Apparatus for producing nano-sized zirconium oxide

Abstract

The utility model belongs to zirconium oxide technical field, specifically relates to preparation device of nano zirconium oxide. Including sol preparation unit, ultrasonic dispersion unit, continuous hydrothermal reaction unit, solid - liquid separation unit and drying unit that pass through pipeline connection in proper order, realize material continuous flow between each unit through the delivery pump, sol preparation unit includes sol kettle, is equipped with raw material feed port on sol kettle, and is connected with solvent pipeline and pH regulator pipeline, ultrasonic dispersion unit includes ultrasonic dispersion jar, is equipped with ultrasonic transducer in ultrasonic dispersion jar inner wall, is equipped with deflector in jar, continuous hydrothermal reaction unit includes tubular reactor, solid - liquid separation unit includes centrifugal separator, drying unit includes vacuum drying box. Through adopting sol preparation - ultrasonic dispersion - continuous hydrothermal reaction integration design, can realize sol - gel reaction and hydrothermal reaction's continuous link, through ultrasonic dispersion reinforced mixing effect, has reduced the particle agglomeration, has promoted production efficiency and quality.

Description

Technical Field

[0001] This invention belongs to the field of zirconium oxide technology, specifically relating to an apparatus for preparing nano-zirconia. Background Technology

[0002] Nano-zirconia is a novel ceramic material with high hardness, high temperature resistance, good biocompatibility, and excellent chemical stability, widely used in structural ceramics, biomedical materials, catalyst supports, and other fields. Among existing nano-zirconia preparation processes, the sol-gel method is widely used due to its advantages of uniform particle size and high purity; however, this method is prone to problems such as sol agglomeration and incomplete reaction. The hydrothermal reaction method can optimize crystal form, but traditional equipment is mostly batch-based, making continuous production difficult. To balance product purity and crystal form quality, a combination of the sol-gel method and the hydrothermal reaction method has gradually become a common choice. However, existing related preparation equipment still has certain shortcomings: some equipment focuses on optimizing a single step, lacking continuous integration of sol preparation, dispersion, reaction, and post-processing, resulting in low production efficiency; the stirring dispersion method used in some equipment has limited effect on breaking up agglomerates in the sol system, making it difficult to guarantee the uniformity of product particle size. Therefore, there is an urgent need for a preparation device with a simple structure, capable of continuous production, and able to effectively solve the problem of particle agglomeration. Utility Model Content

[0003] In view of the shortcomings of the prior art, the purpose of this utility model is to provide a device for preparing nano-zirconia. By adopting an integrated design of sol preparation-ultrasonic dispersion-continuous hydrothermal reaction, the sol-gel reaction and hydrothermal reaction can be continuously connected. Ultrasonic dispersion enhances the mixing effect, reduces particle agglomeration, and improves production efficiency and quality.

[0004] This utility model is achieved using the following technical solution: The nano-zirconia preparation apparatus includes a sol preparation unit, an ultrasonic dispersion unit, a continuous hydrothermal reaction unit, a solid-liquid separation unit, and a drying unit connected in sequence by pipelines. The material is continuously transferred between the units by a transfer pump. The sol preparation unit includes a sol kettle, which is equipped with a raw material inlet and connected to a solvent pipeline and a pH adjuster pipeline. The kettle is equipped with a stirring device inside and a constant temperature jacket on the outside of the kettle wall. The ultrasonic dispersion unit includes an ultrasonic dispersion tank. The inlet of the ultrasonic dispersion tank is connected to the outlet of the sol-gel kettle through a pipe. A first delivery pump is installed on the pipe. Multiple ultrasonic transducers are installed on the inner wall of the ultrasonic dispersion tank. A guide plate is installed inside the tank. The continuous hydrothermal reaction unit includes a tubular reactor. The feed inlet of the tubular reactor is connected to the discharge outlet of the ultrasonic dispersion tank via a pipeline. A second delivery pump is installed on the pipeline. A heating device is installed on the outside of the tubular reactor, and a temperature sensor and a pressure sensor are connected inside. The solid-liquid separation unit includes a centrifugal separator, the inlet of which is connected to the outlet of the tubular reactor via a pipe. The drying unit includes a vacuum drying chamber, the inlet of which is connected to the solid outlet of a centrifugal separator.

[0005] The stirring device of the sol-gel reactor is a spiral stirring paddle; the constant temperature jacket is a water bath jacket connected to a temperature controller to control the sol-gel reaction temperature.

[0006] The ultrasonic transducers of the ultrasonic dispersion tank are evenly distributed on the inner wall, numbering 3-4, and connected to the ultrasonic generator; the guide plate is arranged in a spiral shape; the bottom of the ultrasonic dispersion tank is equipped with an anti-settling stirring paddle to prevent material from settling at the bottom of the tank.

[0007] The heating device for the tubular reactor is an electric heating jacket, which is connected to a temperature control system.

[0008] The tubular reactor is equipped with a static mixer at the feed inlet, and the static mixer is connected to an additive pipeline for mixing the ultrasonically dispersed sol with the additive.

[0009] The centrifuge's liquid outlet is connected to a solvent recovery tank.

[0010] The vacuum drying oven is equipped with a material tray and a hot air circulation pipe.

[0011] The working principle of the aforementioned nano-zirconia preparation device is as follows: During operation, zirconium-based raw materials, solvent, and pH adjuster are first added through the raw material inlet, solvent line, and pH adjuster line on the sol-gel reactor, respectively. Under the stirring action of the spiral impeller and the constant temperature control of the water bath jacket, the mixture reacts to generate a uniform sol. Subsequently, the sol is transported to the ultrasonic dispersion tank by the first transfer pump. The ultrasonic vibration generated by the ultrasonic transducer disperses the sol, the spiral guide plate prolongs the material residence time, and the anti-settling impeller at the bottom prevents material deposition, further improving the dispersion effect. The dispersed sol is then transported to the tubular reactor by the second transfer pump. During this process, the static mixer adds stabilizers and other additives through the additive line and mixes them thoroughly with the sol. Under the temperature control of the electric heating jacket and the monitoring of temperature and pressure sensors, the tubular reactor provides a stable hydrothermal reaction environment for the material, completing the crystal form optimization. The reacted material enters the centrifuge to achieve solid-liquid separation. The separated liquid is recycled through the solvent recovery tank, while the solid particles enter the vacuum drying oven and are dried on the material tray by the action of the hot air circulation pipe, finally obtaining the finished nano-zirconia product.

[0012] Compared with the prior art, the beneficial effects of this utility model are as follows: The nano-zirconia preparation device of this utility model achieves integrated continuous production of nano-zirconia from raw material mixing to finished product drying by sequentially connecting the sol preparation unit, ultrasonic dispersion unit, continuous hydrothermal reaction unit, solid-liquid separation unit and drying unit and using a delivery pump to achieve continuous flow. This effectively improves production efficiency. At the same time, the ultrasonic dispersion unit, together with the spiral guide plate and anti-deposition stirring paddle, can specifically improve the problem of sol agglomeration in traditional devices, which helps to ensure the uniformity of nano-zirconia product particle size and solves the shortcomings of poor dispersion effect in the prior art. Moreover, the overall device has a simple structure, is easy to operate and has strong practicality. Attached Figure Description

[0013] Figure 1 This is a schematic diagram of the structure of the nano-zirconia preparation device of this utility model; In the diagram: 1. Solvent vessel; 2. Raw material inlet; 3. Solvent line; 4. pH adjuster line; 5. Spiral agitator; 6. Water bath jacket; 7. Ultrasonic dispersion tank; 8. First transfer pump; 9. Ultrasonic transducer; 10. Baffle plate; 11. Anti-settling agitator; 12. Tubular reactor; 13. Second transfer pump; 14. Electric heating jacket; 15. Temperature sensor; 16. Pressure sensor; 17. Centrifuge; 18. Solvent recovery tank; 19. Vacuum drying oven; 20. Material tray; 21. Hot air circulation pipe; 22. Static mixer; 23. Additive line. Detailed Implementation

[0014] To make the objectives and technical solutions of this utility model clearer, the present utility model will be further described in detail below with reference to the accompanying drawings.

[0015] Example 1 like Figure 1 As shown, the nano-zirconia preparation device includes a sol preparation unit, an ultrasonic dispersion unit, a continuous hydrothermal reaction unit, a solid-liquid separation unit, and a drying unit connected in sequence by pipelines. The material is continuously transferred between each unit by a transfer pump. The sol preparation unit includes a sol tank 1, which is equipped with a raw material inlet 2 and connected to a solvent pipeline 3 and a pH adjuster pipeline 4. The tank is equipped with a stirring device and a constant temperature jacket on the outside of the tank wall. The ultrasonic dispersion unit includes an ultrasonic dispersion tank 7. The inlet of the ultrasonic dispersion tank 7 is connected to the outlet of the sol-gel kettle 1 through a pipe. A first delivery pump 8 is provided on the pipe. Multiple ultrasonic transducers 9 are provided on the inner wall of the ultrasonic dispersion tank 7. A guide plate 10 is provided inside the tank. The continuous hydrothermal reaction unit includes a tubular reactor 12. The inlet of the tubular reactor 12 is connected to the outlet of the ultrasonic dispersion tank 7 through a pipe. A second delivery pump 13 is provided on the pipe. A heating device is provided on the outside of the tubular reactor 12, and a temperature sensor 15 and a pressure sensor 16 are connected inside. The solid-liquid separation unit includes a centrifuge 17, the inlet of which is connected to the outlet of the tubular reactor 12 via a pipe. The drying unit includes a vacuum drying chamber 19, the inlet of which is connected to the solid outlet of the centrifugal separator 17.

[0016] The stirring device of the sol-gel kettle 1 is a spiral stirring paddle 5; the constant temperature jacket is a water bath jacket 6, which is connected to a temperature controller.

[0017] The ultrasonic transducers 9 of the ultrasonic dispersion tank 7 are evenly distributed on the inner wall, with a quantity of 4, and are connected to the ultrasonic generator; the guide plate 10 is arranged in a spiral shape; and the bottom of the ultrasonic dispersion tank 7 is provided with an anti-deposition stirring paddle 11.

[0018] The heating device for the tubular reactor 12 is an electric heating jacket 14, which is connected to a temperature control system.

[0019] The tubular reactor 12 is equipped with a static mixer 22 at the feed inlet, and an auxiliary agent pipeline 23 is connected to the static mixer 22.

[0020] The liquid outlet of the centrifuge 17 is connected to a solvent recovery tank 18.

[0021] The vacuum drying oven 19 is equipped with a material tray 20 and a hot air circulation pipe 21.

[0022] The specific process during work is as follows: Zirconium isopropoxide was used as the raw material and anhydrous ethanol as the solvent. The mixture was added to a sol-gel reactor 1 in a specific ratio, and dilute nitric acid was added to adjust the pH to 3.5. The mixture was reacted for 60 minutes at a stirring speed of 80 r / min and a constant temperature of 45℃ to generate a sol. The sol was then pumped into an ultrasonic dispersion tank 7 via a first transfer pump 8 and dispersed under 40 kHz ultrasound for 30 minutes. The dispersed sol was then pumped into a tubular reactor 12 via a second transfer pump 13. Simultaneously, a 5% yttrium oxide solution was introduced into a static mixer 22 through an auxiliary agent line 23. After mixing with the sol, the solution entered the tubular reactor 12 and reacted for 1.5 hours at 160℃ and 0.8 MPa. The reacted material was then separated in a centrifuge 17. The recovered ethanol solvent could be recycled for sol preparation. The separated solid particles were dried in a vacuum drying oven 19 for 2 hours, ultimately yielding a nano-zirconium oxide product with uniform particle size and good dispersibility.

Claims

1. An apparatus for preparing nano-zirconia, characterized in that, It includes a sol preparation unit, an ultrasonic dispersion unit, a continuous hydrothermal reaction unit, a solid-liquid separation unit, and a drying unit connected in sequence by pipelines. The continuous flow of materials between the units is achieved by a transfer pump. The sol preparation unit includes a sol tank (1), which is provided with a raw material inlet (2) and connected to a solvent pipeline (3) and a pH adjuster pipeline (4). The tank is equipped with a stirring device and a constant temperature jacket is provided on the outside of the tank wall. The ultrasonic dispersion unit includes an ultrasonic dispersion tank (7), the inlet of which is connected to the outlet of the sol-gel kettle (1) via a pipe, a first delivery pump (8) is provided on the pipe, a plurality of ultrasonic transducers (9) are provided on the inner wall of the ultrasonic dispersion tank (7), and a guide plate (10) is provided inside the tank. The continuous hydrothermal reaction unit includes a tubular reactor (12). The feed inlet of the tubular reactor (12) is connected to the discharge outlet of the ultrasonic dispersion tank (7) through a pipe. A second delivery pump (13) is provided on the pipe. A heating device is provided on the outside of the tubular reactor (12), and a temperature sensor (15) and a pressure sensor (16) are connected inside. The solid-liquid separation unit includes a centrifuge (17), the inlet of which is connected to the outlet of the tubular reactor (12) via a pipe. The drying unit includes a vacuum drying chamber (19), the inlet of which is connected to the solid outlet of a centrifugal separator (17).

2. The apparatus for preparing nano-zirconia according to claim 1, characterized in that, The stirring device of the sol-gel kettle (1) is a spiral stirring paddle (5); the constant temperature jacket is a water bath jacket (6) connected to a temperature controller.

3. The apparatus for preparing nano-zirconia according to claim 1, characterized in that, The ultrasonic transducers (9) of the ultrasonic dispersion tank (7) are evenly distributed on the inner wall, with a quantity of 3-4, and are connected to the ultrasonic generator; the guide plate (10) is arranged in a spiral shape; the bottom of the ultrasonic dispersion tank (7) is provided with an anti-deposition stirring paddle (11).

4. The apparatus for preparing nano-zirconia according to claim 1, characterized in that, The heating device for the tubular reactor (12) is an electric heating jacket (14), which is connected to a temperature control system.

5. The apparatus for preparing nano-zirconia according to claim 1, characterized in that, The tubular reactor (12) is equipped with a static mixer (22) at the feed inlet, and an auxiliary agent pipeline (23) is connected to the static mixer (22).

6. The apparatus for preparing nano-zirconia according to claim 1, characterized in that, The liquid outlet of the centrifuge (17) is connected to a solvent recovery tank (18).

7. The apparatus for preparing nano-zirconia according to claim 1, characterized in that, The vacuum drying oven (19) is equipped with a material tray (20) and a hot air circulation pipe (21).

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