Hydroxyapatite nanorod preparation device and preparation method thereof

Abstract

The invention relates to the technical field of hydroxyapatite nanorod preparation, in particular to a hydroxyapatite nanorod preparation device and a preparation method thereof.The hydroxyapatite nanorod preparation device comprises a device fixing frame, a mixed solution stirring reaction kettle is fixedly installed in the middle of the device fixing frame, and a mixed solution discharging pipe is arranged at the bottom of the mixed solution stirring reaction kettle; the method has the beneficial effects that the hydroxyapatite nanorod is prepared through the six steps, the hydroxyapatite nanorod preparation device is provided in a matched mode, the second step and the third step can be synchronously carried out through the hydroxyapatite nanorod preparation device, in addition, the fourth step can be automatically carried out through the hydroxyapatite nanorod preparation device, and the production efficiency is improved. The stirring process in the earlier stage of preparation is simplified, the operation complexity is reduced, and the problems that in the prior art, the preparation process of preparing hydroxyapatite microspheres by sequentially mixing and reacting raw materials through a water bath reaction device under the alkaline condition is complex, and the needed time is long are solved.

Description

Technical Field

[0001] The invention belongs to the technical field of hydroxyapatite nanorod preparation, and particularly relates to a hydroxyapatite nanorod preparation device and a preparation method thereof. Background Art

[0002] Hydroxyapatite is an important bioceramic material. Due to its unique physical and chemical properties, hydroxyapatite nanorods are doped into traditional alumina ceramic slurry to form a more stable spatial structure in the coating. The prepared heat-resistant diaphragm has good mechanical stability and thermal stability. Because hydroxyapatite nanorods have a certain aspect ratio, the composite coating has a higher porosity, and the prepared coated diaphragm has better liquid retention capacity. Therefore, the preparation of hydroxyapatite nanorods is the most important step before preparing lithium battery diaphragms.

[0003] The existing Chinese patent document with publication number CN118221097A proposes to prepare hydroxyapatite microspheres by using EDTA·2Na as a metal ion chelating agent, Ca(NO3)2·4H2O as a calcium source, Na2HPO4·12H2O as a phosphorus source, and NaF as a fluorine substituent, mixing them in sequence in a water bath reaction device under alkaline conditions, and centrifugally separating and washing the precipitate. However, the preparation process requires multiple stirring and mixing, which is relatively complicated and time-consuming.

[0004] Therefore, the present invention proposes a hydroxyapatite nanorod preparation device and a preparation method thereof, which solves the problem that the preparation process of hydroxyapatite microspheres prepared by mixing the raw materials in sequence under alkaline conditions using a water bath reaction device is relatively complicated and takes a long time. By changing the preparation raw materials and coordinating with a specific preparation mixing device, the stirring process in the early stage of preparation is simplified and the operation complexity is reduced. Summary of the invention

[0005] In view of the shortcomings of the prior art, the object of the present invention is to provide a hydroxyapatite nanorod preparation device and a preparation method thereof to solve the problems raised in the above background technology.

[0006] To achieve the above-mentioned purpose, the present invention provides the following technical solutions: a hydroxyapatite nanorod preparation device, comprising a device fixing frame, a mixed solution stirring reactor is fixedly installed in the middle of the device fixing frame, a calcium nitrate mixed solution adding tube and a diammonium hydrogen phosphate ammonia solution adding tube are symmetrically arranged above the mixed solution stirring reactor, a mixed solution discharge pipe is arranged at the bottom of the mixed solution stirring reactor, a stirring motor is fixedly installed above the device fixing frame, a stirring rod is fixedly installed on the output shaft of the stirring motor, the lower end of the stirring rod extends to the lower part of the mixed solution stirring reactor, and the two ends of the device fixing frame are fixedly installed at the bottom of the mixed solution stirring reactor. A mixer component 1 and a mixer component 2 are symmetrically arranged on the side, and the structure of the mixer component 1 is the same as that of the mixer component 2. The mixer component 1 includes a measuring injection tube 1, an injection piston rod 1, a solid-liquid mixer 1 and a mixing connecting tube 1. The mixer component 2 includes a measuring injection tube 2, an injection piston rod 2, a solid-liquid mixer 2 and a mixing connecting tube 2. The outlet side of the measuring injection tube 2 and the measuring injection tube 1 are respectively provided with a liquid outlet pipe 2 and a liquid outlet pipe 1. One end of the liquid outlet pipe 1 is fixedly connected to the upper end of the calcium nitrate mixed solution addition pipe, and one end of the liquid outlet pipe 2 is fixedly connected to the upper end of the diammonium hydrogen phosphate ammonia solution addition pipe.

[0007] Preferably, an ammonia injection pipe is provided on the other side of the outlet of the measuring injection tube, an injection piston rod is movably installed inside the measuring injection tube, the outlet end of the measuring injection tube is fixedly connected to the lower end of the mixing connecting tube, the upper end of the solid-liquid mixer is provided with a solid addition port, the bottom of the solid-liquid mixer is provided with a mixed liquid flow port, the outer surface of the upper end of the mixing connecting tube is fixedly connected to the inner surface of the lower end of the mixed liquid flow port, and a rotating mixing ball is rotatably installed inside the solid-liquid mixer.

[0008] Preferably, a filtering mixing cover net is fixedly installed on the top of the mixing connecting pipe one, a conical flow guide cover is slidably installed on the inner surface of the mixing connecting pipe one, and a flow guide cover limiting gasket matched with the conical flow guide cover is arranged below the filtering mixing cover net, and the flow guide cover limiting gasket is fixedly installed on the inner surface of the mixing connecting pipe one.

[0009] Preferably, a flow tube is fixedly installed at the center of the bottom inner wall of the conical air guide cover, a sealing gasket is fixedly installed at the lower end of the flow tube, the flow tube passes through the center of the inner wall of the sealing gasket, and a sealing ring is slidably installed at the lower inside of the flow tube.

[0010] Preferably, a corrugated extrusion sleeve is fixedly installed in the middle of the inner surface of the mixing connecting pipe 1, and the lower end of the corrugated extrusion sleeve is in contact with the upper surface of the sealing gasket.

[0011] Preferably, a liquid gushing hood is fixedly installed above the filtering and mixing hood net, inclined grooves are evenly distributed on the side walls of the liquid gushing hood, and a spiral fixing rod is fixedly installed in the middle of the liquid gushing hood.

[0012] Preferably, a fixed sleeve is fixedly installed on the upper inner surface of the conical air guide cover, a movable sleeve is arranged above the fixed sleeve, a sliding groove matched with the spiral fixing rod is arranged in the middle of the movable sleeve, and a circular through groove is arranged in the middle of the fixed sleeve.

[0013] Preferably, a cleaning ring is fixedly installed on the outer side of the movable sleeve, an outer surface of the cleaning ring is evenly distributed with oblique fixing pads, and an outer side of the oblique fixing pad is evenly distributed with spiral cleaning needles.

[0014] Preferably, an agitator is fixedly installed on the outer surface of the stirring rod, a solution drip baffle ring is arranged above the outer surface of the stirring rod, and splash-proof guide plates are symmetrically fixedly installed on the inner surface of the solution drip baffle ring, the lower end of the splash-proof guide plate is fixedly connected to the outer surface of the stirring rod, and a drip groove corresponding to the position of the splash-proof guide plate is provided on the upper surface of the solution drip baffle ring, and the upper surface of the solution drip baffle ring is in contact with the lower end of the calcium nitrate mixed solution addition tube.

[0015] The present invention also provides a method for preparing hydroxyapatite nanorods, comprising the following steps:

[0016] Step 1: Preliminary preparation: prepare 200 mL of pH 8 ammonia water;

[0017] Step 2: Take 0.005 mol of calcium nitrate and add it to the solid-liquid mixer, take out 100 mL of PH8 ammonia water and inject it into the measuring injection tube, open the mixing connecting tube, push the injection piston rod upward, and inject all 100 mL of PH8 ammonia water into the solid-liquid mixer to completely dissolve 0.005 mol of calcium nitrate to form a calcium nitrate mixed solution, and pull the injection piston rod downward to make the calcium nitrate mixed solution be completely sucked into the measuring injection tube;

[0018] Step 3: Take 0.003 mol of diamine hydrogen phosphate and add it to the second solid-liquid mixer, take out 100 mL of PH8 ammonia water and inject it into the second mixing connecting tube, open the second mixing connecting tube, push the second injection piston rod upward to inject all 100 mL of PH8 ammonia water into the second solid-liquid mixer, so that 0.003 mol of diamine hydrogen phosphate is completely dissolved to form diamine hydrogen phosphate ammonia solution, and pull the second injection piston rod downward to make the diamine hydrogen phosphate ammonia solution be completely sucked into the second measuring injection tube, and close the second mixing connecting tube;

[0019] Step 4: Open the control valves of the liquid outlet pipe 2 and the liquid outlet pipe 1 respectively, push the injection piston rod 2 and the injection piston rod 1 upward again, and start the stirring motor at the same time, so that the calcium nitrate mixed solution is added dropwise into the diammonium hydrogen phosphate ammonia solution while stirring, and continue stirring for 0.5h after the addition is completed;

[0020] Step 5: Open the mixed solution discharge pipe and transfer the mixed solution into the hydrothermal reactor, keep it at a constant temperature of 175°C for 15 hours, and then cool it naturally to room temperature;

[0021] Step 6: centrifugal separation, ultrasonic washing of the filter residue with ultrapure water, and then drying in an oven at 75° C. for 6 hours to obtain hydroxyapatite nanorods with a length of 200 nm to 400 nm.

[0022] Compared with the prior art, the present invention has the following beneficial effects:

[0023] Six steps are proposed to prepare hydroxyapatite nanorods, and a hydroxyapatite nanorod preparation device is proposed. The hydroxyapatite nanorod preparation device can be used to perform step two and step three simultaneously. In addition, the hydroxyapatite nanorod preparation device can be used to automatically perform step four, thereby simplifying the stirring process in the early stage of preparation and reducing the complexity of operation. The problem that the preparation process of hydroxyapatite microspheres prepared by sequentially mixing the raw materials using a water bath reaction device under alkaline conditions in the prior art is relatively complicated and takes a long time is solved. In addition, the mixer component one and the mixer component two can accelerate the dissolution rate of the powder and ammonia water by using the syringe principle, and the intermediate connecting tubes, the mixing connecting tube one and the mixing connecting tube two, are designed so that the powder that is not completely dissolved is filtered by the mixing cover net and the liquid flow to produce a cutting effect to accelerate its dissolution, thereby greatly improving the production efficiency. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] Figure 1 It is a schematic diagram of the overall structure of the present invention.

[0025] Figure 2 It is a schematic diagram of the overall structure of the other side of the present invention.

[0026] Figure 3 It is a schematic diagram of the cross-sectional structure of the mixed solution stirring reactor of the present invention.

[0027] Figure 4 It is a schematic diagram of the solution drip baffle ring structure of the present invention.

[0028] Figure 5 It is a schematic diagram of the overall structure of the mixer assembly of the present invention.

[0029] Figure 6 It is a schematic diagram of the cross-sectional structure of the measuring injection tube of the present invention for absorbing liquid.

[0030] Figure 7 For the present invention Figure 6 A is an enlarged structural diagram of FIG.

[0031] Figure 8 It is a schematic diagram of the cross-sectional structure of the measuring injection tube of the present invention for pushing out the liquid state.

[0032] Fig. 9 For the present invention Figure 8 Schematic diagram of the enlarged structure at B.

[0033] Fig.10 It is a schematic diagram of the cross-sectional structure of the mixing connecting pipe of the present invention in the liquid upwelling state.

[0034] Fig.11 For the present invention Fig.10 Enlarged structural diagram at C.

[0035] Fig.12 It is a schematic diagram of the cross-sectional structure of the mixing connecting pipe of the present invention in the liquid downward suction state.

[0036] Fig.13 For the present invention Fig.12 Enlarged structural diagram at D.

[0037] Fig.14 It is a schematic diagram of the cross-sectional structure of the conical air guide cover of the present invention in the lowest position.

[0038] Fig.15 For the present invention Fig.14 Enlarged structural diagram at E.

[0039] Fig.16 It is a schematic diagram of the structure of the filter mixing cover net viewed from above.

[0040] Fig.17 For the present invention Fig.16 Enlarged structural diagram of F.

[0041] Fig.18 It is a schematic diagram of the cleaning ring structure of the present invention.

[0042] Fig.19 It is a schematic flow chart of the preparation method of the present invention.

[0043] In the figure: 1, device fixing frame; 2, mixed solution stirring reactor; 21, calcium nitrate mixed solution adding tube; 22, diammonium hydrogen phosphate ammonia solution adding tube; 23, mixed solution discharge tube; 3, stirring motor; 4, stirring rod; 41, stirrer; 42, solution dripping baffle ring; 421, splash-proof guide plate; 422, dripping trough; 5, mixer component 1; 51, measuring injection tube 1; 511, liquid outlet tube 1; 512, ammonia injection tube; 52, injection piston rod 1; 53, solid-liquid mixer 1; 531, solid adding port; 532, mixed solution flow port; 533, rotating mixing ball; 54, mixing connecting pipe 1; 54 1. Filter mixing cover net; 5411. Liquid gushing cover; 5412. Spiral fixing rod; 542. Limiting gasket of guide cover; 543. Conical guide cover; 5431. Fixed sleeve; 5432. Movable sleeve; 5433. Cleaning ring; 54331. Oblique fixing pad; 54332. Spiral cleaning needle; 5434. External sealing ring; 544. Flow pipe; 5441. Sealing ring pad; 545. Sealing gasket; 546. Corrugated extrusion sleeve; 6. Mixer assembly II; 61. Weighing injection tube II; 611. Liquid outlet tube II; 62. Injection piston rod II; 63. Solid-liquid mixer II; 64. Mixing connecting tube II; 7. Connecting handle. DETAILED DESCRIPTION

[0044] In order to make the purpose and technical solution of the present invention clearly and completely described, and the advantages more clearly understood, the embodiments of the present invention are further described in detail with reference to the accompanying drawings. It should be understood that the specific embodiments described herein are part of the embodiments of the present invention, not all of them, and are only used to explain the embodiments of the present invention, and are not used to limit the embodiments of the present invention. All other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0045] For example, see Figures 1 to 18The present invention provides a technical solution: a hydroxyapatite nanorod preparation device, comprising a device fixing frame 1, a mixed solution stirring reactor 2 is fixedly installed in the middle of the device fixing frame 1, a calcium nitrate mixed solution adding tube 21 and a diammonium hydrogen phosphate ammonia solution adding tube 22 are symmetrically arranged above the mixed solution stirring reactor 2, a mixed solution discharge pipe 23 is arranged at the bottom of the mixed solution stirring reactor 2, a stirring motor 3 is fixedly installed above the device fixing frame 1, a stirring rod 4 is fixedly installed on the output shaft of the stirring motor 3, and the lower end of the stirring rod 4 extends to the lower part of the mixed solution stirring reactor 2 , a mixer assembly 1 5 and a mixer assembly 2 6 are symmetrically arranged on both sides of the device fixing frame 1, and the structures of the mixer assembly 1 5 and the mixer assembly 2 6 are the same. The mixer assembly 1 5 includes a measuring injection tube 1 51, an injection piston rod 1 52, a solid-liquid mixer 1 53 and a mixing connecting pipe 1 54, and the mixer assembly 2 6 includes a measuring injection tube 2 61, an injection piston rod 2 62, a solid-liquid mixer 2 63 and a mixing connecting pipe 2 64. The outlet side of the measuring injection tube 2 61 and the measuring injection tube 1 51 are respectively provided with a liquid outlet pipe 2 611 and a liquid outlet pipe 1 511, and one end of the liquid outlet pipe 1 511 is connected to the calcium nitrate The upper end of the mixed solution adding tube 21 is fixedly connected, one end of the liquid outlet tube 2611 is fixedly connected to the upper end of the diammonium hydrogen phosphate ammonia solution adding tube 22, an ammonia solution injection tube 512 is provided on the other side of the outlet of the measuring injection tube 51, an injection piston rod 52 is movably installed inside the measuring injection tube 51, the outlet end of the measuring injection tube 51 is fixedly connected to the lower end of the mixing connecting tube 54, the upper end of the solid-liquid mixer 53 is provided with a solid adding port 531, the bottom of the solid-liquid mixer 53 is provided with a mixed liquid flow port 532, the outer surface of the upper end of the mixing connecting tube 54 is connected to the mixed liquid flow port 531. The inner surface of the lower end of the solid-liquid mixer 53 is fixedly connected, a rotating mixing ball 533 is rotatably installed inside the solid-liquid mixer 53, a stirrer 41 is fixedly installed on the outer surface of the stirring rod 4, a solution dripping retaining ring 42 is arranged above the outer surface of the stirring rod 4, and an anti-splashing guide plate 421 is symmetrically fixedly installed on the inner surface of the solution dripping retaining ring 42, the lower end of the anti-splashing guide plate 421 is fixedly connected to the outer surface of the stirring rod 4, and a dripping groove 422 corresponding to the position of the anti-splashing guide plate 421 is opened on the upper surface of the solution dripping retaining ring 42, and the upper surface of the solution dripping retaining ring 42 is in contact with the lower end of the calcium nitrate mixed solution adding tube 21;In this embodiment, the device fixing frame 1 can fix the mixer component 1 5 and the mixer component 2 6 on both sides of the mixed solution stirring reactor 2. The structures of the mixer component 1 5 and the mixer component 2 6 are exactly the same. The mixer component 1 5 is used to mix calcium nitrate and ammonia water, and the mixer component 2 6 is used to mix diammonium hydrogen phosphate and ammonia water. The surfaces of the measuring injection tube 1 51 and the measuring injection tube 2 61 can also be designed with scales to achieve the precise measurement of ammonia water, simplifying the multiple mixing processes in the early stage of preparation. After the mixing is completed, the two mixed solutions are introduced into the mixed solution stirring reactor 2, and the two solutions are evenly mixed by the stirring motor 3 to drive the stirring rod 4. The stirrer 41 on the outer surface of the stirring rod 4 is vertically distributed below the internal liquid level of the mixed solution stirring reactor 2, so that the mixed solution in the mixed solution stirring reactor 2 is stirred and mixed more evenly. As can be seen from the accompanying drawings, the calcium nitrate mixed solution connected to the liquid outlet pipe 1 511 is added The length of the inlet pipe 21 is adapted to the position of the solution dripping retaining ring 42, while the length of the diammonium hydrogen phosphate ammonia solution adding pipe 22 connected to the second outlet pipe 611 is shorter, so that after the control valves of the first outlet pipe 511 and the second outlet pipe 611 are opened, the diammonium hydrogen phosphate ammonia solution inside the measuring injection pipe 2 61 can be smoothly injected into the mixed solution stirring reactor 2, but when the stirring rod 4 drives the solution dripping retaining ring 42 to rotate, the solution dripping retaining ring 42 will seal the lower end of the outlet pipe 1 511, so that the calcium nitrate mixed solution inside the measuring injection pipe 1 51 can intermittently flow out through the dripping groove 422, and the splash-proof guide plate 421 not only plays the role of fixing the solution dripping retaining ring 42 and the stirring rod 4, but also plays the role of guiding the calcium nitrate mixed solution, so that it can be added to the diammonium hydrogen phosphate ammonia solution while stirring along the surface of the stirring rod 4, so that the mixing is more uniform while avoiding the generation of bubbles caused by splashing. ;

[0046] For example 2, please refer to Figures 1 to 18On the basis of the first embodiment, in order to make the solid raw material powder fully dissolved and evenly mixed with the ammonia water, the present embodiment further proposes that a filtering mixing cover net 541 is fixedly installed above the mixing connecting pipe 1 54, a conical flow guide cover 543 is slidably installed on the inner surface of the mixing connecting pipe 1 54, a flow guide cover limiting gasket 542 adapted to the conical flow guide cover 543 is arranged below the filtering mixing cover net 541, the flow guide cover limiting gasket 542 is fixedly installed on the inner surface of the mixing connecting pipe 1 54, a flow pipe 544 is fixedly installed at the center of the bottom inner wall of the conical flow guide cover 543, and a sealing gasket 545 is fixedly installed at the lower end of the flow pipe 544, The circulation tube 544 passes through the center of the inner wall of the sealing gasket 545, and a sealing ring gasket 5441 is slidably installed at the lower part of the circulation tube 544. A corrugated extrusion sleeve 546 is fixedly installed in the middle of the inner surface of the mixing connection tube 1 54, and the lower end of the corrugated extrusion sleeve 546 is in contact with the upper surface of the sealing gasket 545. In this embodiment, because the structures of the mixer component 1 5 and the mixer component 2 6 are exactly the same, the mixer component 1 5 is taken as an example to specifically describe the uniform mixing principle of calcium nitrate and ammonia water. The mixing principle of diamine hydrogen phosphate and ammonia water is exactly the same. First, take 0.005 mol of calcium nitrate, open the sealing plug of the solid addition inlet 531, and All of them are added into the solid-liquid mixer-53, and then the liquid outlet pipe-511 and the mixing connecting pipe-54 are closed and the ammonia injection pipe-512 is opened, and 100mL of PH8 ammonia is injected into the measuring injection pipe-51, and the ammonia injection pipe-512 is closed and the mixing connecting pipe-54 is opened, and the injection piston rod-52 is pushed upward to inject all 100mL of PH8 ammonia into the solid-liquid mixer-53 through the mixing connecting pipe-54. During the rapid injection of ammonia, the sealing ring gasket 5441 is subjected to the pressure of the injection and the circulation pipe 544 is closed. It is worth noting that the attached figure shows that the sealing ring gasket 5441 is resisted or sucked. The sealing gasket 5441 is separated from the flow pipe 544 under normal conditions. The sealing gasket 5441 is at the lower end of the flow pipe 544. The sealing gasket 545 will be moved upward due to the rise of the liquid level, so that the flow pipe 544 and the conical guide cover 543 are moved upward as a whole. The conical guide cover 543 moves to the inside of the filter mixing cover net 541. At this time, the sealing gasket 5441 cancels the sealing of the flow pipe 544 due to the resistance of the bottom of the spiral fixing rod 5412. In this way, ammonia water will flow into the flow pipe 544 and the conical guide cover 543 through the liquid gushing cover 5411 above the filter mixing cover net 541 and enter the solid-liquid mixer 53, making 0.005mol calcium nitrate is dissolved, and then the injection piston rod 52 is pulled downward to re-absorb the mixed solution into the measuring injection tube 51. In the process of aspirating the mixed solution, the circulation tube 544 moves downward with the cooperation of the corrugated extrusion sleeve 546. At this time, the conical guide cover 543 moves to the position of the guide cover limit washer 542 to expose the filter mixing cover net 541. The sealing ring gasket 5441 cancels the closure of the circulation tube 544 under the action of the downward suction force, so that the mixed solution can be filtered and intercepted by the filter mixing cover net 541. The powder that is not completely dissolved is cut by the filter mixing cover net 541 and the liquid flow to accelerate its dissolution. , the solution is sucked into the measuring injection tube 51 through the circulation tube 544 and the middle of the sealing gasket 545, and the injection piston rod 52 is repeatedly pushed and pulled down to make the solution surge back and forth between the measuring injection tube 51 and the solid-liquid mixer 53 until the calcium nitrate is completely dissolved to form a calcium nitrate mixed solution. Finally, the injection piston rod 52 is pulled down to make the calcium nitrate mixed solution be completely sucked into the measuring injection tube 51, and the mixing connecting tube 54 is closed. The dissolution speed of the powder and ammonia water can be accelerated by using the syringe principle. The purpose of completely dissolving the powder in the ammonia water can be achieved through the cooperation of the mixing connecting tube 54, avoiding the problem of incomplete dissolution of the powder under stirring. .

[0047] For example 3, please refer to Figures 1 to 18On the basis of the second embodiment, in order to make the ammonia water surge back and forth to accelerate the dissolution of the powder, the present embodiment further proposes that a liquid gushing cover 5411 is fixedly installed above the filtering and mixing cover net 541, and the side wall of the liquid gushing cover 5411 is evenly distributed with inclined grooves, and a spiral fixing rod 5412 is fixedly installed in the middle of the liquid gushing cover 5411, and a fixed sleeve 5431 is fixedly installed on the inner surface of the upper part of the conical guide cover 543, and a movable sleeve 5432 is arranged above the fixed sleeve 5431, and the movable sleeve 5432 is arranged above the fixed sleeve 5431. The middle part of the movable sleeve 5432 is provided with a slide groove matched with the spiral fixing rod 5412, the middle part of the fixed sleeve 5431 is provided with a circular through groove, the outer side of the movable sleeve 5432 is fixedly installed with a cleaning ring 5433, the outer surface of the cleaning ring 5433 is evenly distributed with oblique fixing pads 54331, and the outer side of the oblique fixing pads 54331 is evenly distributed with spiral cleaning needles 54332; in this embodiment, the liquid gushing cover 5411 is arranged above the filtering and mixing cover net 541, and when the ammonia water is injected upward, the liquid gushing cover 5411 is provided with a cleaning ring 54333, and the cleaning ring 54333 is provided with a cleaning ring 54331. The spiral cleaning needle 54332 on the surface of the oblique fixed pad 54331 can clean the filter holes of the filter mixing cover net 541 while rotating and rising. In particular, the spiral cleaning needle 54332 is arranged in a spiral shape, which can clear the filter holes of the filter mixing cover net 541 and avoid clogging of the filter holes of the filter mixing cover net 541.

[0048] Example 4, please refer to Figures 1 to 18On the basis of the third embodiment, in order to ensure the sealing of the conical flow guide cover 543 during the movement process, the present embodiment further proposes that an external sealing ring 5434 is fixedly installed on the outer surface of the upper end of the conical flow guide cover 543, and the lower inner wall of the liquid gushing cover 5411 and the lower inner wall of the filtering and mixing cover net 541 are both provided with sealing limit grooves adapted to the liquid gushing cover 5411; the bottom side of the injection piston rod 1 52 and the injection piston rod 2 62 are connected by setting a connecting handle 7; in the present embodiment, the external sealing ring 5434 can contact the inner surface of the filtering and mixing cover net 541 during the movement of the conical flow guide cover 543 to maintain the sealing of the conical flow guide cover 543 during the movement process, and the lower ends of the injection piston rod 1 52 and the injection piston rod 2 62 are jointly fixed by the connecting handle 7, so that by pushing or pulling the connecting handle 7, the injection piston rod 1 52 and the injection piston rod 2 62 can be simultaneously moved synchronously, making the operation process simpler and improving production efficiency.

[0049] For example 5, please refer to Figures 1 to 18On the basis of Example 4, this example further proposes a method for preparing hydroxyapatite nanorods, comprising the following steps: Step 1: preliminary preparation, preparing 200 mL of PH8 ammonia water; Step 2: taking 0.005 mol of calcium nitrate and adding it to a solid-liquid mixer-53, taking out 100 mL of PH8 ammonia water and injecting it into a measuring injection tube-51, opening a mixing connecting tube-54 and pushing the injection piston rod-52 upward to inject all 100 mL of PH8 ammonia water into the solid-liquid mixer-53, so that 0.005 mol of calcium nitrate is completely The mixture is completely dissolved to form a calcium nitrate mixed solution, and the injection piston rod 52 is pulled downward so that the calcium nitrate mixed solution is completely sucked into the measuring injection tube 51, and the mixing connecting tube 54 is closed; Step 3: Take 0.003 mol of diammonium hydrogen phosphate and add it to the solid-liquid mixer 63, take out 100 mL of PH8 ammonia water and inject it into the measuring injection tube 61, open the mixing connecting tube 64 and push the injection piston rod 62 upward to inject all 100 mL of PH8 ammonia water into the solid-liquid mixer 63, so that 0.003 mol of diammonium hydrogen phosphate is completely The calcium nitrate mixed solution is completely dissolved to generate diammonium hydrogen phosphate ammonia solution, and the injection piston rod 2 62 is pulled downward so that the diammonium hydrogen phosphate ammonia solution is completely sucked into the measuring injection tube 2 61, and the mixing connecting tube 2 64 is closed; Step 4: Open the liquid outlet tube 2 611 and the liquid outlet tube 1 511 control valve respectively, push the injection piston rod 2 62 and the injection piston rod 1 52 upward again, and start the stirring motor 3 at the same time, so that the calcium nitrate mixed solution is added dropwise to the diammonium hydrogen phosphate ammonia solution while stirring, and continue stirring for 0.5h after the addition is completed; Step 5: Open the mixed solution discharge pipe 23 to The mixed solution is transferred into a hydrothermal reactor, and after being treated at a constant temperature of 175°C for 15 hours, it is naturally cooled to room temperature; Step six: centrifugal separation, the filter residue is ultrasonically washed with ultrapure water, and then dried in an oven at 75°C for 6 hours to obtain hydroxyapatite nanorods with a length of 200nm-400nm; In this embodiment, step two and step three can be carried out simultaneously by using a hydroxyapatite nanorod preparation device. In addition, step four can be automatically carried out by using a hydroxyapatite nanorod preparation device, which simplifies the stirring process in the early stage of preparation and reduces the complexity of operation.

[0050] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A hydroxyapatite nanorod preparation device, comprising a device fixing frame (1), characterized in that: A mixed solution stirring reaction kettle (2) is fixedly installed in the middle of the device fixing frame (1), a calcium nitrate mixed solution adding pipe (21) and a diammonium phosphate ammonia solution adding pipe (22) are symmetrically arranged above the mixed solution stirring reaction kettle (2), a mixed solution discharge pipe (23) is arranged at the bottom of the mixed solution stirring reaction kettle (2), a stirring motor (3) is fixedly installed above the device fixing frame (1), a stirring rod (4) is fixedly installed on the output shaft of the stirring motor (3), and the lower end of the stirring rod (4) extends to the lower part of the mixed solution stirring reaction kettle (2), and a mixer component 1 (5) and a mixer component 2 (6) are symmetrically arranged on both sides of the device fixing frame (1), and the mixer component 1 (5) and the mixing component 2 (6) are symmetrically arranged. The structure of the mixer component 1 (6) is the same, the mixer component 1 (5) comprises a measuring injection tube 1 (51), an injection piston rod 1 (52), a solid-liquid mixer 1 (53) and a mixing connecting tube 1 (54), the mixer component 2 (6) comprises a measuring injection tube 2 (61), an injection piston rod 2 (62), a solid-liquid mixer 2 (63) and a mixing connecting tube 2 (64), the measuring injection tube 2 (61) and the measuring injection tube 1 (51) are respectively provided with a liquid outlet pipe 2 (611) and a liquid outlet pipe 1 (511) on the outlet side, one end of the liquid outlet pipe 1 (511) is fixedly connected to the upper end of the calcium nitrate mixed solution addition pipe (21), and one end of the liquid outlet pipe 2 (611) is fixedly connected to the upper end of the diammonium hydrogen phosphate ammonia solution addition pipe (22).

2. The hydroxyapatite nanorod preparation device according to claim 1, characterized in that: An ammonia injection pipe (512) is provided on the other side of the outlet of the measuring injection tube (51), an injection piston rod (52) is movably installed inside the measuring injection tube (51), the outlet end of the measuring injection tube (51) is fixedly connected to the lower end of the mixing connecting tube (54), the upper end of the solid-liquid mixer (53) is provided with a solid addition port (531), the bottom of the solid-liquid mixer (53) is provided with a mixed liquid flow port (532), the upper end outer surface of the mixing connecting tube (54) is fixedly connected to the lower end inner surface of the mixed liquid flow port (532), and a rotating mixing ball (533) is rotatably installed inside the solid-liquid mixer (53).

3. The hydroxyapatite nanorod preparation device according to claim 1, characterized in that: A filtering mixing cover net (541) is fixedly installed above the mixing connecting pipe (54), a conical flow guide cover (543) is slidably installed on the inner surface of the mixing connecting pipe (54), and a flow guide cover limiting gasket (542) adapted to the conical flow guide cover (543) is arranged below the filtering mixing cover net (541), and the flow guide cover limiting gasket (542) is fixedly installed on the inner surface of the mixing connecting pipe (54).

4. The hydroxyapatite nanorod preparation device according to claim 3, characterized in that: A circulation tube (544) is fixedly installed at the center of the bottom inner wall of the conical air guide cover (543), a sealing gasket (545) is fixedly installed at the lower end of the circulation tube (544), the circulation tube (544) passes through the center of the inner wall of the sealing gasket (545), and a sealing ring gasket (5441) is slidably installed at the lower part of the interior of the circulation tube (544).

5. The hydroxyapatite nanorod preparation device according to claim 4, characterized in that: A corrugated extrusion sleeve (546) is fixedly installed in the middle of the inner surface of the mixing connecting pipe (54), and the lower end of the corrugated extrusion sleeve (546) is in contact with the upper surface of the sealing gasket (545).

6. The hydroxyapatite nanorod preparation device according to claim 5, characterized in that: A liquid gushing hood (5411) is fixedly installed above the filtering and mixing hood net (541), and inclined grooves are evenly distributed on the side walls of the liquid gushing hood (5411). A spiral fixing rod (5412) is fixedly installed in the middle of the liquid gushing hood (5411).

7. The hydroxyapatite nanorod preparation device according to claim 6, characterized in that: A fixed sleeve (5431) is fixedly installed on the upper inner surface of the conical air guide cover (543), a movable sleeve (5432) is arranged above the fixed sleeve (5431), a sliding groove matched with the spiral fixing rod (5412) is arranged in the middle of the movable sleeve (5432), and a circular through groove is arranged in the middle of the fixed sleeve (5431).

8. The hydroxyapatite nanorod preparation device according to claim 7, characterized in that: A cleaning ring (5433) is fixedly installed on the outer side of the movable sleeve (5432), an outer surface of the cleaning ring (5433) is evenly distributed with oblique fixing pads (54331), and an outer side of the oblique fixing pad (54331) is evenly distributed with spiral cleaning needles (54332).

9. The hydroxyapatite nanorod preparation device according to claim 1, characterized in that: The outer surface of the stirring rod (4) is fixedly mounted with a stirrer (41); a solution dripping retaining ring (42) is arranged above the outer surface of the stirring rod (4); an anti-splashing guide plate (421) is symmetrically fixedly mounted on the inner surface of the solution dripping retaining ring (42); the lower end of the anti-splashing guide plate (421) is fixedly connected to the outer surface of the stirring rod (4); a dripping groove (422) corresponding to the position of the anti-splashing guide plate (421) is formed on the upper surface of the solution dripping retaining ring (42); and the upper surface of the solution dripping retaining ring (42) is in contact with the lower end of the calcium nitrate mixed solution adding tube (21).

10. A method for preparing hydroxyapatite nanorods, achieved by the hydroxyapatite nanorod preparation device according to claim 1, characterized in that: The following steps are involved: Step 1: Preliminary preparation: prepare 200 mL of pH 8 ammonia water; Step 2: Take 0.005 mol of calcium nitrate and add it to the solid-liquid mixer (53), take out 100 mL of pH 8 ammonia water and inject it into the measuring injection tube (51), open the mixing connecting tube (54), push the injection piston rod (52) upward to inject all 100 mL of pH 8 ammonia water into the solid-liquid mixer (53), so that 0.005 mol of calcium nitrate is completely dissolved to form a calcium nitrate mixed solution, and pull the injection piston rod (52) downward to allow the calcium nitrate mixed solution to be completely sucked into the measuring injection tube (51); Step 3: Take 0.003 mol of diamine hydrogen phosphate and add it to the second solid-liquid mixer (63), take out 100 mL of PH8 ammonia water and inject it into the second mixing connecting tube (64), open the second mixing connecting tube (64), push the injection piston rod (62) upward to inject all 100 mL of PH8 ammonia water into the second solid-liquid mixer (63), so that 0.003 mol of diamine hydrogen phosphate is completely dissolved to form diamine hydrogen phosphate ammonia solution, and pull the injection piston rod (62) downward to make the diamine hydrogen phosphate ammonia solution be completely sucked into the measuring injection tube (61), and close the second mixing connecting tube (64); Step 4: Open the control valves of the second liquid outlet pipe (611) and the first liquid outlet pipe (511) respectively, push the second injection piston rod (62) and the first injection piston rod (52) upward again, and start the stirring motor (3) at the same time, so that the calcium nitrate mixed solution is added dropwise into the diammonium hydrogen phosphate ammonia solution while stirring, and continue stirring for 0.5 hours after the addition is completed; Step 5: Open the mixed solution discharge pipe (23) to transfer the mixed solution into a hydrothermal reaction kettle, treat at a constant temperature of 175° C. for 15 hours, and then cool naturally to room temperature; Step 6: centrifugal separation, ultrasonic washing of the filter residue with ultrapure water, and then drying in an oven at 75° C. for 6 hours to obtain hydroxyapatite nanorods with a length of 200 nm to 400 nm.

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