CN210457505U - Device for preparing high-purity nano material - Google Patents
Device for preparing high-purity nano material Download PDFInfo
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- CN210457505U CN210457505U CN201921160405.6U CN201921160405U CN210457505U CN 210457505 U CN210457505 U CN 210457505U CN 201921160405 U CN201921160405 U CN 201921160405U CN 210457505 U CN210457505 U CN 210457505U
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Abstract
The utility model relates to a device of preparation high-purity nano-material, its characterized in that: a. the dissolved salt raw material storage tank (1) is connected with the hydrothermal reaction kettle (7) through a first pipeline (3); b. the additive storage tank (10) is connected with the hydrothermal reaction kettle (7) through a second pipeline (14); c. a metal salt raw material storage tank (15) is connected with the hydrothermal reaction kettle (7) through a third pipeline (17); d. the bottom of the hydrothermal reaction kettle (7) is connected to the top of the hydrothermal reaction kettle (7) through a fourth pipeline (23); e. and the fourth pipeline (23) is connected with a fifth pipeline (26), and the fifth pipeline (26) is sequentially connected with the ceramic membrane cleaning machine and the cold air drying machine. The utility model discloses the advantage: simple structure, low cost, easy operation, high efficiency, wide application range, shortened raw material homogenizing and emulsifying time, no secondary pollution and ensured purity.
Description
Technical Field
The utility model belongs to the field of nano powder material manufacturing, and relates to a device for preparing high-purity nano materials.
Background
In recent years, sonochemistry has unique advantages due to sound energy, no secondary pollution, simple equipment and convenient operation, and has very important application in the fields of nano materials, catalytic reaction, substance synthesis, sewage treatment and the like. Meanwhile, due to special reaction functions and effects of hydrothermal reaction, the development and application of superfine and nano-grade materials are increasingly developed at present, and the principle of the method is a synthesis method of heterogeneous chemical reaction between reaction materials by adopting hydrothermal reaction equipment in a closed system at the temperature of more than 80 ℃ and under the condition of water medium with the pressure of more than 0.1 MPa.
Currently, although research on hydrothermal synthesis techniques has been mainly advanced in countries of the world (china, japan, usa, uk, germany, etc.), research on large-scale application of the combination of sonochemistry and hydrothermal synthesis reaction methods in industrial production has not been much. For example, in patent publication No. CN 102350288A, an apparatus for preparing nano-material by ultrasonic-hydrothermal coupling is composed of an electrothermal constant-temperature control box, a hydrothermal reaction kettle, an ultrasonic amplitude transformer, an ultrasonic transducer and the like, and is only a laboratory apparatus for preparing TiO2Nano powder, TiO2Nano materials such as nano tubes, PbO nano powder, PbO nano tubes or GdS nano tubes and the like can not be applied to production and can completely solve the problems in many hydrothermal synthesis system materials; also, an ultrasonic/microwave hydrothermal/sub-supercritical reaction kettle as disclosed in patent publication No. CN207769762U is also experimental equipment, and is difficult to use in production; for another example, a hydrothermal reaction kettle capable of being added with an ultrasonic field in patent publication No. CN206103910U is an assembling device for a miniature experiment for researching the influence of the ultrasonic field on solution crystallization by using a hydrothermal method; the hydrothermal reaction pressure-bearing device consists of a stainless steel closing cover, a stainless steel outer cylinder and a gasket, wherein an ultrasonic generating device and a hydrothermal reaction container are both positioned in the stainless steel outer cylinder, the gasket is arranged on the hydrothermal reaction container, the stainless steel closing cover and the stainless steel outer cylinder are matched and screwed, the ultrasonic generating device is positioned at the bottom of the hydrothermal reaction container and is separated by a circular truncated cone, and an ultrasonic field generated by the ultrasonic generating device is transmitted into the hydrothermal reaction container through the circular truncated cone. However, the device is only used for directly mixing reaction materials in experiments, adopts an external stainless steel outer cylinder to be heated and then is conducted into a polytetrafluoroethylene reaction tank cover to be ultrasonically combined with the bottom, and has the defects of long hydrothermal reaction time, high energy consumption, difficulty in continuous mass production in subsequent washing and drying production and the like without stirring, circulating emulsification and precursor homogenizing device systems.
SUMMERY OF THE UTILITY MODEL
The utility model aims at solving the defects of the prior art and providing a device for preparing high-purity nano materials, which combines ultrasonic equipment and hydrothermal synthesis equipment to prepare high-purity electronic ceramic nano materials, in particular to nano ceramic raw materials synthesized by the basic principle of a hydrothermal method.
In order to realize the purpose, the utility model discloses a technical scheme as follows:
an apparatus for preparing high-purity nano material is characterized by comprising the following equipment: a dissolved salt raw material storage tank, an additive storage tank, a metal salt raw material storage tank, a hydrothermal reaction kettle, ultrasonic equipment, a ceramic membrane cleaning machine and a cold air drying machine;
the specific connection relationship is as follows:
a. the dissolved salt raw material storage tank is communicated with the interior of the hydrothermal reaction kettle through a first pipeline; a first pipeline is provided with a dissolved salt metering pump, the pipelines at two sides of the dissolved salt metering pump are respectively provided with a valve, the outlet of the first pipeline in the hydrothermal reaction kettle is connected with a first atomizing nozzle, and the first atomizing nozzle is mounted or dismounted through a first seal;
b. the additive storage tank is communicated with the interior of the hydrothermal reaction kettle through a second pipeline; an additive metering pump is arranged on the second pipeline, and a valve is respectively arranged on the pipelines at two sides of the additive metering pump;
c. the metal salt raw material storage tank is communicated with the interior of the hydrothermal reaction kettle through a third pipeline; a metal salt metering pump is arranged on the third pipeline, and a valve is respectively arranged on the pipelines at two sides of the metal salt metering pump;
d. the bottom outlet of the hydrothermal reaction kettle is connected to the top inlet of the hydrothermal reaction kettle through a fourth pipeline; a positive displacement pump is arranged on the fourth pipeline, one side of the positive displacement pump, which is close to the bottom outlet of the hydrothermal reaction kettle, is provided with a valve, one side of the positive displacement pump, which is close to the top inlet of the hydrothermal reaction kettle, is provided with two valves, the outlet of the fourth pipeline in the hydrothermal reaction kettle is connected with a second atomizing nozzle, and the second atomizing nozzle is arranged on or detached from the fourth pipeline through a second seal;
e. and a fifth pipeline is connected between the displacement pump and a valve adjacent to an outlet of the displacement pump, the fifth pipeline is sequentially connected with the ceramic membrane cleaning machine and the cold air dryer through the valve, and the hydrothermal reaction kettle is provided with ultrasonic equipment.
Further, the inner linings of the salt dissolving raw material storage tank and the metal salt raw material storage tank are made of polyurethane and polytetrafluoroethylene, and the additive storage tank is made of plastic or glass; the first pipeline and the third pipeline are made of any one of polytetrafluoroethylene, polypropylene and 316 stainless steel materials, the second pipeline is made of Polytetrafluoroethylene (PTFE) or polypropylene (PP), the fourth pipeline is made of carbon steel materials with Polytetrafluoroethylene (PTFE) as an inner lining and plastic carbon steel materials as an outer lining, and the fifth pipeline is made of polypropylene (PP) or Polyethylene (PE); the first atomizer and the second atomizer are spiral nozzles made of alumina ceramics or polypropylene (PP).
Further, the ultrasonic equipment comprises a sound insulation protective cover, an ultrasonic vibrator and a PLC controller thereof, wherein the sound insulation protective cover is made of foamed aluminum or centrifugal glass wool.
A method for preparing high-purity nano materials is characterized by comprising the following steps:
1) a soluble zirconium salt solution, a soluble barium salt solution, a soluble titanium salt solution, a soluble rare earth metal salt solution, a soluble transition metal salt solution, a soluble polyethylene glycol dispersant, a soluble ketone dispersant, a soluble ester dispersant, a soluble acrylate dispersant, a soluble amide dispersant, a soluble alkyl dispersant and a soluble alcohol dispersant are respectively filled in a soluble salt raw material storage tank and an additive storage tank, the soluble zirconium salt solution, the soluble barium salt solution, the soluble titanium salt solution and the soluble transition metal salt solution are respectively filled in a hydrothermal reaction kettle through a soluble salt metering pump, an additive metering pump and a metal salt metering pump according to raw materials required for producing a nano powder material and corresponding molar ratios (the corresponding molar ratio of the reaction is common knowledge in the field) of the hydrothermal reaction kettle to prepare mixed reaction slurry, the stirring linear speed of the reaction kettle;
2) forming a uniformly mixed solution in the hydrothermal reaction kettle by the mixed reaction slurry through a second spray head under the action of a positive displacement pump;
3) opening the ultrasonic equipment, controlling the ultrasonic frequency to be 10-60KHZ, taking out the first atomizing nozzle and the second atomizing nozzle after carrying out ultrasonic treatment for 10-60 minutes, closing the first seal and the second seal, and keeping the hydrothermal reaction kettle sealed;
4) heating the hydrothermal reaction kettle to raise the temperature, controlling the temperature at 130-150 ℃, increasing the linear velocity of the stirring paddle to 10-20m/S, carrying out heat preservation reaction for 0.5-8h, and then cooling to 40-60 ℃;
5) and washing the nano slurry solution obtained after the reaction by a ceramic membrane cleaning machine (with the aperture of 5-10 nm) and drying by a cold air drying machine (with the vacuum degree of-0.09-0.096 MPa and the temperature of 20-30 ℃) to obtain the high-purity nano powder material.
The ultrasonic wave is a sound wave with the frequency higher than 20000HZ, the wavelength is short, the ultrasonic wave is approximately in linear propagation, the directivity is good, the penetrating capability is strong, more concentrated sound energy is easy to obtain, when the ultrasonic sound energy acts on liquid, liquid molecules in a liquid environment can form a cavitation effect, and further the liquid material is emulsified and dispersed, the ultrasonic wave is a dispersion means with very high intensity, and the ultrasonic wave cavitation is adopted for dispersing the superfine powder suspension, so that the effects of reducing agglomeration and stabilizing dispersed superfine particles can be achieved.
Before hydrothermal reaction, emulsifying and dispersing the raw materials in an ultrasonic sound energy mode, impacting, dispersing and emulsifying liquid accumulated in dead corners in mechanical stirring under the action of ultrasonic sound wave fluid to enable the liquid materials to form a uniformly distributed and dispersed state in a closed hydrothermal reaction kettle, and after the hydrothermal reaction is finished, washing and filtering by using a ceramic membrane and drying by using cold air to prepare the high-purity, superfine and uniformly-distributed nano powder material.
The utility model has the advantages that: 1. the ultrasonic equipment and the hydrothermal synthesis equipment are combined, the structure is simple, and the effective cooperation of the functions of the ultrasonic equipment and the hydrothermal synthesis equipment is realized; 2. the device has low cost, easy operation, high efficiency and wide application range; 3. the raw material homogenization and emulsification time is shortened, and the harsh preparation conditions (high temperature and high pressure) of a hydrothermal reaction kettle are avoided; 4. the yield is greatly improved, secondary pollution is prevented, and the purity is ensured; 5. provides reference for the industrialized preparation of the nano material with high purity, superfine and uniform particle size distribution.
Drawings
FIG. 1 is a schematic diagram of the basic structure of the device;
FIG. 2 is an electron microscope image of high purity nano cubic phase barium titanate produced by the apparatus and method of the present invention;
FIG. 3 is an XRD pattern of high purity nano cubic phase barium titanate produced by the apparatus and method of the present invention;
FIG. 4 is an electron microscope image of high purity nano anatase titanium dioxide produced by the apparatus and method of the present invention;
figure 5 is an XRD pattern of the high purity nano anatase titanium dioxide produced by the apparatus and method of the present invention.
Detailed Description
In order to make the present invention more clear, the present invention is further explained with reference to fig. 1 as follows:
an apparatus for preparing high-purity nano material comprises the following equipment:
a. a dissolved salt raw material storage tank 1 (made of polyurethane) is communicated with an inlet of a first seal 7a at the top of a hydrothermal reaction kettle 7 through a first pipeline 3 (made of polytetrafluoroethylene), the first pipeline 3 is sequentially connected with an adjusting gate valve 2, a dissolved salt metering pump 4 and a one-way stop valve 5 in series, and an outlet of the first pipeline 3 in the hydrothermal reaction kettle 7 is connected with a first atomizing nozzle 6 (made of alumina ceramic) with a spiral nozzle;
b. an additive storage tank 10 (made of plastic) is communicated with the top of the hydrothermal reaction kettle 7 through a second pipeline 14 (made of polytetrafluoroethylene), and an adjusting gate valve 11, an additive metering pump 12 and a one-way stop valve 13 are sequentially connected on the second pipeline 14 in series;
c. a metal salt raw material storage tank 15 (made of polytetrafluoroethylene) is communicated with the top of the hydrothermal reaction kettle 7 through a third pipeline 17 (made of polypropylene), and a regulating gate valve 16, a metal salt metering pump 18 and a one-way stop valve 19 are sequentially connected on the third pipeline 17 in series;
d. an outlet at the bottom of the hydrothermal reaction kettle 7 is communicated with an inlet of a second seal 7b at the top of the hydrothermal reaction kettle 7 through a fourth pipeline 23 (made of polytetrafluoroethylene-lined outer plastic carbon steel), the fourth pipeline 23 is sequentially connected with an adjusting gate valve 20, a displacement pump 21, a one-way stop valve 22 and a one-way stop valve 24 in series, and an outlet of the fourth pipeline 23 in the hydrothermal reaction kettle 7 is connected with a second atomizing nozzle 25 (made of polypropylene) with a spiral nozzle;
e. a fifth pipeline 26 (made of polypropylene) is connected between the displacement pump 21 and the one-way stop valve 22 adjacent to the outlet of the displacement pump 21, and the fifth pipeline 26 is sequentially connected with the one-way stop valve 27, the ceramic membrane cleaning machine and the cold air drying machine in series; the hydrothermal reaction kettle 7 is provided with ultrasonic equipment 9, and the ultrasonic equipment 9 comprises a sound insulation protective cover 8 (made of centrifugal glass wool), an ultrasonic vibrator 28 and a PLC (programmable logic controller).
Example 1
A method for preparing high-purity barium titanate nano powder material comprises the following specific implementation steps:
1. closing the adjusting gate valve 20 and the one-way stop valve 24, opening the one-way stop valves 5, 13 and 19 in sequence, opening the adjusting gate valves 2, 11 and 16, adding the barium hydroxide solution in the dissolved salt raw material storage tank 1, the hydrated titanium dioxide solution in the metal salt raw material storage tank 15 and the polyethylene glycol and acetamide mixed dispersion solvent (the molar ratio of the polyethylene glycol to the acetamide is 5: 1) in the dispersion solvent storage tank 10 into the hydrothermal reaction kettle 7 through the dissolved salt metering pump 4, the additive metering pump 12 and the metal salt metering pump 18 in sequence, adding the solution in the dissolved salt raw material storage tank 1, the metal salt raw material storage tank 15 and the additive storage tank 10 into the hydrothermal reaction kettle 7 through the spiral nozzle of the first atomizing nozzle 6, the pipe orifice of the second pipeline 14 and the pipe orifice of the third pipeline 17 in the molar ratio of 15:10:2 to prepare mixed reaction slurry, adjusting the stirring linear velocity of the hydrothermal reaction kettle to 8.25m, stirring for 20 minutes to mix thoroughly;
2. firstly, opening the regulating gate valve 20, the one-way stop valve 22 and the one-way stop valve 24, closing the one-way stop valve 27, the regulating gate valve 2, the one-way stop valve 5, the regulating gate valve 11, the one-way stop valve 13, the regulating gate valve 16 and the one-way stop valve 19, and then opening the displacement pump 21 to enable the mixed reaction slurry to form a uniformly mixed solution in the hydrothermal reaction kettle 7 through the spiral nozzle of the second atomizer 25;
3. opening an ultrasonic vibrator 28, controlling the ultrasonic frequency to be 45KHZ, closing the regulating gate valve 20 and the volumetric pump 21 after 30 minutes of ultrasonic treatment, taking out the first atomizing nozzle 6 and the second atomizing nozzle 25, closing the first seal 7a and the second seal 7b, and keeping the interior of the hydrothermal reaction kettle 7 sealed;
4. heating the hydrothermal reaction kettle 7, controlling the highest temperature to be 135 ℃, increasing the linear velocity of the stirring paddle to 15m/S, carrying out heat preservation reaction for 4 hours, and then cooling to 60 ℃;
5. opening the adjusting gate valve 20 and the one-way stop valve 24 for sealing, closing the one-way stop valve 22, opening the one-way stop valve 27, starting the displacement pump 21, washing the reacted nano slurry solution by a ceramic membrane cleaning machine with the aperture of 10nm, and then carrying out cold air drying under the conditions of vacuum degree of-0.09-0.096 MPa and 30 ℃ to obtain the high-purity barium titanate nano powder material.
Example 2
A method for preparing high-purity titanium dioxide nano powder material comprises the following specific implementation steps:
1. closing the regulating gate valve 20 and the one-way stop valve 24, opening the one-way stop valves 5, 13 and 19 in sequence, opening the regulating gate valves 2, 11 and 16, passing through the dissolved salt metering pump 4 and the additive metering pump 12 in sequence, adding a titanium sulfate solution in a dissolved salt raw material storage tank 1, an ammonia water solution in a metal salt raw material storage tank 15 and a polyethylene glycol dispersion solvent in an additive storage tank 10 into a hydrothermal reaction kettle 7 by a metal salt metering pump 18, adding the solutions in the dissolved salt raw material storage tank 1, the metal salt raw material storage tank 15 and the additive storage tank 10 into the hydrothermal reaction kettle 7 respectively through a spiral nozzle of a first atomizing nozzle 6, a pipe orifice of a second pipeline 14 and a pipe orifice of a third pipeline 17 according to a molar ratio of 1:4:0.2 to prepare mixed reaction slurry (the pH is between 8 and 9), adjusting the stirring linear speed of the hydrothermal reaction kettle to be 7.5m/s, and stirring for 30 minutes to fully mix;
2. firstly, opening the regulating gate valve 20, the one-way stop valve 22 and the one-way stop valve 24, closing the one-way stop valve 27, the regulating gate valve 2, the one-way stop valve 5, the regulating gate valve 11, the one-way stop valve 13, the regulating gate valve 16 and the one-way stop valve 19, and then opening the displacement pump 21 to enable the mixed reaction slurry to form a uniformly mixed solution in the hydrothermal reaction kettle 7 through the spiral nozzle of the second atomizer 25;
3. opening an ultrasonic vibrator 28, controlling the ultrasonic frequency to be 50KHZ, closing the adjusting gate valve 20 and the volumetric pump 21 after ultrasonic treatment is carried out for 20 minutes, taking out the first atomizing nozzle 6 and the second atomizing nozzle 25, closing the first seal 7a and the second seal 7b, and keeping the interior of the hydrothermal reaction kettle 7 sealed;
4. heating the hydrothermal reaction kettle 7, controlling the highest temperature to be 150 ℃, increasing the linear velocity of the stirring paddle to 10m/S, carrying out heat preservation reaction for 3 hours, and then cooling to 50 ℃;
5. opening the regulating gate valve 20 and the one-way stop valve 24 for sealing, closing the one-way stop valve 22, opening the one-way stop valve 27, starting the displacement pump 21, washing the reacted nano slurry solution by a ceramic membrane cleaning machine with the aperture of 5nm, and then carrying out cold air drying under the conditions of vacuum degree of-0.09-0.096 MPa and 20 ℃ to obtain the high-purity titanium dioxide nano powder material.
Example 3
A method for preparing a high-purity yttrium-stabilized zirconia nano-powder material comprises the following specific implementation steps:
1. closing the adjusting gate valve 20 and the one-way stop valve 24, opening the one-way stop valves 5, 13 and 19 in sequence, opening the adjusting gate valves 2, 11 and 16, adding the zirconium nitrate solution in the dissolved salt raw material storage tank 1, the hydrous yttrium nitrate solution in the metal salt raw material storage tank 15 and the mixed dispersion solvent of the polyethylene glycol and the sodium hydroxide aqueous solution (the molar ratio of the polyethylene glycol to the sodium hydroxide aqueous solution is 1: 15) in the dispersing agent storage tank 10 into the hydrothermal reaction kettle 7 through the dissolved salt metering pump 4, the additive metering pump 12 and the metal salt metering pump 18 in sequence, adding the solutions in the dissolved salt raw material storage tank 1, the metal salt raw material storage tank 15 and the additive storage tank 10 into the hydrothermal reaction kettle 7 through the spiral nozzle (PP material) of the first atomizing nozzle 6, the pipe orifice of the second pipeline 14 and the third pipeline 17 according to the molar ratio of 15:1:2 to prepare mixed reaction slurry, adjusting the stirring linear velocity of the hydrothermal reaction kettle to 4., stirring for 15 minutes to mix thoroughly;
2. firstly, opening the regulating gate valve 20, the one-way stop valve 22 and the one-way stop valve 24, closing the one-way stop valve 27, the regulating gate valve 2, the one-way stop valve 5, the regulating gate valve 11, the one-way stop valve 13, the regulating gate valve 16 and the one-way stop valve 19, and then opening the displacement pump 21 to enable the mixed reaction slurry to form a uniformly mixed solution in the hydrothermal reaction kettle 7 through the spiral nozzle of the second atomizer 25;
3. opening an ultrasonic vibrator 28, controlling the ultrasonic frequency to be 40KHZ, closing the regulating gate valve 20 and the volumetric pump 21 after ultrasonic treatment is carried out for 30 minutes, taking out the first atomizing nozzle 6 and the second atomizing nozzle 25, closing the first seal 7a and the second seal 7b, and keeping the interior of the hydrothermal reaction kettle 7 sealed;
4. heating the hydrothermal reaction kettle 7, controlling the highest temperature to be 150 ℃, increasing the linear velocity of the stirring paddle to 8m/S, carrying out heat preservation reaction for 8h, and then cooling to 40 ℃;
5. opening the regulating gate valve 20 and the one-way stop valve 24 for sealing, closing the one-way stop valve 22, opening the one-way stop valve 27, starting the displacement pump 21, washing the reacted nano slurry solution by a ceramic membrane cleaning machine with the aperture of 5nm, and then carrying out cold air drying under the conditions of vacuum degree of-0.09-0.096 MPa and 20 ℃ to obtain the high-purity yttrium-stabilized zirconia nano powder material.
The barium titanate nanopowder and the titanium dioxide nanopowder prepared in examples 1 and 2 were subjected to surface morphology, particle size and crystal structure test analysis by using a field emission Scanning Electron Microscope (SEM). And (3) repeatedly testing each batch of samples, wherein each electron microscope image has at least 100 particles, and the average value of the particle morphology and size statistical results is taken. The prepared barium titanate nano powder material is of a cubic phase high-purity crystal structure, and the average electron microscope size particle size is 62.49 nm; the titanium dioxide nano powder material has an anatase type high-purity crystal structure, no other impurity peak and an average electron microscope size particle diameter of 28.42 nm; the yttrium-stabilized zirconia nano powder is of a semi-stable structure, and the average electron microscope size particle size is 20.15 nm.
In the present invention, "mounted", "connected", etc. should be understood in a broad sense. For example, the connection may be a fixed connection, a detachable connection, or an integral connection, a direct connection, an intermediate connection, or an external connection or an internal connection.
The above embodiments are merely illustrative of the specific embodiments of the present invention, and are not intended to limit the scope of the present invention, and those skilled in the art can make various modifications and changes based on the prior art, and without departing from the spirit of the present invention, various modifications and improvements made by the technical solutions of the present invention by those skilled in the art are all within the scope of the present invention defined by the claims.
Claims (3)
1. An apparatus for preparing high-purity nano material is characterized by comprising the following equipment: a dissolved salt raw material storage tank (1), an additive storage tank (10), a metal salt raw material storage tank (15), a hydrothermal reaction kettle (7), ultrasonic equipment (9), a ceramic membrane cleaning machine and a cold air drying machine;
the specific connection relationship is as follows:
a. the dissolved salt raw material storage tank (1) is connected with the interior of the hydrothermal reaction kettle (7) through a first pipeline (3); a dissolved salt metering pump (4) is arranged on the first pipeline (3), valves are respectively arranged on the pipelines at two sides of the dissolved salt metering pump (4), a first atomizing nozzle (6) is connected with the outlet of the first pipeline (3) in the hydrothermal reaction kettle (7), and the first atomizing nozzle (6) is mounted or dismounted through a first seal (7 a);
b. the additive storage tank (10) is connected with the interior of the hydrothermal reaction kettle (7) through a second pipeline (14); an additive metering pump (12) is arranged on the second pipeline (14), and valves are respectively arranged on the pipelines at two sides of the additive metering pump (12);
c. a metal salt raw material storage tank (15) is connected with the interior of the hydrothermal reaction kettle (7) through a third pipeline (17); a metal salt metering pump (18) is arranged on the third pipeline (17), and valves are respectively arranged on the pipelines at two sides of the metal salt metering pump (18);
d. an outlet at the bottom of the hydrothermal reaction kettle (7) is connected to an inlet at the top of the hydrothermal reaction kettle (7) through a fourth pipeline (23); a positive displacement pump (21) is installed on the fourth pipeline (23), one side of the positive displacement pump (21) close to the outlet at the bottom of the hydrothermal reaction kettle (7) is provided with a valve, one side of the positive displacement pump (21) close to the inlet at the top of the hydrothermal reaction kettle (7) is provided with two valves, the outlet of the fourth pipeline (23) in the hydrothermal reaction kettle (7) is connected with a second atomizing nozzle (25), and the second atomizing nozzle (25) is installed or detached through a second seal (7 b);
e. and a fifth pipeline (26) is connected between the displacement pump (21) and a valve adjacent to an outlet of the displacement pump, the fifth pipeline (26) is sequentially connected with the ceramic membrane cleaning machine and the cold air dryer through the valve, and the hydrothermal reaction kettle (7) is provided with ultrasonic equipment (9).
2. The apparatus for preparing high-purity nano-material according to claim 1, wherein: the inner linings of the salt dissolving raw material storage tank (1) and the metal salt raw material storage tank (15) are made of polyurethane and polytetrafluoroethylene, and the additive storage tank (10) is made of plastic or glass; the first pipeline (3) and the third pipeline (17) are made of any one of polytetrafluoroethylene, polypropylene and 316 stainless steel, the second pipeline (14) is made of polytetrafluoroethylene or polypropylene, and the fourth pipeline (23) is made of carbon steel with polytetrafluoroethylene as an inner lining and plastic outer lining; the fifth pipeline (26) is made of polypropylene or polyethylene; the first atomizing nozzle (6) and the second atomizing nozzle (25) are spiral nozzles and are made of alumina ceramics or polypropylene.
3. The apparatus for preparing high-purity nano-material according to claim 1, wherein: the ultrasonic equipment (9) comprises a sound insulation protective cover (8), an ultrasonic vibrator (28) and a PLC (programmable logic controller) thereof, wherein the sound insulation protective cover is made of foamed aluminum or centrifugal glass wool.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113979770A (en) * | 2021-12-01 | 2022-01-28 | 安徽中创电子信息材料有限公司 | Preparation method of enhanced yttrium-stabilized nano composite zirconia ceramic powder |
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2019
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113979770A (en) * | 2021-12-01 | 2022-01-28 | 安徽中创电子信息材料有限公司 | Preparation method of enhanced yttrium-stabilized nano composite zirconia ceramic powder |
| CN113979770B (en) * | 2021-12-01 | 2022-08-19 | 安徽凯盛应用材料有限公司 | Preparation method of enhanced yttrium-stabilized nano composite zirconia ceramic powder |
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Address after: 233000 28 yuan yuan Road, Huaihe Industrial Park, Huaishang District, Bengbu, Anhui Patentee after: Anhui Kaisheng Applied Materials Co.,Ltd. Patentee after: CHINA BUILDING MATERIALS BENGBU GLASS INDUSTRY DESIGN & RESEARCH INSTITUTE Co.,Ltd. Patentee after: ANHUI TAIGU NANO MATERIALS Co.,Ltd. Address before: 233000 28 yuan yuan Road, Huaihe Industrial Park, Huaishang District, Bengbu, Anhui Patentee before: ANHUI ZHONGCHUANG ELECTRONIC INFORMATION MATERIAL Co.,Ltd. Patentee before: CHINA BUILDING MATERIALS BENGBU GLASS INDUSTRY DESIGN & RESEARCH INSTITUTE Co.,Ltd. Patentee before: ANHUI TAIGU NANO MATERIALS Co.,Ltd. |
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Effective date of registration: 20230808 Address after: 233000 28 yuan yuan Road, Huaihe Industrial Park, Huaishang District, Bengbu, Anhui Patentee after: Anhui Kaisheng Applied Materials Co.,Ltd. Address before: 233000 room 1206, building C, Yongchang international building, No. 35 Mingzhu Road, Huaishang District, Bengbu City, Anhui Province Patentee before: ANHUI TAIGU NANO MATERIALS Co.,Ltd. |
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