1, regulation gate valve 20 and unidirectional stop valve 24 are closed, first successively opens unidirectional stop valve 5,13 and 19, then open regulator
Valve 2,11 and 16, respectively successively by dissolved salt metering pump 4, additive metering pump 12, metal salt metering pump 18 to hydrothermal reaction kettle 7
It is middle to add the barium hydroxide solution in dissolved salt raw material storage tank 1, the hydrated titanium dioxide solution in metal salt starting materials storage tank 15 and divide
Polyethylene glycol in powder storage tank 10 mixes dispersion solvent (5 ﹕ 1 of molar ratio of polyethylene glycol and acetamide), dissolved salt with acetamide
The spiral that solution passes through the first atomizer 6 respectively in raw material storage tank 1, metal salt starting materials storage tank 15 and additive storage tank 10 is sprayed
Mouth, 14 nozzle of second pipe are added in hydrothermal reaction kettle 7 to be made and be mixed instead with 17 nozzle of third pipeline by the molar ratio of 15:10:2
Slurry is answered, hydrothermal reaction kettle is adjusted and stirs linear velocity 8.25m/s, stirring makes to be sufficiently mixed for 20 minutes；
2, first open regulation gate valve 20, unidirectional stop valve 22, unidirectional stop valve 24, close unidirectional stop valve 27, regulation gate valve 2,
Unidirectional stop valve 5, regulation gate valve 11, unidirectional stop valve 13, regulation gate valve 16 and unidirectional stop valve 19, are then turned on positive displacement pump 21,
Hybrid reaction slurry is set to form uniformly mixed solution in hydrothermal reaction kettle 7 by the spiral nozzle of the second atomizer 25；
3, ultrasonic vibrator 28 is opened, control supersonic frequency closes regulation gate valve 20 and positive displacement pump in 45KHZ, ultrasound after 30 minutes
21, the first atomizer 6 and the second atomizer 25 are taken out, the first sealing 7a, the second sealing 7b is closed, keeps hydrothermal reaction kettle
It is closed in 7；
4, heat temperature raising is carried out to hydrothermal reaction kettle 7, controls 135 DEG C of maximum temperature, improved agitating paddle linear velocity to 15m/S, protect
Temperature reaction 4h, is then cooled to 60 DEG C；
5, it opens at regulation gate valve 20 and unidirectional stop valve 24 and seals, close unidirectional stop valve 22, open unidirectional stop valve 27, open
Dynamic positive displacement pump 21 is washed the nano pulp solution after reaction by aperture 10nm ceramic membrane cleaning machine, then in vacuum degree-
0.09-0.096MPa, cold air drying is carried out under the conditions of 30 DEG C, can be prepared by high-purity barium titanate nano-powder material.
Embodiment 2
A method of high-purity titanium dioxide nano-powder material being prepared, specific implementation step is as follows:
1, regulation gate valve 20 and unidirectional stop valve 24 are closed, first successively opens unidirectional stop valve 5,13 and 19, then open regulator
Valve 2,11 and 16, respectively successively by dissolved salt metering pump 4, additive metering pump 12, metal salt metering pump 18 to hydrothermal reaction kettle 7
Titanium sulfate solution, the ammonia spirit in metal salt starting materials storage tank 15 and additive storage tank 10 in middle addition dissolved salt raw material storage tank 1
In polyethylene glycol dispersion solvent, dissolved salt raw material storage tank 1, metal salt starting materials storage tank 15 and solution in additive storage tank 10 pass through respectively
The spiral nozzle, 14 nozzle of second pipe and 17 nozzle of third pipeline for crossing the first atomizer 6 are added by the molar ratio of 1:4:0.2
It is made in hydrothermal reaction kettle 7 hybrid reaction slurry (pH is between 8-9), adjusts hydrothermal reaction kettle and stir linear velocity 7.5m/s, stir
Mixing 30 minutes makes to be sufficiently mixed；
2, first open regulation gate valve 20, unidirectional stop valve 22, unidirectional stop valve 24, close unidirectional stop valve 27, regulation gate valve 2,
Unidirectional stop valve 5, regulation gate valve 11, unidirectional stop valve 13, regulation gate valve 16 and unidirectional stop valve 19, are then turned on positive displacement pump 21,
Hybrid reaction slurry is set to form uniformly mixed solution in hydrothermal reaction kettle 7 by the spiral nozzle of the second atomizer 25；
3, ultrasonic vibrator 28 is opened, control supersonic frequency closes regulation gate valve 20 and positive displacement pump in 50KHZ, ultrasound after twenty minutes
21, the first atomizer 6 and the second atomizer 25 are taken out, the first sealing 7a, the second sealing 7b is closed, keeps hydrothermal reaction kettle
It is closed in 7；
4, heat temperature raising is carried out to hydrothermal reaction kettle 7, controls 150 DEG C of maximum temperature, improved agitating paddle linear velocity to 10m/S, protect
Temperature reaction 3h, is then cooled to 50 DEG C；
5, it opens at regulation gate valve 20 and unidirectional stop valve 24 and seals, close unidirectional stop valve 22, open unidirectional stop valve 27, open
Dynamic positive displacement pump 21 is washed the nano pulp solution after reaction by aperture 5nm ceramic membrane cleaning machine, then in vacuum degree-
0.09-0.096MPa, cold air drying is carried out under the conditions of 20 DEG C, can be prepared by high-purity titanium dioxide nano-powder material.
Embodiment 3
A method of high-purity yttrium stable zirconium oxide nano-powder material being prepared, specific implementation step is as follows:
1, regulation gate valve 20 and unidirectional stop valve 24 are closed, first successively opens unidirectional stop valve 5,13 and 19, then open regulator
Valve 2,11 and 16, respectively successively by dissolved salt metering pump 4, additive metering pump 12, metal salt metering pump 18 to hydrothermal reaction kettle 7
Zirconium nitrate solution in middle addition dissolved salt raw material storage tank 1, nitric hydrate yttrium solution and dispersing agent in metal salt starting materials storage tank 15
Polyethylene glycol and sodium hydrate aqueous solution in storage tank 10 mix dispersion solvent (mole of polyethylene glycol and sodium hydrate aqueous solution
Than 1 ﹕ 15), dissolved salt raw material storage tank 1, metal salt starting materials storage tank 15 and solution in additive storage tank 10 pass through the first atomization spray respectively
Hydro-thermal is added by the molar ratio of 15:1:2 in first 6 spiral nozzle (PP material), 14 nozzle of second pipe and 17 nozzle of third pipeline
Hybrid reaction slurry is made in reaction kettle 7, adjusts hydrothermal reaction kettle and stirs linear velocity 4.5m/s, stirring makes sufficiently mixed for 15 minutes
It closes；
2, first open regulation gate valve 20, unidirectional stop valve 22, unidirectional stop valve 24, close unidirectional stop valve 27, regulation gate valve 2,
Unidirectional stop valve 5, regulation gate valve 11, unidirectional stop valve 13, regulation gate valve 16 and unidirectional stop valve 19, are then turned on positive displacement pump 21,
Hybrid reaction slurry is set to form uniformly mixed solution in hydrothermal reaction kettle 7 by the spiral nozzle of the second atomizer 25；
3, ultrasonic vibrator 28 is opened, control supersonic frequency closes regulation gate valve 20 and positive displacement pump in 40KHZ, ultrasound after 30 minutes
21, the first atomizer 6 and the second atomizer 25 are taken out, the first sealing 7a, the second sealing 7b is closed, keeps hydrothermal reaction kettle
It is closed in 7；
4, heat temperature raising is carried out to hydrothermal reaction kettle 7, controls 150 DEG C of maximum temperature, improve agitating paddle linear velocity to 8m/S, heat preservation
8h is reacted, is then cooled to 40 DEG C；
5, it opens at regulation gate valve 20 and unidirectional stop valve 24 and seals, close unidirectional stop valve 22, open unidirectional stop valve 27, open
Dynamic positive displacement pump 21 is washed the nano pulp solution after reaction by aperture 5nm ceramic membrane cleaning machine, then in vacuum degree-
0.09-0.096MPa, cold air drying is carried out under the conditions of 20 DEG C, can be prepared by high-purity yttrium stable zirconium oxide nano-powder material.
As with field emission scanning electron microscope (SEM) to barium titanate nano made from embodiment 1, embodiment 2
Powder and nano TiO 2 powder carry out surface topography, granular size and its crystal structure test analysis.Every batch of sample repeats
Test is not less than 3, and particle is no less than 100 in every electron microscope, and granule-morphology size statistical result takes its average value.It is made
Barium Titanate nano-powder material be cubic phase high-purity crystal structure, average Electronic Speculum size is in 62.49nm；Titanium dioxide is received
Rice powder body material is anatase titanium dioxide high-purity crystal structure, and without other miscellaneous peaks, average Electronic Speculum size is in 28.42nm；Yttrium Stable Oxygen
Change zirconium nano-powder is semi-stability structure, and average Electronic Speculum size is in 20.15nm.
In the present invention, " installation ", " connected " etc. shall be understood in a broad sense.It, can also be with for example, for example it may be said that be fixedly connected
Say dismantling connection or integrally connected, it may be said that be directly connected to be also possible to connect by intermediary, can be external connection
It may be said that internal connection.
Above embodiments are only that a specific embodiment of the invention is described, and are not carried out to the scope of the present invention
It limits, those skilled in the art can also do numerous modifications and variations in prior art basis, not depart from spirit of that invention
Under the premise of, this field ordinary engineering and technical personnel each falls within this to all variations and modifications that technical solution of the present invention is made
In the protection scope that invention claims determine.
Claims (4)
1. a kind of device for preparing high purity nano material, it is characterised in that including following equipment: dissolved salt raw material storage tank (1), addition
Agent storage tank (10), metal salt starting materials storage tank (15), hydrothermal reaction kettle (7), ultrasonic device (9), ceramic membrane cleaning machine, cold air drying
Machine；
Specific connection relationship is as follows:
A. dissolved salt raw material storage tank (1) inside first pipe (3) and hydrothermal reaction kettle (7) by being connected；First pipe is installed on (3)
Have dissolved salt metering pump (4), a valve is respectively installed on the pipeline of dissolved salt metering pump (4) two sides, in hydrothermal reaction kettle (7)
First pipe (3) outlet is connected with the first atomizer (6), and the first atomizer (6) is loaded onto or unloaded by the first sealing (7a)；
B. additive storage tank (10) inside second pipe (14) and hydrothermal reaction kettle (7) by being connected；Second pipe is pacified on (14)
Equipped with additive metering pump (12), a valve is respectively installed on the pipeline of additive metering pump (12) two sides；
C. metal salt starting materials storage tank (15) inside third pipeline (17) and hydrothermal reaction kettle (7) by being connected；Third pipeline (17)
On be equipped with metal salt metering pump (18), a valve is respectively installed on the pipeline of metal salt metering pump (18) two sides；
D. hydrothermal reaction kettle (7) outlet at bottom is connected to hydrothermal reaction kettle (7) top entry by the 4th pipeline (23)；4th pipeline
(23) it is equipped on positive displacement pump (21), positive displacement pump (21) is equipped with a valve close to the side of hydrothermal reaction kettle (7) outlet at bottom
Door, positive displacement pump (21) is close to the installation of the side of hydrothermal reaction kettle (7) top entry there are two valve, in hydrothermal reaction kettle (7)
The 4th pipeline (23) outlet be connected with the second atomizer (25), the second atomizer (25) by second sealing (7b) load onto or
It unloads；
E. positive displacement pump (21) and its export between adjacent valve the 5th pipeline (26) of connection, the 5th pipeline (26) passes through valve
Successively it is connected with ceramic membrane cleaning machine, cold wind drier, ultrasonic device (9) is installed on hydrothermal reaction kettle (7).
2. a kind of device for preparing high purity nano material according to claim 1, it is characterised in that: the dissolved salt raw material storage tank
(1) and metal salt starting materials storage tank (15) liner is polyurethane, polytetrafluoro material, and additive storage tank (10) is plastic material or glass
Material；First pipe (3), third pipeline (17) be any one of polytetrafluoroethylene (PTFE), polypropylene, 316 stainless steel materials, second
Pipeline (14) is polytetrafluoroethylene (PTFE) or polypropylene material, and the 4th pipeline (23) is that carbon steel material is moulded outside inner liner polytetrafluoroethylene；The
Five pipelines (26) are polypropylene or polyethylene material；First atomizer (6), the second atomizer (25) are spiral nozzle, material
Matter is aluminium oxide ceramics or polypropylene material.
3. a kind of device for preparing high purity nano material according to claim 1, it is characterised in that: the ultrasonic device (9)
Including sound insulation shield (8), ultrasonic vibrator (28) and its PLC controller, wherein sound insulation shield is foamed aluminium or centrifugation glass
Glass cotton material.
4. a kind of method for preparing high purity nano material using device described in claim 1,2 or 3, it is characterised in that including with
Lower step:
1) dissolved salt raw material storage tank (1) is equipped with soluble zirconates or barium salt or titanium salt solution, metal salt starting materials storage tank (15) are equipped with
Rare earth metal solubility salt or transition metal solubility salt solution, additive storage tank (10) equipped with polyethylene glycols, ketone,
The water soluble dispersing agent of any one or two kinds of compositions of esters, acrylic compounds, amides, alkyls, alcohols, by production nano-powder
Raw material needed for material and its corresponding mol ratio pass through dissolved salt metering pump (4), additive metering pump (12), metal salt metering respectively
Pump (18) carries out charging in hydrothermal reaction kettle (7) and hybrid reaction slurry is made, and adjusts reaction kettle and stirs linear velocity 5- 10m/s,
Stirring is sufficiently mixed hybrid reaction slurry in 10-30 minutes；
2) the subsequent hybrid reaction slurry of passes through second spray head (25) in hydrothermal reaction kettle (7) interior shape under positive displacement pump (21) effect
At uniformly mixed solution；
3) opens ultrasonic device (9), controls supersonic frequency in 10-60KHZ, the first atomizer is taken out after 10-60 minutes ultrasonic
(6), the second atomizer (25) close the first sealing (7a), the second sealing (7b), keep closed in hydrothermal reaction kettle (7)；
4) carries out heat temperature raising to hydrothermal reaction kettle (7), controls temperature at 130-150 DEG C, improves agitating paddle linear velocity to 10-
20m/S, insulation reaction 0.5-8h, is then cooled to 40-60 DEG C；
5) the nano pulp solution obtained after reaction is carried out the washing of ceramic membrane cleaning machine by and cold wind drier is dry, is obtained
High purity nanometer powders material.
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