Device and method for purifying and preparing nano zirconium oxide powder

Abstract

The invention relates to a purification preparation device and method of nano zirconium oxide powder, and relates to the technical field of zirconium oxide powder preparation. Comprising a reaction cylinder, a feeding port and a discharging port are formed in the upper end and the lower end of the reaction cylinder, a preparation box is installed above the reaction cylinder, the interior of the preparation box is divided into an acid liquor chamber, an alkali liquor chamber and a water storage chamber through partition plates, and the water storage chamber is located between the acid liquor chamber and the alkali liquor chamber. The problems that in the prior art, in the zirconium oxide powder preparation process, an independent working chamber needs to be used in each treatment link, then unified treatment is carried out, and therefore remarkable capital investment is needed for building and maintaining a plurality of independent working chambers; the method comprises the steps of equipment purchasing, facility building and subsequent operation and maintenance cost; the mechanical action generated by stirring blades during high-speed rotation causes microdefects on the surfaces of zirconia particles, and the surface defects may affect the optical properties and chemical activity of materials or the mechanical properties of final products.

Description

Technical Field

[0001] The invention relates to the technical field of zirconium oxide powder preparation, and in particular to a device and method for purifying and preparing nano zirconium oxide powder. Background Art

[0002] Zirconia, also known as zirconium dioxide, is the main oxide of zirconium. It is usually white, odorless and tasteless crystals and is difficult to dissolve in water, hydrochloric acid and dilute sulfuric acid. It is chemically inactive and has the properties of high melting point, high resistivity, high refractive index and low thermal expansion coefficient, making it an important high temperature resistant material, ceramic insulation material and ceramic sunscreen, and also the main raw material for artificial diamonds.

[0003] When preparing nano-zirconia powder, factors that need to be considered include raw material selection, reaction conditions, impurity analysis, environmental safety, and equipment selection. Acidification and alkalization to remove impurities and purification technology is a common method for preparing high-purity nano-zirconia powder. Impurities in the raw materials are removed by acidification and alkalization, and high-purity nano-zirconia powder is obtained through washing and drying steps.

[0004] For example, Chinese patent publication number CN117509726A discloses an automated purification device for zirconium oxide; The invention relates to the technical field of zirconium oxide purification, and comprises a base, wherein two fixing rods are fixedly connected to the top of the base, and the opposite sides of the two fixing rods are fixedly connected to the same processing chamber, and a feed hole is opened on the outer side of the processing chamber located at the top. The automatic purification device of zirconium oxide has a process in which a heating component raises the temperature inside the processing chamber during the introduction of hydrogen, and a second driving motor is started, and the second driving motor drives each rotating plate to turn and drive the solid inside the purification frame. When the rotating plate rotates from the bottom to the top, the forward and reverse motors are started to drive the contact arc rod on the deflection plate to separate from the rotating plate, and the rotating plate deflects under the action of the solid gravity, and the solid above the rotating plate gradually pours downward, so that the hydrogen is fully in contact with the fixed part, so as to avoid the effect of incomplete reduction of some impurities caused by incomplete contact of the introduction of hydrogen.

[0005] However, the above hydrolysis device for zirconium oxide powder production has some shortcomings in actual use: 1. The above-mentioned device can avoid the effect of incomplete reduction of some impurities due to incomplete contact of hydrogen introduction, thereby improving the efficiency of automatic purification of zirconium oxide. However, each processing link requires the use of an independent working chamber and then unified processing, which will result in significant capital investment in the establishment and maintenance of multiple independent working chambers, including the purchase of equipment, construction of facilities, and subsequent operation and maintenance costs.

[0006] 2. The above device drives each rotating plate to flip the solid inside the purification frame through the driving motor 2. However, the mechanical action generated by the stirring blades when rotating at high speed may also cause microscopic defects on the surface of the zirconium oxide particles. These surface defects may affect the optical properties, chemical activity or mechanical properties of the final product.

[0007] Therefore, based on the above-stated viewpoints, there is still room for improvement in the existing hydrolysis equipment for zirconium oxide powder production. Summary of the invention

[0008] In order to solve the above problems, the present invention provides a device and method for purifying and preparing nano zirconium oxide powder.

[0009] On the one hand, a device for purifying and preparing nano zirconium oxide powder comprises a reaction cylinder, wherein a feed port and a discharge port are provided at the upper and lower ends of the reaction cylinder, a preparation box is installed above the reaction cylinder, and the interior of the preparation box is divided into an acid liquid chamber, an alkali liquid chamber and a water storage chamber by a partition, and the water storage chamber is located between the acid liquid chamber and the alkali liquid chamber.

[0010] The reaction tube is provided with a mixing mechanism for mixing zirconium oxide powder with a reactant, the mixing mechanism includes an air outlet pipe, the air outlet pipe is rotatably arranged inside the reaction tube, a working bucket connected to the air outlet pipe is arranged at the lower end of the preparation box, an acid conduit is coaxially arranged inside the air outlet pipe, an alkali conduit is arranged inside the acid conduit, a water supply pipe connected to a water storage chamber is installed inside the alkali conduit, a nozzle connected to the water supply pipe is arranged at one end of the water supply pipe away from the preparation box, and a through pipe penetrating to the outer wall of the air outlet pipe is arranged on the acid conduit and the alkali conduit.

[0011] Preferably, an air pump is installed on the reaction cylinder, the air pump is connected to the working bucket, and a plurality of air holes connected to the inside of the air outlet pipe are opened on the air outlet pipe.

[0012] Preferably, connecting pipes respectively connected to the acid solution chamber and the alkali solution chamber are installed inside the working bucket, and the two connecting pipes are respectively connected to the acid solution conduit and the alkali solution conduit through control components.

[0013] Preferably, a booster plate is installed inside the reaction cylinder, which is sleeved on the outside of the air outlet pipe and slidably arranged inside the reaction cylinder. A supporting plate is arranged at the lower end of the reaction cylinder, and a separation hole is opened on the supporting plate. A control plate is installed below the supporting plate, and a water outlet matching the water outlet is opened on the control plate.

[0014] Preferably, the reaction cylinder is provided with a control component for driving the acid liquid conduit and the alkali liquid conduit to discharge materials in an offset manner, the control component includes a control gear, a transverse groove is provided in the middle of the working bucket, the control gear is rotatably arranged in the transverse groove, and a connecting port 1 and a connecting port 2 are provided on the control gear, and the connecting port 1 and the connecting port 2 are movably cooperated with the acid liquid conduit and the alkali liquid conduit respectively.

[0015] Preferably, a control shaft is rotatably mounted on the reaction tube, a driving gear meshing with the control gear is mounted on one end of the control shaft located in the reaction tube, a spiral groove is provided on an outer wall of a section of the control shaft located in the reaction tube, a through hole slidably matched with the control shaft is provided on the booster plate, and a protrusion sliding in the spiral groove is provided in the through hole.

[0016] Preferably, a matching component is provided in the reaction cylinder to drive the supporting plate and the control plate to cooperate in discharging water, and the matching component includes a matching gear, and the matching gear is arranged at one end of the control shaft located in the reaction cylinder, and an arc-shaped matching groove is opened on the control plate, and a matching rack meshing with the matching gear is connected in the matching groove.

[0017] Preferably, a pushing member for driving the air outlet pipe to rotate is also installed on the reaction cylinder, and the pushing member includes a pushing sleeve, and the pushing sleeve is rotatably installed on the reaction cylinder and penetrates the reaction cylinder, the air outlet pipe and the pushing sleeve are connected by a belt drive, a motor is arranged above the reaction cylinder through a motor seat, and the pushing sleeve is connected to the motor output shaft through a ratchet member.

[0018] Preferably, the reaction tube is also provided with a lifting member for driving the booster plate to rise and fall, the lifting member includes a connecting shaft, the connecting shaft is rotatably mounted inside the reaction tube and is coaxially arranged with the pushing sleeve, and the connecting shaft is connected to the motor output shaft through a second ratchet member.

[0019] On the other hand, a method for purifying and preparing nano zirconium oxide powder is provided. The method for purifying and preparing nano zirconium oxide powder is as follows: S1. Powder placement: placing zirconium oxide powder into the reaction tube from the feed port, and then transporting the acid solution in the acid chamber into the reaction tube; S2, impurity dissolution: blow cold air into the reaction tube, then turn on the motor, the air outlet pipe rotates, and the zirconium oxide powder and the acid solution are stirred with the cooperation of the air outlet pipe and the air pump to drive the two to be fully mixed, and then wait for some impurities in the zirconium oxide powder to dissolve in the acid solution; S3, impurity separation: After the impurities react with the dissolved acid solution, the booster plate is driven down, the water outlet and the separation hole overlap on the booster plate, and the booster plate is further lowered to apply pressure to the inside of the reaction tube, and the acid solution inside the reaction tube flows out from the water outlet with the dissolved impurities; S4, powder washing: the booster plate rises again, and the separated zirconium oxide powder is washed by using the water supply pipe and the nozzle until the acidity and alkalinity of the zirconium oxide powder is neutral, and the booster plate descends again to remove the moisture in the zirconium oxide powder; S5. Impurity separation: After removing the water, add the alkaline solution again, and then repeat the above steps to remove another part of the impurities in the zirconium oxide powder by the acidic solution.

[0020] In summary, the present application includes at least one of the following beneficial technical effects: 1. The present invention sets an air outlet pipe in the reaction tube, uses an air pump to blow cold air and hot air into the reaction tube through the air outlet pipe, and when the zirconium oxide powder is mixed with the acidic solution and the alkaline solution, the air outlet pipe rotates, and the air output by the air pump can stir the mixed liquid, so that the acidification reaction and the alkalization reaction of the reaction tube are more complete, thereby improving the efficiency of purifying the zirconium oxide powder.

[0021] 2. The present invention arranges an acid conduit and an alkali conduit in the air outlet pipe, so that when the zirconium oxide powder in the reaction tube is treated, acidification treatment and alkalization treatment can be completed in the same reaction tube. This arrangement can reduce the transfer and waiting time of materials between different equipment, improve the overall operating efficiency, and better control the reaction conditions, such as temperature, concentration and reaction time, thereby improving the consistency of product quality. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] The present invention is further described below in conjunction with the accompanying drawings and embodiments.

[0023] Figure 1 It is a schematic diagram of the overall structure of the present invention.

[0024] Figure 2 It is a cross-sectional structural schematic diagram of the present invention.

[0025] Figure 3 It is a partial structural schematic diagram of the present invention.

[0026] Figure 4 It is a schematic diagram of the structure inside the air outlet pipe of the present invention.

[0027] Figure 5 It is a schematic diagram of the structure inside the reaction tube of the present invention.

[0028] Figure 6 The present invention Figure 5 Schematic diagram of the structure at A in the middle.

[0029] Figure 7 It is a schematic structural diagram of the matching part of the present invention.

[0030] Figure 8It is a schematic diagram of the position structure of the pusher of the present invention.

[0031] Fig. 9 It is a schematic diagram of the structure inside the push sleeve of the present invention.

[0032] In the figure, 1, reaction cylinder; 10, feed port; 11, discharge port; 12, preparation box; 13, acid chamber; 14, alkali chamber; 15, water storage chamber; 16, through pipe; 17, air hole; 2, mixing mechanism; 20, air outlet pipe; 21, working bucket; 22, acid conduit; 23, alkali conduit; 24, water supply pipe; 25, nozzle; 30, booster plate; 31, bearing plate; 32, separation hole; 33, control board; 34, water outlet; 4, control member; 40, control gear; 41, connecting rod Through port one; 42, connecting port two; 43, control shaft; 44, driving gear; 5, matching piece; 50, matching gear; 51, matching groove; 52, matching rack; 6, pushing piece; 60, pushing sleeve; 61, motor; 62, ratchet piece one; 620, ratchet ring; 621, ratchet tooth one; 7, lifting piece; 70, connecting shaft; 71, ratchet piece two; 710, driving plate; 711, ratchet; 712, ratchet tooth two; 80, supporting plate; 8, discharging mechanism; 81, pull ring; 82, push ring. DETAILED DESCRIPTION

[0033] The following is combined with Figure 1-Figure 9 While embodiments of the invention have been described in detail, the invention can be implemented in many different ways as defined and covered by the claims.

[0034] The embodiment of the present application discloses a device and method for purifying and preparing nano zirconium oxide powder. It is explained that the present application is mainly used in the process of preparing zirconium oxide powder. In terms of technical effect, it can avoid the need for different devices to purify the zirconium oxide powder by acid treatment and practice treatment, which leads to long production time and low efficiency; further, it can also solve the problem of damage to the zirconium oxide powder caused by stirring and filtering mechanical devices during the purification process of the zirconium oxide powder in the prior art.

[0035] Embodiment 1: Reference Figure 1 and Figure 2 As shown, a purification and preparation device for nano zirconium oxide powder includes a reaction tube 1, wherein a feed port 10 and a discharge port 11 are provided at the upper and lower ends of the reaction tube 1, a preparation box 12 is installed above the reaction tube 1, and the interior of the preparation box 12 is divided into an acid liquid chamber 13, an alkali liquid chamber 14 and a water storage chamber 15 by a partition, and the water storage chamber 15 is located between the acid liquid chamber 13 and the alkali liquid chamber 14.

[0036] Zirconia powder enters the reaction tube 1 through the feed port 10, and then the acidic solution in the acid solution chamber 13 enters the reaction tube 1 to react with the zirconium oxide powder. Since the zirconium oxide powder does not react with the acidic solution, a part of the impurities in the zirconium oxide powder will dissolve in the acidic solution. The acidic solution is then filtered, and then the alkaline solution in the alkaline solution chamber 14 is added. Since the zirconium oxide powder does not react with the alkaline solution either, another part of the impurities in the zirconium oxide powder will dissolve in the alkaline solution. The alkaline solution is then filtered. The purity of the zirconium oxide powder after the acidic and alkaline treatments is improved.

[0037] The reaction tube 1 is provided with a mixing mechanism 2 for mixing zirconium oxide powder with a reactant, the mixing mechanism 2 includes an air outlet pipe 20, the air outlet pipe 20 is rotatably arranged inside the reaction tube 1, a working bucket 21 connected to the air outlet pipe 20 is arranged at the lower end of the preparation box 12, an acid conduit 22 is coaxially arranged inside the air outlet pipe 20, an alkali conduit 23 is arranged inside the acid conduit 22, a water supply pipe 24 connected to the water storage chamber 15 is installed inside the alkali conduit 23, a nozzle 25 connected to the water supply pipe 24 away from the preparation box 12 is arranged at one end thereof, and is used for washing the zirconium oxide powder after acid treatment and alkaline treatment, the acid conduit 22 and the alkali conduit 23 are both provided with a through pipe 16 penetrating to the outer wall of the air outlet pipe 20, and the acidic liquid and the alkaline liquid are sprayed into the reaction tube 1 through the through pipe 16.

[0038] The working bucket 21 is internally provided with connecting pipes which are respectively connected with the acid liquid chamber 13 and the alkali liquid chamber 14. The connecting pipes are both provided with electronic valves (not shown in the figure). The two electronic valves are operated alternately according to specific needs. The two connecting pipes are respectively connected with the acid liquid conduit 22 and the alkali liquid conduit 23 through the control component 4. The control component 4 makes the acid liquid conduit 22 and the alkali liquid conduit 23 connected with the corresponding connecting pipes in a staggered arrangement. Then, when the acid liquid conduit 22 is connected with its corresponding connecting pipe, the alkali liquid conduit 23 at this time will not be connected with the connecting pipe under the control of the control component 4. On the contrary, when the alkali liquid conduit 23 is working, the acid liquid conduit 22 is not working, so that the acid treatment and the alkaline treatment can be carried out in the same chamber without transferring the zirconium oxide powder, thereby reducing the working time and improving the treatment efficiency.

[0039] Reference Figure 2 and Figure 3 As shown, it is a schematic diagram of the structure of adding air into the reaction tube 1; specifically, an air pump is installed on the reaction tube 1, the air pump is connected to the working bucket 21, and a plurality of air holes 17 connected to the inside of the air outlet pipe 20 are opened on the air outlet pipe 20.

[0040] Among them, the air pump can not only blow cold air, but also blow hot air. In this way, after the acid solution and the alkaline solution are added to the reaction cylinder 1, when the air outlet pipe 20 rotates, the air outlet pipe 20 blows cold air, which can stir the liquid and promote the zirconium oxide powder to be fully mixed with the acid solution and the alkaline solution. Conventional mechanical stirring method is not used, thereby avoiding the possible damage to the zirconium oxide powder caused by mechanical stirring.

[0041] After the acid treatment and the alkaline treatment are completed, the filtered zirconium oxide powder needs to be dried. At this time, the air pump blows hot air into the air outlet pipe to dry the zirconium oxide powder through hot air circulation. Thus, the air outlet pipe 20 can achieve the dual effects of stirring and drying, further improving the efficiency of zirconium oxide powder purification.

[0042] Reference Figure 2 , Figure 3 and Figure 5 As shown, it is a schematic diagram of the structure for filtering the zirconium oxide powder after acid-base treatment; specifically, a booster plate 30 is installed inside the reaction tube 1, which is sleeved on the outside of the air outlet pipe 20 and slidably arranged inside the reaction tube 1. The air pressure in the reaction tube 1 is increased by descending the booster plate 30. A supporting plate 31 is arranged at the lower end of the reaction tube 1. A separation hole 32 is provided on the supporting plate 31. A filter membrane is installed in the separation hole 32 to filter the zirconium oxide powder. A control board 33 is installed below the supporting board 31. A water outlet 34 is provided on the control board 33 to match the water outlet 34. When the separation hole 32 coincides with the water outlet 34, the acidic solution and the alkaline solution mixed with impurities in the reaction tube 1 will be squeezed out through the water outlet 34 under the drive of the booster plate 30, thereby filtering the zirconium oxide powder. At the same time, when the zirconium oxide powder is cleaned, the zirconium oxide powder and the water can also be separated by the booster plate 30.

[0043] Reference Figure 5 and Figure 6 As shown, it is a schematic diagram of the structure that drives the acid liquid conduit 22 and the alkali liquid conduit 23 to discharge materials in a dislocated manner; specifically, the control member 4 includes a control gear 40, a transverse groove is opened in the middle of the working bucket 21, the control gear 40 is rotatably set in the transverse groove, and a connecting port 1 41 and a connecting port 2 42 are opened on the control gear 40, and the connecting port 1 41 and the connecting port 2 42 are movably cooperated with the acid liquid conduit 22 and the alkali liquid conduit 23 respectively.

[0044] The connecting port 1 41 corresponds to the acid conduit 22 and the connecting pipe corresponding to the acid conduit 22, and the connecting port 2 42 corresponds to the alkali conduit 23 and the connecting pipe corresponding to the alkali conduit 23. It should be noted that the angle between the acid conduit 22 and the alkali conduit 23 is 180 degrees, and the angle between the connecting port 1 41 and the connecting port 2 42 is an obtuse angle less than 180 degrees. This results in that when the control gear 40 rotates so that the connecting port 1 41 is connected to the acid conduit 22, the connecting port 2 42 will not be connected to the alkali conduit 23. At this time, only the acidic solution will enter the reaction cylinder 1, otherwise only the alkaline solution will enter. In this way, the acidic solution and the alkaline solution can be alternately placed in the reaction cylinder 1 to perform different purification operations.

[0045] Reference Figure 4 As shown, it is a schematic diagram of the structure that drives the control gear 40 to rotate; specifically, a control shaft 43 is rotatably installed on the reaction tube 1, and a driving gear 44 meshing with the control gear 40 is installed on one end of the control shaft 43 located outside the reaction tube 1, and a spiral groove is provided on an outer wall of a section of the control shaft 43 located inside the reaction tube 1, and a through hole that slides with the control shaft 43 is provided on the booster plate 30, and a protrusion that slides in the spiral groove is provided in the through hole.

[0046] When the boost plate 30 descends in the reaction tube 1, the protrusion in the perforation will slide in the spiral groove, and the protrusion can only move up and down, which will drive the control shaft 43 to rotate, and then the driving gear 44 on the control shaft 43 will rotate, and the driving gear 44 will drive the control gear 40 to rotate until the connecting port 1 41 on the control gear 40 coincides with the acid conduit 22. When the boost plate 30 rises in the reaction tube 1, the connecting port 2 42 on the control gear 40 coincides with the alkaline conduit 23, thereby realizing the control gear 40 regulating the release of the acidic solution and the alkaline solution.

[0047] Reference Figure 5 and Figure 7 As shown, it is a schematic diagram of the structure for driving the control plate 33 to rotate; specifically, a matching piece 5 for driving the supporting plate 31 and the control plate 33 to cooperate in water discharge is arranged in the reaction tube 1, and the matching piece 5 includes a matching gear 50, and the matching gear 50 is arranged at one end of the control shaft 43 located in the reaction tube 1, and an arc-shaped matching groove 51 is opened on the control plate 33, and a matching rack 52 meshing with the matching gear 50 is connected in the matching groove 51. The control shaft 43 rotates to drive the matching gear 50 to rotate, and then the control plate 33 is driven to rotate under the cooperation of the matching gear 50 and the matching rack 52, until the water outlet 34 on the control plate 33 coincides with the separation hole 32 on the supporting plate 31.

[0048] During the specific implementation process, the boost plate 30 descends, and the protrusion on the boost plate 30 cooperates with the spiral groove on the control shaft 43, driving the control shaft 43 to rotate, and then driving the matching gear 50 on the control shaft 43 to rotate, and the matching gear 50 rotates in the matching groove 51 along the matching groove 51, driving the control plate 33 to rotate in the reverse direction.

[0049] Reference Figure 6 and Fig. 9 As shown, that is, a schematic diagram of the structure of driving the air outlet pipe 20 to rotate so that the air discharged from the air outlet pipe 20 stirs the liquid in the reaction tube 1; specifically, the reaction tube 1 is also equipped with a driving member 6 for driving the air outlet pipe 20 to rotate, the driving member 6 includes a driving sleeve 60, the driving sleeve 60 is rotatably installed on the reaction tube 1 and penetrates the reaction tube 1, the air outlet pipe 20 is connected to the driving sleeve 60 through a belt drive, a motor 61 is arranged above the reaction tube 1 through a motor seat, and the driving sleeve 60 is connected to the output shaft of the motor 61 through a ratchet member 62.

[0050] When the motor 61 rotates clockwise, the ratchet wheel 62 drives the push sleeve 60 to rotate, and then the air outlet pipe 20 connected to the push sleeve 60 through the belt drive rotates. During the air outlet process, the rotation of the air outlet pipe 20 can stir the liquid in the reaction tank and drive the reaction to be more complete.

[0051] The ratchet component 62 includes a ratchet ring 620, which is installed inside one end of the push sleeve 60 located in the reaction tube 1. A ratchet 621 that cooperates with the ratchet ring 620 is installed on the output shaft of the motor 61 through a torsion spring. When the output shaft of the motor 61 rotates clockwise, the ratchet 621 can cooperate with the ratchet ring 620 to drive the push sleeve 60 to rotate, thereby driving the air outlet pipe 20 to rotate. Otherwise, the air outlet pipe 20 will not be driven to rotate.

[0052] Reference Figure 6 and Fig. 9 As shown, it is a schematic diagram of the structure for driving the boost plate 30 to move inside the reaction tube 1; specifically, the reaction tube 1 is also provided with a lifting member 7 for driving the boost plate 30 to rise and fall, and the lifting member 7 includes a connecting shaft 70, which is rotatably mounted inside the reaction tube 1 and coaxially arranged with the pushing sleeve 60, and the connecting shaft 70 is connected to the output shaft of the motor 61 through a ratchet member 71, and a reciprocating spiral groove is provided on the connecting shaft 70, and a thread groove matching the thread on the connecting shaft 70 is provided on the boost plate 30.

[0053] When the connecting shaft 70 rotates, the pressurizing plate 30 threadedly connected to the connecting shaft 70 will rise and fall in the reaction tube 1 , so that the pressurizing plate 30 pressurizes the interior of the reaction tube 1 .

[0054] The ratchet component 71 includes a drive plate 710, which is arranged on the output shaft of the motor 61. A drive groove is opened in the drive plate 710. A ratchet 711 is installed on the connecting shaft 70. A ratchet 712 that cooperates with the ratchet 711 is installed in the drive groove through a torsion spring. When the output shaft of the motor 61 rotates clockwise, the ratchet 712 will not drive the ratchet 711 to rotate, and when the output shaft of the motor 61 rotates counterclockwise, the ratchet 712 will drive the ratchet 711 to rotate, thereby driving the boost plate 30 to rise and fall.

[0055] Embodiment 2: On the basis of the first embodiment, in order to further improve the applicability of the present invention, a discharging mechanism 8 is also proposed, which is conducive to conveying the zirconium oxide powder out of the reaction tube 1 after the acidification treatment and the alkalization treatment are completed.

[0056] Reference Figure 1 and Figure 5 As shown, it is a schematic diagram of the structure in which the finished zirconium oxide powder is transported out of the reaction tube 1 for collection; specifically, a collecting port is opened on the side wall of the reaction tube 1 at one end away from the preparation box 12, and a supporting plate 80 for discharging materials in cooperation with the collecting port is installed on the outside of the reaction tube 1, a pull ring 81 consistent with the shape of the collecting port is slidably installed on the collecting port, and a push ring 82 connected to the pull ring 81 is slidably provided on the supporting plate 31.

[0057] By driving the pull ring 81 to slide inside the collection port, the pull ring 81 then drives the push ring 82 to transport the purified zirconium oxide powder on the supporting plate 31 out of the reaction tube 1 and pass through the supporting plate 80 for subsequent collection.

[0058] During operation: In the first step, zirconium oxide powder is placed into the reaction tube 1 through the feed port 10 , and then the acid solution in the acid chamber 13 is transported to the reaction tube 1 through the acid conduit 22 .

[0059] Step 2: Turn on the air pump to blow cold air into the reaction tube 1, then turn on the motor 61, use the motor 61 to drive the air outlet pipe 20 to rotate, stir the zirconium oxide powder and the acid solution with the cooperation of the air outlet pipe 20 and the air pump, drive the two to be fully mixed, and then wait for some impurities in the zirconium oxide powder to dissolve in the acid solution.

[0060] Step 3: After the impurities react with the dissolved acidic solution, the motor 61 rotates in the opposite direction to drive the booster plate 30 to descend. At the same time, the water outlet 34 on the control plate 33 and the separation hole 32 on the carrier plate 31 coincide with each other under the drive of the booster plate 30. During the descent of the booster plate 30, the inside of the reaction tube 1 is pressurized. Then, the acidic solution inside the reaction tube 1 will flow out from the water outlet 34 with the dissolved impurities, and then flow out of the reaction tube 1 from the discharge port 11 for collection.

[0061] Step 4: The booster plate 30 rises again, and the separated zirconium oxide powder is washed by the water supply pipe 24 and the nozzle 25 until the acidity and alkalinity of the zirconium oxide powder is neutral. The booster plate 30 descends again to remove the moisture in the zirconium oxide powder.

[0062] Step 5: After removing the moisture, add the alkaline solution again, and then repeat the above steps to remove another part of the impurities in the zirconium oxide powder through the acidic solution.

[0063] Step 6: After the impurities are removed, the air pump and the air outlet pipe 20 are used to blow hot air into the reaction tube 1 to dry the zirconium oxide powder. After the drying is completed, the push ring 82 is pulled to move the purified zirconium oxide powder to the outside of the reaction tube 1 for collection.

[0064] It is obvious to those skilled in the art that the present invention is not limited to the details of the above exemplary embodiments, and that the present invention can be implemented in other specific forms without departing from the spirit or essential features of the present invention. Therefore, from any point of view, the embodiments should be regarded as exemplary and non-restrictive. The scope of the present invention is defined by the appended claims rather than the above description, and therefore it is intended that all changes within the meaning and scope of the equivalent elements of the claims are included in the present invention, and any figure marks in the claims should not be regarded as limiting the claims involved.

[0065] In addition, it should be understood that although the present specification is described according to implementation modes, not every implementation mode contains only one independent technical solution. This description of the specification is only for the sake of clarity. Those skilled in the art should regard the specification as a whole. The technical solutions in each embodiment may also be appropriately combined to form other implementation modes that can be understood by those skilled in the art.

Claims

1. A device for purifying and preparing nano zirconium oxide powder, comprising a reaction tube (1), characterized in that: The reaction cylinder (1) is provided with a feed inlet (10) and a discharge outlet (11) at the upper and lower ends thereof; a preparation box (12) is installed above the reaction cylinder (1); the interior of the preparation box (12) is divided into an acid liquid chamber (13), an alkali liquid chamber (14) and a water storage chamber (15) by a partition; the water storage chamber (15) is located between the acid liquid chamber (13) and the alkali liquid chamber (14); The reaction tube (1) is provided with a mixing mechanism (2) for mixing zirconium oxide powder with a reactant, the mixing mechanism (2) comprising an air outlet pipe (20), the air outlet pipe (20) being rotatably arranged inside the reaction tube (1), the lower end of the preparation box (12) being provided with a working bucket (21) connected to the air outlet pipe (20), the air outlet pipe (20) being coaxially provided with an acid conduit (22), the acid conduit (22) being provided with an alkali conduit (23), the alkali conduit (23) being provided with a water supply pipe (24) connected to a water storage chamber (15), the water supply pipe (24) being provided with a nozzle (25) connected to the water storage chamber (15), the end of the water supply pipe (24) being away from the preparation box (12), and the acid conduit (22) and the alkali conduit (23) being provided with a through pipe (16) penetrating to the outer wall of the air outlet pipe (20).

2. The device for purifying and preparing nano zirconium oxide powder according to claim 1, characterized in that: An air pump is installed on the reaction cylinder (1), the air pump is connected to the working bucket (21), and the air outlet pipe (20) is provided with a plurality of air holes (17) connected to the inside of the air outlet pipe (20).

3. The device for purifying and preparing nano zirconium oxide powder according to claim 2, characterized in that: Connecting pipes respectively connected to the acid liquid chamber (13) and the alkali liquid chamber (14) are installed inside the working bucket (21); the two connecting pipes are respectively connected to the acid liquid conduit (22) and the alkali liquid conduit (23) through the control member (4).

4. The device for purifying and preparing nano zirconium oxide powder according to claim 1, characterized in that: A pressurizing plate (30) is installed inside the reaction cylinder (1) and is sleeved on the outside of the air outlet pipe (20) and slidably arranged inside the reaction cylinder (1). A bearing plate (31) is arranged at the lower end of the reaction cylinder (1). A separation hole (32) is provided on the bearing plate (31). A control plate (33) is installed below the bearing plate (31). A water outlet (34) matching with the water outlet (34) is provided on the control plate (33).

5. The device for purifying and preparing nano zirconium oxide powder according to claim 4, characterized in that: The reaction cylinder (1) is provided with a control member (4) for driving the acid liquid conduit (22) and the alkali liquid conduit (23) to discharge materials in a displaced manner. The control member (4) comprises a control gear (40). A transverse groove is provided in the middle of the working bucket (21). The control gear (40) is rotatably arranged in the transverse groove. A first connecting port (41) and a second connecting port (42) are provided on the control gear (40). The first connecting port (41) and the second connecting port (42) are movably matched with the acid liquid conduit (22) and the alkali liquid conduit (23) respectively.

6. The device for purifying and preparing nano zirconium oxide powder according to claim 5, characterized in that: A control shaft (43) is rotatably mounted on the reaction cylinder (1); a driving gear (44) meshing with the control gear (40) is mounted on one end of the control shaft (43) located inside the reaction cylinder (1); a spiral groove is formed on a section of the outer wall of the control shaft (43) located inside the reaction cylinder (1); a through hole slidably engaged with the control shaft (43) is formed on the pressure boosting plate (30); a protrusion sliding in the spiral groove is formed in the through hole.

7. The device for purifying and preparing nano zirconium oxide powder according to claim 6, characterized in that: The reaction tube (1) is provided with a matching component (5) for driving the carrier plate (31) and the control plate (33) to cooperate in discharging water. The matching component (5) comprises a matching gear (50). The matching gear (50) is arranged at one end of the control shaft (43) located in the reaction tube (1). The control plate (33) is provided with an arc-shaped matching groove (51). A matching rack (52) meshing with the matching gear (50) is connected to the matching groove (51).

8. The device for purifying and preparing nano zirconium oxide powder according to claim 1, characterized in that: The reaction cylinder (1) is also provided with a pushing member (6) for driving the air outlet pipe (20) to rotate. The pushing member (6) comprises a pushing sleeve (60). The pushing sleeve (60) is rotatably mounted on the reaction cylinder (1) and penetrates the reaction cylinder (1). The air outlet pipe (20) and the pushing sleeve (60) are connected via a belt drive. A motor (61) is provided above the reaction cylinder (1) via a motor seat. The pushing sleeve (60) is connected to an output shaft of the motor (61) via a ratchet member 1 (62).

9. The device for purifying and preparing nano zirconium oxide powder according to claim 8, characterized in that: The reaction cylinder (1) is also provided with a lifting member (7) for driving the booster plate (30) to move up and down. The lifting member (7) comprises a connecting shaft (70). The connecting shaft (70) is rotatably mounted inside the reaction cylinder (1) and is coaxially arranged with the push sleeve (60). The connecting shaft (70) is connected to the output shaft of the motor (61) via a second ratchet member (71).

10. A method for purifying and preparing nano zirconium oxide powder, further comprising a device for purifying and preparing nano zirconium oxide powder according to any one of claims 1 to 9, characterized in that: The purification and preparation method of nano zirconium oxide powder is as follows: S1, powder placement: placing zirconium oxide powder into the reaction tube (1) from the feed port (10), and then transporting the acid solution in the acid liquid chamber (13) into the reaction tube (1); S2, impurity dissolution: cold air is blown into the reaction tube (1), and then the motor (61) is turned on to rotate the air outlet pipe (20). The zirconium oxide powder and the acid solution are stirred in cooperation with the air outlet pipe (20) and the air pump to drive the two to be fully mixed, and then wait for some impurities in the zirconium oxide powder to dissolve in the acid solution; S3, impurity separation: after the impurities react with the dissolved acidic solution, the pressurizing plate (30) is driven to descend, the water outlet (34) and the separation hole (32) on the pressurizing plate (30) are overlapped, and the pressurizing plate (30) is further descended to apply pressure to the inside of the reaction tube (1), and the acidic solution inside the reaction tube (1) flows out from the water outlet (34) with the dissolved impurities; S4, powder washing: the booster plate (30) rises again, and the separated zirconium oxide powder is washed by using the water supply pipe (24) and the nozzle (25) until the acidity and alkalinity of the zirconium oxide powder are neutral, and the booster plate (30) descends again to remove moisture from the zirconium oxide powder; S5. Impurity separation: After removing the water, add the alkaline solution again, and then repeat the above steps to remove another part of the impurities in the zirconium oxide powder by the acidic solution.

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