A kind of calcium hydroxyphosphate synthesis granulation equipment and process

Abstract

The present invention belongs to the technical field of calcium phosphate preparation, in particular to a hydroxy calcium phosphate synthesis granulation device and process, comprising a reactor and a reactor cover, a heating component is arranged outside the reactor, a reaction chamber is arranged inside the reactor, a stirring component and a dosing component are arranged inside the reaction chamber, the dosing component comprises a second shaft sleeve and a rotating disk which are arranged on a stirring shaft and rotate synchronously and can move vertically, a fixed cover plate is slidably connected to the upper part of the second shaft sleeve and the rotating disk, the fixed cover plate is connected to the reactor cover through a telescopic rod, the fixed cover plate, the second shaft sleeve and the rotating disk form an annular dosing chamber, a drug solution is pumped into the dosing chamber through a first dosing pipe, and a second dosing pipe connected to the dosing chamber is arranged on the lower side of the rotating disk. The present application can effectively utilize the heat generated by the reaction, reduce the temperature difference between the slurry at the stirring shaft and the reactor wall, so that the grains generated by the reaction have a similar growth environment in the entire axial flow circulation process.

Description

Technical Field

[0001] The invention relates to the technical field of calcium phosphate preparation, and in particular to a hydroxy calcium phosphate synthesis granulation device and process. Background Art

[0002] In the process of preparing calcium hydroxyphosphate by neutralization method, a reactor is required. The slurry is stirred by the reactor and kept at a preset reaction temperature. In the reaction process, reactants are simultaneously crystallized and generated. Therefore, on the one hand, sufficient shear stirring effect needs to be provided, and on the other hand, a stable generation environment needs to be provided so that the grains have a similar growth environment in the circulation system. However, the existing reactor is generally heated by an external heating component. Therefore, the slurry temperature near the reactor wall is higher, while the slurry temperature near the stirring shaft is relatively low, which reduces the reaction rate and makes the growth environment of the grains different inside and outside. In addition, when phosphoric acid is added during the reaction, there will be an exothermic effect, and the released heat cannot be well utilized. Summary of the invention

[0003] The invention provides a hydroxy calcium phosphate synthesis granulation device and process, which solves the disadvantages in the prior art that the slurry temperature near the reactor wall is relatively high, while the slurry temperature near the stirring shaft is relatively low, thereby reducing the reaction rate and making the growth environment of the grains different inside and outside, and that there is an exothermic effect when phosphoric acid is added during the reaction process, but the released heat cannot be well utilized.

[0004] The present invention provides the following technical solutions:

[0005] On the one hand, the present application provides a hydroxy calcium phosphate synthesis granulation device, including a reactor and a reactor cover, a heating component is arranged on the outside of the reactor, a reaction chamber is arranged in the reactor, a stirring component and a dosing component are arranged in the reaction chamber, the dosing component includes a second sleeve and a rotating disk which are arranged on the stirring shaft and rotate synchronously and can move vertically, the second sleeve and the upper part of the rotating disk are slidably connected with a fixed cover plate, the fixed cover plate is connected to the reactor cover through a telescopic rod, the fixed cover plate, the second sleeve and the rotating disk form an annular dosing chamber, the dosing chamber is pumped with a drug solution through a first dosing pipe, and a second dosing pipe connected to the dosing chamber is arranged on the lower side of the rotating disk, so that the second dosing pipe and the stirring shaft are connected. The mixing shaft rotates synchronously, and the depth of the second dosing tube extending into the liquid surface can be adjusted by adjusting the height of the rotating disk. An elastic reset part and an adjustment component are arranged between the rotating disk, the second sleeve and the mixing shaft. The adjustment component includes a first connecting rod arranged on the mixing shaft and rotating in a fan shape. The rotating axis of the first connecting rod is perpendicular to the mixing shaft. A counterweight block is arranged at the end of the first connecting rod. A connecting part is arranged between the first connecting rod and the rotating disk, so that when the mixing shaft accelerates, the first connecting rod and the counterweight block drive the rotating disk to move downward. When the mixing shaft decelerates, the elastic reset part drives the rotating disk to move upward. The mixing component includes a mixing shaft and a mixing paddle. The mixing paddle is provided with a built-in radial liquid guide channel.

[0006] In a possible implementation, a circumferential limiting assembly is provided between the second shaft sleeve and the stirring shaft, so that the second shaft sleeve can reciprocate on the stirring shaft and rotate together with the stirring shaft.

[0007] In a possible implementation, the circumferential limit assembly includes a first sleeve, the first sleeve is provided with a limit rod that fits the stirring shaft, the second sleeve is sleeved on the limit rod and the stirring shaft, and the elastic reset member is arranged between the first sleeve and the second sleeve.

[0008] In a possible embodiment, a first mounting hole is formed on the stirring shaft, and a corresponding second mounting hole is formed on the first sleeve. Studs are inserted into the first mounting hole and the second mounting hole, and rotating sleeves are sleeved at both ends of the studs. A limiting ring is fixed at the first end of the first connecting rod, and the limiting ring is sleeved on the rotating sleeve. The rotating sleeve is pressed onto the first sleeve by locking nuts at both ends of the stud.

[0009] In a possible implementation manner, a plurality of groups of the adjustment components are disposed on the first sleeve, and the central axes of the plurality of groups of the adjustment components are symmetrically disposed on the stirring shaft.

[0010] In a possible implementation manner, a vertical constraint is formed between the first connecting rod and the rotating disk through a connecting piece.

[0011] In a possible implementation, the connecting member includes a mounting seat fixed to the bottom of the rotating disk, the mounting seat is rotatably connected to the second connecting rod via a pin, a strip hole is provided at the end of the second connecting rod, and the first connecting rod passes through the strip hole.

[0012] In a possible implementation, the radial liquid guiding channel is composed of a liquid inlet hole arranged on the liquid-facing surface of the outer side of the blade, an internal connecting pipe, and a liquid outlet hole on the liquid-receiving surface of the inner side of the blade.

[0013] In a possible implementation manner, the fixed cover plate is rotatably connected to the second sleeve or the rotating disk via a bearing, and a sealing groove is provided between the fixed cover plate and the second sleeve or the rotating disk, and a sliding sealing ring is provided in the sealing groove.

[0014] In a possible implementation manner, a distance is left between the second dosing tube and the stirring shaft.

[0015] In a possible implementation manner, a driving assembly is disposed on the kettle cover, and the driving assembly drives the stirring assembly to rotate. The driving assembly includes a driving motor, a transmission device, a shaft sealing device, and a frequency converter.

[0016] In a possible implementation manner, the kettle cover is also provided with a manhole, a sight glass, a feeding hole, an air outlet, a sampling hole, a thermometer hole, and a drug adding hole.

[0017] In a possible implementation manner, a medicine storage box is further provided on the kettle cover, and the medicine storage box is connected to a pumping component through a pipeline at the bottom, and the output end of the pumping component is connected to the first medicine adding pipe.

[0018] In a possible implementation manner, a discharge port is provided at the bottom of the reactor.

[0019] On the other hand, the present application provides a synthetic granulation process for calcium hydroxyphosphate, wherein stone powder slurry is added into a reactor, steam is introduced into the jacket of the reactor to heat the reactor, the stone powder slurry is heated and stirred by the reactor, and then an excess of phosphoric acid solution is added and metered, and lime milk is added and metered after slaking, until the calcium-phosphorus ratio of the reaction slurry reaches a preset range, and then slaking again, centrifugal filtration and dehydration are performed, and the filter cake is flash-dried.

[0020] It is to be understood that the foregoing general description and the following detailed description are exemplary only and are not restrictive of the invention.

[0021] In the present invention, phosphoric acid is dispersed into the downward flowing slurry near the stirring shaft by the dosing assembly, so that the heat released by the reaction increases the axial flow temperature at the stirring shaft and reduces the temperature difference between the slurry at the stirring shaft and the reactor wall.

[0022] In the present invention, the second dosing tube rotates synchronously with the stirring shaft and the stirring paddle, so that the speed difference between the second dosing tube and the slurry is reduced, the turbulence formed is reduced, and the overall reaction environment is more uniform.

[0023] In the present invention, when the stirring shaft rotates, the slurry will form an axial flow in the reactor, and a downward vortex will be formed at the slurry liquid surface near the stirring shaft. At the beginning of the reaction, the reaction will release carbon dioxide to help mixing, so the stirring speed can be appropriately reduced. At this time, the depth of the vortex is shallow, and the centrifugal force on the counterweight is weak, so that the second dosing tube extends into the adapted depth. When carbon dioxide is no longer released in the later stage, it is necessary to appropriately increase the stirring shaft speed. The vortex depth formed after the stirring shaft speed is increased is also deeper, and the centrifugal force on the counterweight is also greater, so the rotating disk is driven to move downward, so that the depth of the second dosing tube can be automatically adjusted, so that the second dosing tube is matched with the stirring condition, so that phosphoric acid can be smoothly sent into the downward axial flow, the heat generated by the reaction can be effectively utilized, and direct contact between phosphoric acid and the stirring shaft can be avoided.

[0024] In the present invention, the rotation of the stirring paddle forms an axial flow in the reactor, and a radial flow is formed from the reactor wall to the stirring shaft along the liquid inlet, connecting pipe and liquid outlet, and the radial flow flows in the connecting pipe inside the stirring paddle. On the one hand, the high-temperature liquid close to the reactor wall can be directly radially guided to the stirring shaft, so that the temperature at the stirring shaft and the reactor wall is more uniform. On the other hand, the influence of the radial flow on the overall axial flow can be reduced, thereby improving the microscopic shear strength, accelerating the mass transfer effect at the solid-liquid interface, and promoting the solid-liquid reaction. In addition, it can also provide a better axial flow circulation effect, so that all grains generated by the reaction have a similar growth environment in the entire axial flow circulation path. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] Figure 1 A schematic diagram of the three-dimensional structure of a calcium hydroxyphosphate synthesis granulation device provided in an embodiment of the present invention;

[0026] Figure 2 A schematic diagram of the internal structure of a calcium hydroxyphosphate synthesis granulation device provided in an embodiment of the present invention;

[0027] Figure 3 A schematic diagram of the structure of a stirring component and a dosing component of a calcium hydroxyphosphate synthesis granulation equipment provided in an embodiment of the present invention;

[0028] Figure 4 for Figure 3 One of the partial enlarged schematic diagrams;

[0029] Figure 5 An enlarged schematic diagram of a dosing component of a calcium hydroxyphosphate synthesis granulation device provided in an embodiment of the present invention;

[0030] Figure 6 A schematic diagram of the three-dimensional structure of a dosing component of a calcium hydroxyphosphate synthesis granulation device provided in an embodiment of the present invention;

[0031] Figure 7 A schematic diagram of the structure of a stirring shaft and a first shaft sleeve of a hydroxy calcium phosphate synthesis granulation device provided in an embodiment of the present invention;

[0032] Figure 8 A schematic diagram of a first sleeve, a second sleeve, a rotating disk and a spring structure of a hydroxy calcium phosphate synthesis granulation device provided in an embodiment of the present invention;

[0033] Fig. 9 A schematic diagram of the structure of an adjustment component and a connector of a hydroxy calcium phosphate synthesis granulation device provided in an embodiment of the present invention;

[0034] Fig.10 A schematic diagram of the cross-sectional structure of a second sleeve and a rotating disk of a hydroxy calcium phosphate synthesis granulation device provided in an embodiment of the present invention;

[0035] Fig.11 A schematic diagram of the stirring paddle structure of a calcium hydroxyphosphate synthesis granulation device provided in an embodiment of the present invention;

[0036] Fig.12 A schematic diagram of the blade structure of a calcium hydroxyphosphate synthesis granulation device provided in an embodiment of the present invention;

[0037] Fig.13 This is a schematic diagram of the cross-sectional structure of a blade of a hydroxy calcium phosphate synthesis granulation equipment provided in an embodiment of the present invention.

[0038] Reference numerals:

[0039] 1. Reactor; 2. Reactor cover; 3. Drive motor; 4. Jacket; 5. Stirring shaft; 6. Dosing assembly; 7. Stirring paddle; 501. First mounting hole; 601. Telescopic rod; 602. Fixed cover; 603. Rotating plate; 604. Counterweight; 605. First connecting rod; 606. First dosing pipe; 607. First shaft sleeve; 608. Dosing port; 609. Second dosing pipe; 610. Limit rod; 611. Second shaft sleeve; 612. Mounting seat; 613. Second Connecting rod; 614, strip hole; 615, rotating sleeve; 616, spring; 617, dosing chamber; 618, second mounting hole; 619, stud; 620, locking nut; 621, limiting ring; 622, limiting groove; 623, first axial hole; 624, mounting plane; 625, second axial hole; 626, sliding sealing ring; 701, paddle; 702, third shaft sleeve; 703, third axial hole; 704, liquid inlet hole; 705, connecting pipe; 706, liquid outlet hole. DETAILED DESCRIPTION

[0040] The embodiments of the present invention are described below in conjunction with the accompanying drawings in the embodiments of the present invention.

[0041] There are various processes for preparing calcium hydroxyphosphate, such as the one-step synthesis and molding method, in which the mixed slurry obtained by mixing inorganic calcium salt powder with feed liquid is injected into a mold at room temperature and pressure, reacted and solidified under closed conditions to form a solid material containing calcium hydroxyphosphate. The sol-gel method uses organic calcium compounds and phosphates with high chemical activity components to evenly mix these raw materials in the liquid phase, and hydrolyze and condense chemical reactions to form a stable transparent sol system. After aging, the sol slowly polymerizes between the colloid particles to form a gel with a three-dimensional network structure. The gel network is filled with solvents that have lost their fluidity to form a gel, which can obtain molecular uniformity in a short time, and the reaction temperature is usually low. The chemical precipitation method uses inorganic calcium salts and phosphates as raw materials, and the two are dissolved in water at a certain concentration to form a solution, and then mixed at a certain Ca / P ratio to perform a hydrothermal reaction. By setting parameters such as stirring speed, heating speed, heating temperature and insulation time, the reaction is complete. After the reaction is completed, hydroxyapatite powder is obtained through filtering, washing and drying.

[0042] When preparing hydroxy calcium phosphate (HAP), compared with the sol-gel method and one-step synthesis and molding method, the chemical precipitation method for preparing hydroxy calcium phosphate (HAP) usually uses more common chemical reagents, such as calcium hydroxide, phosphoric acid, etc. The cost of raw materials is relatively low, and the required equipment is relatively simple. No expensive professional equipment is required, thereby reducing the equipment investment cost. The process flow is relatively simple, mainly including the steps of raw material mixing, reaction, precipitation, filtration, washing, drying, etc. It is easy to control, and operators can master the operating skills after simple training, reducing the requirements for technical personnel.

[0043] The key step in preparing calcium hydroxyphosphate by chemical precipitation is the reaction process. The neutralization reaction is carried out through the reactor 1. During the neutralization reaction, on the one hand, the slurry and phosphoric acid need to be evenly mixed by stirring, and on the other hand, the stability of the overall environment during the grain growth process needs to be maintained. Therefore, the reactor 1 needs to provide axial flow stirring while avoiding the formation of turbulence. The reactor 1 is generally heated by the outer jacket 4 or the heating coil. Therefore, the slurry temperature at the reactor wall of the reactor 1 is generally higher than the slurry temperature at the stirring shaft 5. In the case of uneven temperature, on the one hand, the reaction rate will be reduced, and on the other hand, the uniformity of the grain growth environment will be destroyed. In the process of adding phosphoric acid, on the one hand, it is necessary to ensure uniform and quantitative addition, and on the other hand, phosphoric acid will release heat when reacting with the slurry. Directly adding phosphoric acid to the liquid surface will further destroy the temperature uniformity and fail to fully utilize the heat released by the reaction.

[0044] Therefore, the present application provides a synthetic granulation process for calcium hydroxyphosphate, which includes adding stone powder slurry into a reactor 1, introducing steam into a jacket 4 to heat the reactor 1, heating the stone powder slurry through the reactor 1, and then adding an excess of phosphoric acid solution and metering it, adding lime milk and metering it after slaking, until the calcium-phosphorus ratio of the reaction slurry reaches a preset range, slaking it again, performing centrifugal filtration and dehydration, and flash-drying the filter cake to obtain the product.

[0045] In the early stage of the reaction, when there is less material, the carbon dioxide released by the reaction can assist in stirring, so the stirring speed can be reduced to reduce energy consumption. In the later stage of the reaction, when there is more material, the stirring speed should be increased to ensure the mixing of the materials.

[0046] The present application provides a hydroxy calcium phosphate synthesis granulation device, which can provide a more uniform crystallization environment for the preparation of hydroxy calcium phosphate. The radial slurry is guided by the built-in channel, so that the slurry at the wall of the reactor 1 can be quickly guided to the axial flow liquid flow near the stirring shaft 5, which can avoid the generation of turbulence and make the temperature inside and outside more uniform. On the other hand, by directly transporting phosphoric acid to the axial flow, the heat released during the phosphoric acid reaction is dispersed in the axial flow direction close to the stirring shaft 5, further making the temperature inside and outside more uniform. When the stirring shaft 5 changes from slow rotation to fast rotation, the position of releasing phosphoric acid will also change accordingly, avoiding the release position from being separated from the liquid surface or being washed onto the stirring paddle 7 by the liquid flow after release.

[0047] Specifically, Figure 1-2As shown, a hydroxy calcium phosphate synthesis granulation equipment includes a reactor 1 and a reactor cover 2, which are used to seal the reaction chamber to prevent the volatilization of substances or the entry of external impurities during the reaction process. A heating component is arranged on the outside of the reactor 1 to keep the materials in the reactor 1 at an optimal reaction temperature. A reaction chamber is arranged in the reactor 1, and a stirring component and a dosing component 6 are arranged in the reaction chamber. The stirring component is used to mix the reaction materials to promote the uniform progress of the chemical reaction. The dosing component 6 includes a second sleeve 611 and a rotating disk 603 which are arranged on the stirring shaft 5 and rotate synchronously and can move vertically. The second sleeve 611 and the rotating disk 603 are a whole. The second sleeve 611 and the rotating disk 603 can rotate together with the stirring shaft 5, so that the phosphoric acid is evenly distributed on the one hand, and the second dosing tube 609 can rotate synchronously with the stirring paddle 7 and the stirring shaft 5 on the other hand, so that the relative displacement of the second dosing tube 609 extending into the liquid surface and the slurry is small, thereby reducing the generated turbulence. The upper part of 603 is slidably connected with a fixed cover plate 602, so that when the second shaft sleeve 611 and the rotating disk 603 rotate with the stirring shaft 5, the fixed cover plate 602 can not rotate. The fixed cover plate 602 is connected to the kettle cover 2 through a telescopic rod 601. The telescopic rod 601 can prevent the fixed cover plate 602 from rotating on the one hand, and can make the fixed cover plate 602 move up and down synchronously with the second shaft sleeve 611 and the rotating disk 603 on the other hand. The sleeve 611 and the rotating disk 603 form an annular dosing chamber 617, and the dosing chamber 617 is pumped with liquid medicine through the first dosing pipe 606. A dosing port 608 is arranged on the fixed cover plate 602, and the dosing port 608 is connected to the first dosing pipe 606. A second dosing pipe 609 connected to the dosing chamber 617 is arranged on the lower side of the rotating disk 603, so that the second dosing pipe 609 rotates synchronously with the stirring shaft 5, and the depth of the second dosing pipe 609 extending into the liquid surface can be adjusted by adjusting the height of the rotating disk 603.

[0048] Furthermore, a driving assembly is arranged on the kettle cover 2, and the driving assembly can drive the stirring assembly to rotate. The driving assembly includes a driving motor 3, a transmission device, a shaft sealing device, and a frequency converter. The kettle cover 2 is also provided with a manhole, a sight glass, a feeding hole, an air outlet, a sampling hole, a thermometer hole, and a dosing hole. A discharge port is arranged at the bottom of the reactor 1, and the stirring shaft 5 is driven to rotate by the driving motor 3 to ensure that the materials in the reactor 1 can be fully mixed and reacted. The shaft sealing device prevents leakage at the shaft seal to ensure the sealing of the reactor 1. A larger opening is provided through the manhole to facilitate staff to enter the reactor 1 for inspection, cleaning or maintenance, observe the material state and reaction situation inside the reactor 1 through the sight glass, add materials to the reactor 1 through the feeding hole, discharge the gas generated during the reaction through the air outlet, take out a small amount of material for detection and analysis through the sampling hole during the reaction, and install a thermometer through the thermometer hole to monitor the temperature in the reactor 1.

[0049] Specifically, a frame is set at the center of the kettle cover 2 for installing components such as a drive motor 3, a reducer, a coupling, and a frequency converter. The drive motor 3 provides rotational power. The reducer converts the high-speed rotation of the motor into the low-speed rotation required by the agitator. The coupling connects the agitator shaft 5 and the reducer to transmit motion and power. The frequency converter adjusts the speed of the motor to achieve precise control of the stirring speed. The drive motor 3 is installed on the frame, the power input end of the frequency converter is connected to a three-phase AC power supply, the output end of the frequency converter is connected to the input end of the motor, the output end of the drive motor 3 is connected to the input end of the reducer, the output end of the reducer is connected to the upper end of the coupling, and the lower end of the coupling is connected to the agitator shaft 5.

[0050] Furthermore, the upper end of the stirring shaft 5 is rotatably connected to the reactor 1 through a bearing, and a shaft sealing device is provided at the position where the stirring shaft 5 passes through the reactor body. A bearing seat is provided at the lower end of the stirring shaft 5, and the bearing seat is fixedly connected to the lower part of the reactor body through a support rod. Specifically, three support rods are provided, and the bearing seat is supported into a plane by the three support rods. The stability and coaxiality of the stirring shaft 5 during rotation are ensured by the upper bearing and the lower bearing seat.

[0051] Furthermore, a medicine storage box is also provided on the kettle cover 2 , and a pumping assembly is connected to the medicine storage box through a pipeline at the bottom, and the output end of the pumping assembly is connected to the first medicine adding pipe 606 .

[0052] Specifically, the medicine storage box needs to have corrosion resistance, sealing, and strength. A storage tank lined with polyethylene, stainless steel, or polytetrafluoroethylene (PTFE) can be used. The bottom of the medicine storage box and a pumping assembly are connected by a pipeline. The pumping assembly pumps the phosphoric acid in the medicine storage box into the first dosing pipe 606, and the phosphoric acid is pumped into the dosing chamber 617 formed by the rotating disk 603, the second shaft sleeve 611, and the fixed cover plate 602 through the first dosing pipe 606.

[0053] Specifically, the pump body in the pumping assembly is a high-pressure metering pump made of polytetrafluoroethylene, and is equipped with a controller responsible for monitoring and controlling the pumping process, including monitoring equipment such as pressure sensors, flow sensors, temperature sensors, and control equipment such as PLC (programmable logic controller).

[0054] Further, such as Figure 3-10As shown, during the processing, the reactor 1 and the reactor cover 2 form a closed reaction space. After the slurry is placed in the reactor 1, it is heated by the heating component arranged on the outside of the reactor 1. The internal slurry axial flow is driven to circulate through the stirring component inside the reactor 1, so that the phosphoric acid and the slurry are fully mixed. The external medicine storage box pumps the phosphoric acid into the dosing chamber 617 through the pumping component, and then the phosphoric acid in the dosing chamber 617 is added to the reaction chamber of the reactor 1 through the second dosing pipe 609. The stirring shaft 5 will drive the second shaft sleeve 611 and the rotating disk 603 to rotate together during the rotation process. Therefore, the second dosing pipe 609, the second shaft sleeve 611, the rotating disk 603, the stirring shaft 5, and the stirring paddle 7 will not rotate relative to each other, and the second dosing pipe 609 moves in the same direction as the internal slurry. Therefore, compared with the static dosing pipe, the dosing pipe in the present application The relative displacement between the second dosing tube 609 and the slurry is small, which can reduce the turbulence formed. When the second sleeve 611 and the rotating disk 603 rotate with the stirring shaft 5, the fixed cover plate 602 slides relative to the second sleeve 611 and the rotating disk 603, so as to facilitate the installation of the first dosing tube 606 on the fixed cover plate 602, which can not only play a sealing role, but also will not rotate with the second sleeve 611 and the rotating disk 603. When the second sleeve 611 and the rotating disk 603 move upward or downward, the fixed cover plate 602 is driven to move upward or downward. When the fixed cover plate 602 moves upward, the telescopic rod 601 is compressed, and when the fixed cover plate 602 moves downward, the telescopic rod 601 is stretched. Therefore, the second sleeve 611 and the rotating disk 603 will not affect the first dosing tube 606 on the fixed cover plate 602 during the rotation process.

[0055] Furthermore, a circumferential limit assembly is arranged between the second sleeve 611 and the stirring shaft 5, so that the second sleeve 611 rotates together with the stirring shaft 5, and at the same time the second sleeve 611 can reciprocate on the stirring shaft 5. When the stirring shaft 5 rotates, the circumferential limit assembly will be driven to rotate together, and the circumferential limit assembly provides a circumferential force to the second sleeve 611 so that the second sleeve 611 rotates therewith, and the stirring shaft 5 and the circumferential limit assembly do not provide a vertical force to the second sleeve 611, so the second sleeve 611 can slide relatively in the vertical direction.

[0056] Furthermore, the circumferential limit assembly includes a first sleeve 607, on which a limit rod 610 is provided that fits the stirring shaft 5, and a second sleeve 611 is sleeved on the limit rod 610 and the stirring shaft 5, and an elastic reset member is provided between the first sleeve 607 and the second sleeve 611. When the stirring shaft 5 rotates, the first sleeve 607 and the limit rod 610 are driven to rotate together, and the limit rod 610 provides a circumferential force to the second sleeve 611, so that the second sleeve 611 also rotates together. When the second sleeve 611 moves downward, the second sleeve 611 applies a downward force to the elastic reset member, and the elastic reset member is compressed. When the rotation speed of the stirring shaft 5 decreases, the downward force on the second sleeve 611 is smaller than the upward force provided by the elastic reset member, so that the second sleeve 611 moves upward.

[0057] Specifically, a first shaft hole 623 is provided in the middle of the first shaft sleeve 607, and the aperture of the first shaft hole 623 is adapted to the diameter of the stirring shaft 5. The stirring shaft 5 passes through the first shaft hole 623, so that the first shaft sleeve 607 can be fixedly installed with the stirring shaft 5, and two limit rods 610 are provided on the upper part of the first shaft sleeve 607. The limit rods 610 are symmetrically arranged, and the inner sides of the limit rods 610 are close to the edge of the first shaft hole 623, and the inner sides of the limit rods 610 are arc-shaped, so that they can be completely fitted with the stirring shaft 5. The length of the limit rod 610 is set to 2-3 times that of the second shaft sleeve 611, so that the second shaft sleeve 611 can slide freely on the limit rod 610 and the stirring shaft 5 instead of leaving the range of the limit rod 610. Vertical Installation plane 624, when the first connecting rod 605 is installed on the two vertical installation planes 624, the first connecting rod 605 can rotate freely without being disturbed, and when installing the first shaft sleeve 607, the two first connecting rods 605 can be installed simultaneously to improve the installation efficiency. A second shaft sleeve 611 is provided with a second shaft hole 625 in the middle part, and a limiting groove 622 adapted to the limiting rod 610 is provided on the inner side of the second shaft hole 625. When the second shaft sleeve 611 is sleeved on the limiting rod 610 and the stirring shaft 5, the limiting rod 610 extends into the limiting groove 622, so that the second shaft sleeve 611 can move back and forth freely on the limiting rod 610, and the stirring shaft 5 can drive the limiting rod 610 and the second shaft sleeve 611 to rotate together during the rotation.

[0058] Furthermore, a first mounting hole 501 is provided on the stirring shaft 5, and a corresponding second mounting hole 618 is provided on the first sleeve 607. Studs 619 are inserted into the first mounting hole 501 and the second mounting hole 618, and rotating sleeves 615 are sleeved on both ends of the studs 619. A limiting ring 621 is fixed to the head end of the first connecting rod 605, and the limiting ring 621 is sleeved on the rotating sleeve 615. The rotating sleeve 615 is pressed onto the first sleeve 607 by locking nuts 620 at both ends of the stud 619. The first sleeve 607 is fixed to the stirring shaft 5 by the studs 619 and the locking nuts 620, and the rotating sleeve 615 is fixed on both sides of the first sleeve 607. The end of the first connecting rod 605 can rotate around the rotating sleeve 615, and the moving trajectory of the end of the first connecting rod 605 is an arc trajectory rotating around the stud 619 and the rotating sleeve 615.

[0059] Furthermore, an elastic reset member and an adjustment component are provided between the rotating disk 603 and the stirring shaft 5. The reset force is provided by providing the elastic reset member. The adjustment component includes a first connecting rod 605 which is arranged on the stirring shaft 5 and rotates in a fan shape. The rotating axis of the first connecting rod 605 is perpendicular to the stirring shaft 5. A counterweight 604 is provided at the end of the first connecting rod 605. A connecting member is provided between the first connecting rod 605 and the rotating disk 603, so that when the stirring shaft 5 accelerates, the first connecting rod 605 and the counterweight 604 drive the rotating disk 603 to move downward. When the stirring shaft 5 decelerates, the elastic reset member drives the rotating disk 603 to move upward, so that the height of the rotating disk 603 can be adjusted according to the rotation speed of the stirring shaft 5.

[0060] Specifically, Figure 6-9As shown, the first mounting hole 501 vertically penetrates the stirring shaft 5 and is arranged at the upper end of the stirring shaft 5, so that the first sleeve 607, the second sleeve 611, the rotating disk 603, the first connecting rod 605, the second connecting rod 613 and other components are always located on the upper part of the slurry and will not be soaked by the slurry. The first sleeve 607 is provided with a corresponding second mounting hole 618, and the second mounting hole 618 is located at the center of the vertical mounting plane 624. The stud 619 penetrates the first mounting hole 501 and the second mounting hole 618, and both ends of the stud 619 extend out of the second mounting hole 618, and the extended part is sleeved with a rotating sleeve 615, and a limiting ring 621 is sleeved on the rotating sleeve 615, and the limiting ring 621 can rotate freely on the rotating sleeve 615, and the inner end of the rotating sleeve 615 is pressed on the vertical mounting plane 624, and a circular ring extension is arranged on the outer side of the rotating sleeve 615. The inner diameter of the rotating sleeve 615 is adapted to the diameter of the stud 619. When both ends of the stud 619 After the locking nut 620 is installed, the locking nut 620 is pressed on the annular extension, thereby completely fixing the rotating sleeve 615, and the limiting ring 621 can rotate on the rotating sleeve 615, that is, the first connecting rod 605 can rotate up and down around the rotating sleeve 615. When the stirring shaft 5 rotates, it will drive the first shaft sleeve 607 to rotate, and the first shaft sleeve 607 will drive the first connecting rod 605 to rotate around the stirring shaft 5. The counterweight block 604 at the rotating end of the first connecting rod 605 is subjected to the centrifugal force to make the area of ​​the first connecting rod 605 horizontal, so that the first connecting rod 605 rotates downward around the rotating sleeve 615, thereby driving the connecting member and the rotating disk 603 to move downward, so that the elastic reset member is compressed. When the rotation speed of the stirring shaft 5 decreases, the elastic reset member originally compressed resets upward, so that the rotating disk 603 moves upward, the rotating disk 603 drives the connecting member to move upward, and the connecting member drives the first connecting rod 605 to rotate upward.

[0061] Specifically, the elastic reset member is a spring 616, the upper end of the spring 616 is fixedly connected to the bottom of the rotating disk 603 or the bottom of the second sleeve 611, and the lower end of the spring 616 is fixedly connected to the upper surface of the first sleeve 607. The spring 616 is sleeved on the stirring shaft 5 and the limit rod 610. When the stirring shaft 5 rotates at a faster speed, the first connecting rod 605 and the connecting member drive the rotating disk 603 to move downward and press the spring 616, causing the spring 616 to undergo elastic deformation. When the rotation speed of the stirring shaft 5 decreases, the pulling force of the connecting member on the rotating disk 603 is smaller than the upward force of the spring 616, and the pressed spring 616 returns to its original state upward to provide an upward force to the rotating disk 603.

[0062] Furthermore, a plurality of adjustment components are arranged on the first sleeve 607 , and the plurality of adjustment components are symmetrically arranged around the central axis of the stirring shaft 5 , so that the force acting on the stirring shaft 5 during the rotation process is more uniform, and the stirring shaft 5 rotates stably.

[0063] Specifically, Figure 6 , Fig. 9 As shown, in the present application, a total of two groups of adjustment components are provided, and the two groups of adjustment components are symmetrically arranged on both sides of the first sleeve 607, one group of adjustment components is arranged to the left, and the other group is arranged to the right, including two connecting pieces arranged on the lower side of the rotating disk 603, two first connecting rods 605 rotatably arranged on two vertical mounting planes 624, a counterweight block 604 is installed at the end of the two first connecting rods 605, and the two first connecting rods 605 are respectively connected to the corresponding connecting pieces, the first connecting rod 605 on the left side is connected to the connecting piece on the left side, and the first connecting rod 605 on the right side is connected to the connecting piece on the right side. When the stirring shaft 5 rotates, the first connecting rod 605 on the left side tilted upward rotates downward to drive the connecting piece on the left side to move downward together, so that The left connecting piece applies a downward force to the rotating disk 603, and the first connecting rod 605 on the right side that is inclined upward rotates downward, driving the connecting piece on the right side to move downward together, so that the right connecting piece applies a downward force to the rotating disk 603. The rotating disk 603 moves downward under the downward force exerted by the two connecting pieces to compress the spring 616 on the lower side. When the speed of the stirring shaft 5 decreases, the centrifugal force exerted on the counterweight block decreases, so the downward pulling force on the rotating disk 603 will also decrease and be less than the upward force of the spring 616. The spring 616 resets upward, and the spring 616 moves upward to provide an upward force for the rotating disk 603. The rotating disk 603 moves upward, thereby driving the first connecting rods 605 on both sides to rotate upward and reset.

[0064] Furthermore, a vertical constraint is formed between the first connecting rod 605 and the rotating disk 603 through a connecting piece. When the first connecting rod 605 rotates downward, a downward force is applied to the rotating disk 603 through the connecting piece. When the first connecting rod 605 rotates upward, an upward force is applied to the rotating disk 603 through the connecting piece. As a result, the first connecting rod 605 drives the rotating disk 603 to change its adaptability under the centrifugal action, thereby automatically adjusting the height of the rotating disk 603 through the rotation speed of the stirring shaft 5.

[0065] Furthermore, the connecting member includes a mounting seat 612 fixed to the bottom of the rotating disk 603, and the mounting seat 612 is rotatably connected to the second connecting rod 613 through a pin shaft. A strip hole 614 is set at the end of the second connecting rod 613, and the first connecting rod 605 passes through the strip hole 614. When the first connecting rod 605 rotates downward, a downward force is applied to the lower side of the strip hole 614. When the second connecting rod 613 rotates around the pin shaft, a downward force is applied to the rotating disk 603. When the first connecting rod 605 rotates upward, an upward force is applied to the upper side of the strip hole 614. The force, on the one hand, makes the second connecting rod 613 rotate upward around the pin axis, and at the same time provides an upward force, thereby driving the rotating disk 603 to move upward. By setting the mounting seat 612, the second connecting rod 613 and the strip hole 614, the first connecting rod 605 is rotated upward or downward, driving the rotating disk 603 to move downward or upward, and the speed of rotation of the stirring shaft 5 will correspondingly change the rotation angle of the first connecting rod 605, so that the rotating disk 603 can adaptably change with the speed of rotation of the stirring shaft 5.

[0066] Specifically, Fig. 9 As shown, the mounting seat 612 is arranged downward, and the top of the mounting seat 612 is fixedly installed on the lower surface of the rotating disk 603. The mounting seat 612 is provided with facing ears, and a pin shaft is fixed between the ears. A corresponding pin hole is provided on the second connecting rod 613, and the pin hole is sleeved on the pin shaft, so that the second connecting rod 613 can rotate around the pin shaft. A strip hole 614 is provided at the lower end of the second connecting rod 613, and the two sides of the opening of the strip hole 614 are in the same extension direction as the first connecting rod 605, so that during the rotation of the first connecting rod 605, on the one hand, a downward force can be applied to the rotating disk 603 through the second connecting rod 613.

[0067] Furthermore, the fixed cover plate 602 is rotatably connected to the second sleeve 611 or the rotating disk 603 through a bearing, and a sealing groove is provided between the fixed cover plate 602 and the second sleeve 611 and the rotating disk 603, and a sliding sealing ring 626 is provided in the sealing groove. On the one hand, the rotation of the rotating disk 603 and the second sleeve 611 will not affect the fixed cover plate 602. On the other hand, the rotating disk 603, the second sleeve 611 and the fixed cover plate 602 can also achieve a sealing effect when they rotate relative to each other, so that the dosing chamber 617 is sealed.

[0068] Furthermore, a distance is left between the second dosing tube 609 and the stirring shaft 5, so that when phosphoric acid is introduced into the slurry from the dosing chamber 617, the phosphoric acid is sent into the axial flow flowing downward near the stirring shaft 5 after passing through the second dosing tube 609. Since there is a distance between the second dosing tube 609 and the stirring shaft 5, the end position of the second dosing tube 609 is in the axial flow range close to the stirring shaft 5 but not in direct contact with the stirring shaft 5, thereby preventing the sprayed phosphoric acid from being entrained by the axial flow and directly contacting the stirring shaft 5.

[0069] Specifically, Figure 5-Figure 6 As shown, the end of the second dosing tube 609 extends downward into the liquid surface, and the end of the second dosing tube 609 is tilted outward away from the stirring shaft 5. A distance is left between the second dosing tube 609 and the stirring shaft 5, so that the liquid in the dosing chamber 617 is pushed by the downward axial flow after entering the liquid through the second dosing tube 609, so that the added liquid can be quickly distributed in the downward axial flow close to the stirring shaft 5. On the one hand, the second dosing tube 609 rotates synchronously with the stirring shaft 5. Compared with the dosing tube set statically, the turbulence formed by the convection of the dosing tube and the liquid can be reduced, and the uniformity of the crystal growth environment can be maintained. On the other hand, compared with the dosing tube set above the liquid surface, the liquid added by the second dosing tube 609 is directly sent into the axial flow downward along the stirring shaft 5, so that the liquid can be spread faster in the axial flow, and the added phosphoric acid will release part of the heat during the reaction with the axial stone powder slurry, further compensating for the temperature difference between the fluid temperature close to the stirring shaft 5 and the fluid temperature at the wall of the reactor 1.

[0070] Specifically, when the stirring shaft 5 rotates, the slurry will form an axial flow in the reactor 1, and a downward vortex will be formed at the slurry surface near the stirring shaft 5. At the beginning of the reaction, the reaction will release carbon dioxide to help mixing, so the stirring speed can be appropriately reduced. At this time, the depth of the vortex is shallow, and the centrifugal force on the counterweight 604 is weak, so that the second dosing tube 609 extends to an adapted depth. When carbon dioxide is no longer released in the later stage, it is necessary to appropriately increase the speed of the stirring shaft 5. The depth of the vortex formed after the speed of the stirring shaft 5 is increased is also deeper, and the centrifugal force on the counterweight 604 is also greater, so it drives the rotating disk 603 to move downward, so that the depth of the second dosing tube 609 can be automatically adjusted, so that the second dosing tube 609 matches the stirring situation.

[0071] Further, such as Figure 11-13 As shown, the stirring assembly includes a stirring shaft 5 and a stirring paddle 7. The stirring paddle 7 is provided with a built-in radial liquid guiding channel. The stirring shaft 5 will drive the stirring paddle 7 to rotate during its rotation. The rotation of the stirring paddle 7 will cause the slurry in the reactor 1 to flow axially. During the rotation of the stirring paddle 7, the slurry on the outside of the reactor 1 will enter the radial liquid guiding channel and then flow out from the other end. On the one hand, a radial flow channel is provided so that the outer slurry can be mixed with the inner slurry to achieve uniform temperature distribution. On the other hand, the radial flow occurs in the radial liquid guiding channel, so it will not affect the axial flow, making the crystallization environment more stable.

[0072] Specifically, Fig.11As shown, the stirring paddle 7 includes a third shaft sleeve 702 in the middle, and a plurality of blades 701 fixed on the third shaft sleeve 702. A third shaft hole 703 is opened in the middle of the third shaft sleeve 702. The third shaft hole 703 is adapted to the size of the stirring shaft 5. The stirring shaft 5 passes through the third shaft hole 703. The third shaft sleeve 702 is fixedly connected to the stirring shaft 5 by bolts or welding.

[0073] Furthermore, the radial liquid guiding channel is composed of a liquid inlet 704 arranged on the liquid-facing surface of the outer side of the paddle 701, an internal connecting pipe 705, and a liquid outlet 706 on the liquid-receiving surface of the inner side of the paddle 701. Since the liquid inlet 704 is arranged on the liquid-facing surface of the outer side of the paddle 701, when the stirring paddle 7 is rotating and pushing the slurry, part of the slurry will enter from the liquid inlet 704, and the entered slurry will flow through the connecting pipe 705 and then flow out from the liquid outlet 706. On the one hand, the local shearing effect is enhanced to improve the mixing effect. On the other hand, the slurry near the wall of the reactor 1 can be quickly guided through the connecting pipe 705 to the downward axial flow slurry near the stirring shaft 5, which not only reduces the temperature difference between the inside and the outside, but also does not destroy the crystallization growth environment of the axial flow circulation.

[0074] The above are only specific embodiments of the present invention, but the protection scope of the present invention is not limited thereto. Any person skilled in the art can easily think of changes or substitutions within the technical scope disclosed by the present invention, which should be included in the protection scope of the present invention; the embodiments of the present invention and the features in the embodiments can be combined with each other without conflict. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.

Claims

1. A hydroxy calcium phosphate synthesis granulation equipment, comprising a reactor and a reactor cover, a heating component is arranged outside the reactor, a reaction chamber is arranged inside the reactor, a stirring component and a dosing component are arranged inside the reaction chamber, characterized in that: The dosing assembly includes a second sleeve and a rotating disk that are arranged on the stirring shaft and rotate synchronously and can move vertically. The second sleeve and the upper part of the rotating disk are slidably connected with a fixed cover plate, and the fixed cover plate is connected to the kettle cover through a telescopic rod. The fixed cover plate, the second sleeve and the rotating disk form an annular dosing chamber, and the dosing chamber is pumped with liquid medicine through the first dosing tube. A second dosing tube that is connected to the dosing chamber is arranged on the lower side of the rotating disk, so that the second dosing tube and the stirring shaft rotate synchronously, and the depth of the second dosing tube extending into the liquid surface can be adjusted by adjusting the height of the rotating disk. An elastic reset member and an adjusting assembly are arranged between the rotating disk, the second sleeve and the stirring shaft, and a circumferential limit assembly is arranged between the second sleeve and the stirring shaft, so that the second sleeve can move upward and downward on the stirring shaft The stirring shaft is provided with a first sleeve, and a limit rod that fits the stirring shaft is arranged on the first sleeve. The second sleeve is sleeved on the limit rod and the stirring shaft. The elastic reset member is arranged between the first sleeve and the second sleeve. The adjusting member comprises a first connecting rod that is arranged on the stirring shaft and rotates in a fan shape. The rotating axis of the first connecting rod is perpendicular to the stirring shaft. A counterweight block is arranged at the end of the first connecting rod. A connecting member is arranged between the first connecting rod and the rotating disk, so that when the stirring shaft accelerates, the first connecting rod and the counterweight block drive the rotating disk to move downward. When the stirring shaft decelerates, the elastic reset member drives the rotating disk to move upward. The stirring member comprises a stirring shaft and a stirring paddle. The stirring paddle is provided with a built-in radial liquid guide channel.

2. A calcium hydroxyphosphate synthesis granulation equipment according to claim 1, characterized in that, The first shaft sleeve is provided with a plurality of adjustment components, and the central axes of the plurality of adjustment components are symmetrically arranged on the stirring shaft.

3. A calcium hydroxyphosphate synthesis granulation equipment according to claim 1, characterized in that, A vertical constraint is formed between the first connecting rod and the rotating disk through a connecting piece.

4. A calcium hydroxyphosphate synthesis granulation equipment according to claim 1, characterized in that, The radial liquid guiding channel is composed of a liquid inlet hole arranged on the liquid-facing surface of the outer side of the blade, an internal connecting pipe, and a liquid outlet hole on the liquid-repelling surface of the inner side of the blade.

5. A calcium hydroxyphosphate synthesis granulation equipment according to claim 1, characterized in that, The fixed cover plate is rotatably connected to the second sleeve or the rotating disk via a bearing, and a sealing groove is provided between the fixed cover plate and the second sleeve or the rotating disk, and a sliding sealing ring is provided in the sealing groove.

6. A calcium hydroxyphosphate synthesis granulation equipment according to claim 1, characterized in that, There is a distance between the second dosing tube and the stirring shaft.

7. A hydroxy calcium phosphate synthesis granulation process, based on the hydroxy calcium phosphate synthesis granulation equipment according to any one of claims 1 to 6, characterized in that: The stone powder slurry is added into the reactor, and steam is introduced into the jacket of the reactor to heat the reactor. The stone powder slurry is heated and stirred by the reactor, and then an excess of phosphoric acid solution is added and measured. After slaking, lime milk is added and measured until the calcium-phosphorus ratio of the reaction slurry reaches a preset range. After slaking again, centrifugal filtration and dehydration are performed, and the filter cake is flash-dried.

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