A device and method for preparing polymer microspheres with uniform particle size
By designing a device including a constant pressure nozzle and an S-type granulation kettle, using surface tension to form polymer microspheres with uniform particle size, the problems of uneven particle size and poor spherical shape in the prior art are solved, and the problem of uneven particle size and poor spherical shape in the prior art is realized Large-scale production and efficient use of resources.
Patent Information
- Application Number
- CN202110572593.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2021-05-25
- Publication Date
- 2024-12-17
- Estimated Expiration
- 2041-05-25
AI Technical Summary
It is difficult for the prior art to produce polymer microspheres with uniform particle size and good spherical morphology on a large scale, and the existing methods require strict speed control, making it difficult to ensure the consistency of particle size and spherical morphology.
A device including a dispersed phase storage tank, a prepolymerization kettle, a spray head, a constant pressure device, a granulation kettle and a curing kettle is designed. The granulation kettle is sprayed into the granulation kettle through a constant pressure nozzle, and the surface tension of the continuous phase and the dispersant is formed. Microsphere particles with uniform particle size are cured in a curing kettle. The S-shaped setting and jacket heating of the granulator achieve consistency of spherical shape and temperature.
The preparation of polymer microspheres with uniform particle size and good spherical shape is achieved, which is suitable for large-scale production, and through the recycling of continuous phases and the design of multiple curing kettles, the resource utilization and production efficiency are improved.
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Abstract
Description
Technical Field
[0001] The invention belongs to the field of chemistry and relates to a preparation technology of polymer microspheres with uniform particle size, in particular to a preparation device and method of polymer microspheres with uniform particle size. Background Art
[0002] With the development of bioengineering and separation engineering, the demand for specific polymer microspheres is increasing, requiring polymer microspheres to have specific particle sizes and uniform particle size distribution. Although researchers have conducted a lot of technical research on the production technology of polymer microspheres with uniform particle sizes, the technology is still not mature enough to achieve satisfactory results.
[0003] For example, CN101690879 discloses a method for preparing polymer microspheres with uniform particle size and controllable size, in which the dispersed phase is injected into the continuous phase through a sharp hole device to form polymer microspheres with uniform particle size, but the dispersed phase dripping speed of this method is slow, and it is difficult to achieve large-scale production. CN110172117A discloses a technology for preparing uniform particle resin by injection method, in which the dispersed phase and the continuous phase are injected together through a nozzle, and microsphere particles are formed by the difference in speed between the two, but this method is very strict in speed control. Once the speed fluctuates slightly, the particle size will change, and the shape of the microspheres formed in this way is related to the speed and the pipe diameter, and it is difficult to ensure the sphericity. Summary of the invention
[0004] In view of the problems existing in the prior art, the present invention provides a device and method for preparing polymer microspheres with uniform particle size, which can synthesize polymer microspheres with uniform particle size and good sphericity and are suitable for large-scale production.
[0005] The present invention is achieved through the following technical solutions:
[0006] A preparation device for polymer microspheres with uniform particle size, comprising a dispersed phase storage tank, a prepolymerization kettle, a dispersant storage tank, a nozzle, a constant pressure device, a granulation kettle, a continuous phase storage tank and a curing kettle;
[0007] The outlet of the dispersed phase storage tank is connected to the inlet of the prepolymerization kettle, the outlet of the prepolymerization kettle is connected to the inlet of the nozzle through a constant pressure device, the outlet of the nozzle is connected to the inlet at the bottom of the granulation kettle, the outlet at the top of the granulation kettle is connected to the inlet of the curing kettle, the outlet of the continuous phase storage tank is connected to the continuous phase inlet at the top of the granulation kettle, the bottom of the granulation kettle is also provided with a continuous phase outlet, and the dispersant storage tank is connected to the dispersant inlet at the bottom of the granulation kettle;
[0008] The granulation kettle is arranged in an S shape.
[0009] Preferably, the prepolymerization kettle is funnel-shaped, with the large end of the prepolymerization kettle facing upward as an inlet and the small end of the prepolymerization kettle facing downward as an outlet.
[0010] Preferably, more than two curing kettles are provided. When one curing kettle is filled with polymer microspheres during the curing period, another curing kettle is used to continue receiving the polymer microspheres.
[0011] Preferably, the continuous phase outlet at the bottom of the granulation kettle is also connected to the inlet of the continuous phase storage tank.
[0012] Preferably, a solid-liquid separation device is further included, the material outlet of the solidification kettle is connected to the inlet of the solid-liquid separation device, and the liquid phase outlet at the bottom of the solid-liquid separation device is connected to the inlet of the continuous phase storage tank.
[0013] Preferably, a jacket is provided outside the granulation kettle, a hot fluid inlet is provided at the lower end of the jacket, and a hot fluid outlet is provided at the upper end of the jacket; the jacket is also arranged in an S shape, and the S-shaped direction of the jacket is consistent with the S-shaped direction of the granulation kettle.
[0014] Preferably, the granulation kettle is composed of a plurality of spherical structures connected in series.
[0015] Preferably, the nozzle includes a nozzle barrel and a spray plate, the nozzle barrel includes a large head end and a small head end, and the spray plate is installed at the large head end of the nozzle barrel; the large head end of the nozzle barrel is connected to the inlet of the granulation kettle, and the nozzle barrel is filled with particles.
[0016] Preferably, the constant pressure device includes a pressure sensor, a piston booster, a frequency converter, a central controller and a dispersed phase delivery pump;
[0017] The outlet of the prepolymerization kettle is connected to the feed port of the piston booster through a dispersed phase delivery pump; the discharge port of the piston booster is connected to the inlet of the nozzle;
[0018] The pressure sensor collects the pressure of the dispersed phase in the piston booster or the nozzle and transmits it to the central controller. The central controller controls the speed of the dispersed phase delivery pump according to the pressure of the dispersed phase to make the dispersed phase pressure in the nozzle constant;
[0019] The central controller transmits control instructions to the frequency converter according to the pressure of the dispersed phase. The frequency converter adjusts the voltage according to the control instructions to control the output of the piston booster to make the dispersed phase pressure in the nozzle constant.
[0020] A method for preparing polymer microspheres with uniform particle size is disclosed. Based on the device, a dispersed phase enters a prepolymerization kettle from a dispersed phase storage tank, is prepolymerized in the prepolymerization kettle, is pumped into a nozzle at a constant pressure by a constant pressure device, and is then sprayed into a granulation kettle by the nozzle. At the same time, a continuous phase enters the granulation kettle from the top of the continuous phase storage tank, moves from top to bottom to the bottom of the granulation kettle, and is discharged from the continuous phase outlet at the bottom; a dispersant enters the granulation kettle from a dispersant inlet at the bottom of the granulation kettle, moves from bottom to top to the top of the granulation kettle, and is discharged from a curing kettle; the dispersed phase forms microsphere particles under the action of the surface tension of the continuous phase and the dispersant, the microsphere particles move from bottom to top and further undergo a polymerization reaction, are discharged from the top of the granulation kettle and sent to a curing kettle, and are cured in the curing kettle to obtain polymer microspheres.
[0021] Compared with the prior art, the present invention has the following beneficial technical effects:
[0022] The present invention discloses a device for preparing polymer microspheres with uniform particle size. When in use, the dispersed phase enters the prepolymerization kettle from the dispersed phase storage tank. After the dispersed phase is prepolymerized in the prepolymerization kettle to a certain viscosity, it is driven into the nozzle by the constant pressure device at a constant pressure, and then sprayed into the granulation kettle by the nozzle. At the same time, the continuous phase enters the granulation kettle from the top from the continuous phase storage tank, and the dispersant enters the granulation kettle from the bottom from the dispersant storage tank. The dispersed phase forms microsphere particles with uniform particle size under the action of the surface tension of the continuous phase and the dispersant. Since the density of the dispersed phase is less than that of the continuous phase, the dispersed microsphere particles will move from bottom to top, and further polymerization reaction will occur at the same time. When the microsphere particles complete stable polymerization in the granulation kettle and reach a non-adhesive state, they enter the curing kettle, and are cured in the curing kettle and separated to obtain polymer microspheres with uniform particle size; the continuous phase moves from top to bottom to the bottom of the granulation kettle and is discharged from the continuous phase outlet at the bottom; the dispersant enters from the bottom of the granulation kettle, moves from bottom to top, and is discharged from the polymer microsphere outlet at the top of the granulation kettle. The dispersed phase is sprayed into the granulation kettle by the nozzle. The pressure of the dispersed phase entering the nozzle is constant and the nozzle aperture is the same. Therefore, the uniformity of the particle size of the formed polymer microspheres can be ensured. The granulation kettle is arranged in an S shape. The continuous phase and the dispersed phase move up and down in opposite directions along the S-shaped path during movement, thereby forming a vortex. The vortex further polishes the sphericity of the microsphere particles formed by the dispersed phase, thereby improving the surface smoothness of the polymer microspheres. In addition, the S-shaped arrangement of the granulation kettle can also shorten the height of the granulation kettle and reduce the overall height of the device, which is convenient for operation and saves space.
[0023] Furthermore, the prepolymerization kettle is funnel-shaped, with the large end of the prepolymerization kettle facing upward as an inlet and the small end of the prepolymerization kettle facing downward as an outlet. This design can ensure that the dispersed phase that enters the prepolymerization kettle first can be discharged from the prepolymerization kettle first, and ensure that the residence time of all dispersed phases in the prepolymerization kettle is consistent and controllable, thereby ensuring that the degree of prepolymerization is consistent and controllable, and avoiding excessive polymerization of some dispersed phases due to excessive residence time and inability to perform subsequent granulation.
[0024] Furthermore, more than two curing kettles are provided, and when one curing kettle is full, another curing kettle is switched to continue receiving the continuous phase and microsphere particles during the curing period, thereby realizing continuous production.
[0025] Furthermore, the continuous phase outlet at the bottom of the granulation kettle is also connected to the inlet of the continuous phase storage tank, so that the continuous phase can be recycled, the waste of resources can be avoided, and the impact of waste liquid on the environment can be avoided.
[0026] Furthermore, the continuous phase of the curing kettle is also circulated back to the continuous phase storage tank, and this part of the continuous phase is also recycled, further improving resource utilization.
[0027] Furthermore, a jacket is provided outside the granulation kettle. When in use, a hot fluid is introduced to heat the granulation kettle, so that the liquid in the granulation kettle is maintained at a suitable reaction temperature, which facilitates the polymerization reaction of the dispersed phase in the granulation kettle. The jacket is also arranged in an S shape, and its direction is consistent with the granulation kettle, so that the hot fluid in the jacket is evenly distributed at various positions, ensuring that the heat received at different positions of the granulation kettle is the same, and ensuring the consistency of the overall temperature of the granulation kettle.
[0028] Furthermore, the granulation kettle is composed of multiple spherical structures connected in series. When the continuous phase moves, the movement direction is further changed at the side wall of the granulation kettle, which further polishes the sphericity of the polymer microspheres and improves the surface smoothness of the polymer microspheres. When the microsphere particles move, they will be resisted by the side wall of the granulation kettle, which reduces the floating speed of the microsphere particles and reduces the overall height of the granulation kettle device.
[0029] Furthermore, the variable diameter design of the nozzle barrel reduces the speed of the dispersed phase after entering the nozzle, and can be stably sprayed from the nozzle hole into the continuous phase to form microsphere particles with uniform particle size, and finally polymerize into polymer microspheres with a certain strength. The presence of particles in the nozzle can further buffer the injection pressure of the dispersed phase and ensure the consistency of the pressure of each nozzle hole.
[0030] Furthermore, the central controller processes the collected dispersed phase pressure data in the nozzle and transmits control instructions to the dispersed phase delivery pump. The dispersed phase delivery pump controls the feed speed of the dispersed phase by adjusting the speed to ensure that the dispersed phase pressure in the nozzle is constant. The central controller also transmits control instructions to the frequency converter based on the collected dispersed phase pressure data in the nozzle. The frequency converter adjusts the voltage according to the control instructions to control the output of the piston booster to ensure that the dispersed phase pressure in the nozzle is constant. BRIEF DESCRIPTION OF THE DRAWINGS
[0031] Figure 1 This is a schematic diagram of a device for preparing polymer microspheres with uniform particle size according to the present invention;
[0032] Figure 2It is a schematic diagram of the granulation kettle and jacket of the present invention;
[0033] Figure 3 A schematic diagram of a granulation kettle in one embodiment of the present invention;
[0034] Figure 4 It is a schematic diagram of the nozzle and constant pressure device of the present invention.
[0035] In the figure: curing kettle 1, stirring rod 2, continuous phase storage tank 3, granulation kettle 4, dispersant inlet 5, dispersed phase storage tank 6, prepolymerization kettle 7, nozzle 8, continuous phase outlet 9, piston booster 10, dispersant storage tank 12, solid-liquid separation device 13, jacket 14, hot fluid inlet 15, hot fluid outlet 16. DETAILED DESCRIPTION
[0036] The present invention is further described in detail below in conjunction with specific embodiments, which are intended to explain the present invention rather than to limit it.
[0037] like Figure 1 As shown, the device for preparing polymer microspheres with uniform particle size described in the present invention includes a dispersed phase storage tank 6, a prepolymerization kettle 7, a nozzle 8, a constant pressure device, a granulation kettle 4, a continuous phase storage tank 3 and a curing kettle 1.
[0038] The outlet of the dispersed phase storage tank 6 is connected to the top inlet of the prepolymerization kettle 7, the bottom outlet of the prepolymerization kettle 7 is connected to the inlet of the nozzle 8 through a constant pressure device, the outlet of the nozzle 8 is connected to the inlet at the bottom of the granulation kettle 4, the polymer microsphere outlet at the top of the granulation kettle 4 is connected to the inlet of the curing kettle 1, the outlet of the continuous phase storage tank 3 is connected to the continuous phase inlet at the top of the granulation kettle 4, and the bottom of the granulation kettle 4 is also provided with a continuous phase outlet 9. A stirring rod 2 is provided in the curing kettle 1.
[0039] The granulation kettle 4 is arranged in an S shape. The granulation kettle 4 is arranged in an S shape, and a vortex is formed when the continuous phase and the dispersed phase move up and down in opposite directions along the S-shaped path. The vortex further polishes the sphericity of the formed microsphere particles, thereby improving the surface smoothness of the polymer microspheres. In addition, the S-shaped arrangement of the granulation kettle 4 can also shorten the height of the granulation kettle 4 and reduce the overall height of the device, which is convenient for operation and saves space.
[0040] The dispersed phase is sprayed into the granulation kettle 4 from the nozzle 8 at a constant pressure. The nozzle holes of the nozzle 8 have the same diameter, so the uniformity of the particle size of the formed polymer microspheres can be ensured.
[0041] The present invention has found that styrene can not be granulated after being completely solidified after prepolymerization for 60 minutes at 45°C. Therefore, in one embodiment of the present invention, the prepolymerization kettle 7 is funnel-shaped, with the large end of the prepolymerization kettle 7 facing upward as an inlet, and the small end of the prepolymerization kettle 7 facing downward as an outlet. This design can ensure that the dispersed phase that first enters the prepolymerization kettle 7 can be discharged from the prepolymerization kettle 7 first, and ensure that the residence time of all dispersed phases in the prepolymerization kettle 7 is consistent and controllable, thereby ensuring that the degree of prepolymerization is consistent and controllable, and avoiding that some dispersed phases cannot be granulated later due to excessive polymerization due to too long residence time.
[0042] In one embodiment of the present invention, more than two curing kettles 1 are provided. When one curing kettle 1 is full, another curing kettle 1 is used to continue receiving the continuous phase and microsphere particles during the curing period, thereby achieving continuous production.
[0043] In one embodiment of the present invention, the continuous phase outlet 9 at the bottom of the granulation kettle 4 is also connected to the inlet of the continuous phase storage tank 3, and the continuous phase outlet of the curing kettle 1 is also connected to the inlet of the continuous phase storage tank 3. Thus, the continuous phase can be recycled to avoid waste of resources and the impact of waste liquid on the environment.
[0044] In one embodiment of the present invention, a solid-liquid separation device 13 is further included. The polymer microsphere outlet of the curing kettle 1 is connected to the inlet of the solid-liquid separation device 13 , and the bottom liquid phase outlet of the solid-liquid separation device 13 is connected to the inlet of the continuous phase storage tank 3 .
[0045] In one embodiment of the present invention, Figure 2 As shown, a jacket 14 is provided outside the granulation kettle 4. A hot fluid inlet 15 is provided at the lower end of the jacket 14, and a hot fluid outlet 16 is provided at the upper end of the jacket 14. When in use, the hot fluid enters the jacket from the hot fluid inlet 15 and flows out of the jacket 14 from the hot fluid outlet 16, thereby achieving a heating effect on the granulation kettle 4, so that the liquid in the granulation kettle 4 is maintained at a suitable polymerization temperature, which is convenient for the dispersed phase to perform a polymerization reaction in the granulation kettle 4.
[0046] In one embodiment of the present invention, the jacket is also arranged in an S shape, and its direction is consistent with the granulation kettle 4. The jacket and the granulation kettle 4 are designed to be of the same shape, so that the hot fluid in the jacket 14 is evenly distributed at various positions, ensuring that the heat received at different positions of the granulation kettle 4 is the same, and ensuring the consistency of the overall temperature of the granulation kettle 4.
[0047] In one embodiment of the present invention, the jacket is coated with a heat-insulating layer to play a role in heat preservation, avoid heat loss, improve heat utilization efficiency, and reduce energy consumption.
[0048] In one embodiment of the present invention, Figure 3As shown, the side wall of the granulation kettle 4 is composed of a plurality of spherical structures connected in series, and the connection between two adjacent spherical structures is connected. When the continuous phase moves, the movement direction is further changed at the side wall of the granulation kettle 4, which further polishes the sphericity of the polymer microspheres and improves the surface smoothness of the polymer microspheres.
[0049] In one embodiment of the present invention, a dispersant storage tank 12 is further included, and a dispersant inlet is also provided at the lower end of the granulation kettle 4. When in use, the dispersant in the dispersant storage tank 12 is injected into the granulation kettle 4 through the dispersant inlet 5.
[0050] In one embodiment of the present invention, the nozzle 8 includes a nozzle barrel and a spray plate, the nozzle barrel includes a large head end and a small head end, and the spray plate is installed at the large head end of the nozzle barrel. The large head end of the nozzle barrel is connected to the inlet of the granulation kettle 4. The nozzle barrel is filled with granules, which can be glass beads.
[0051] The variable diameter design of the nozzle barrel reduces the speed of the dispersed phase after entering the nozzle 8, and can be stably sprayed from the nozzle hole into the continuous phase to form microsphere particles with uniform particle size, and finally polymerize into polymer microspheres with a certain strength. The presence of particles in the nozzle can further buffer the injection pressure of the dispersed phase and ensure the consistency of the pressure of each nozzle hole.
[0052] In one embodiment of the present invention, Figure 4 The constant pressure device includes a pressure sensor, a piston booster 10, a frequency converter 11, a central controller 17 and a dispersed phase delivery pump; the outlet of the dispersed phase storage tank 6 is connected to the feed port of the piston booster 10 through the dispersed phase delivery pump; the discharge port of the piston booster 10 is connected to the inlet of the nozzle 8; the pressure sensor collects the pressure of the dispersed phase in the piston booster or the nozzle 8, and transmits it to the central controller 17, and the central controller 17 controls the speed of the dispersed phase delivery pump according to the pressure of the dispersed phase, so that the dispersed phase pressure in the nozzle is constant; the central controller 17 transmits a control instruction to the frequency converter according to the pressure of the dispersed phase, and the frequency converter adjusts the voltage according to the control instruction to control the output of the piston booster, so that the dispersed phase pressure in the nozzle is constant.
[0053] In one embodiment of the present invention, a flow meter is provided on the pipeline between the dispersed phase storage tank 6 and the prepolymerization kettle 7, and pumps are provided on the pipeline between the prepolymerization kettle 7 and the piston booster 10, on the pipeline connecting the continuous phase storage tank 3 and the granulation kettle 4, on the pipeline connecting the solidification kettle 1 and the solid-liquid separation device 13, and on the pipeline connecting the dispersant storage tank 12 and the granulation kettle 4.
[0054] In the present invention, the dispersed phase is one or more of styrene, divinylbenzene, acrylonitrile, methyl acrylate, toluene, liquid wax, etc., and one or more of initiators such as azobisisobutyronitrile, dibenzoyl peroxide, isopropylbenzene hydroperoxide, tert-butyl hydroperoxide, etc. are added to the dispersed phase.
[0055] In the present invention, the prepolymerization kettle is made of stainless steel with a heating jacket, the prepolymerization temperature is controlled at 50-90°C, and the prepolymerization time is controlled at 20-60min. The prepolymerization temperature and time are different for different dispersed phases. Styrene monomer is prepolymerized at 45°C for 25min.
[0056] In the present invention, the flow meter is a rotor flow meter.
[0057] In the present invention, the diameter of the spray holes on the spray head is between 0.1-2 mm, and the optimal spacing between the spray holes is 2-4 mm.
[0058] In the present invention, the continuous phase is water, or one or two of sodium chloride and methylene blue are added to water.
[0059] In the present invention, the dispersant is one or more of aqueous solutions of polyvinyl alcohol, gelatin, cellulose, sodium dodecylbenzene sulfonate, etc.
[0060] In the present invention, the curing kettle 1 is a stainless steel reactor with a heating jacket, and the temperature of the reactor is controlled between 70-100°C.
[0061] The working process is as follows: the dispersed phase enters the prepolymerization kettle 7 from the dispersed phase storage tank 6, and after the dispersed phase is prepolymerized in the prepolymerization kettle 7, it is driven into the nozzle 8 by the piston booster at a constant pressure, and then sprayed into the granulation kettle 4 by the nozzle 8. At the same time, the continuous phase enters the granulation kettle 4 from the top from the continuous phase storage tank 3, and the dispersant enters the granulation kettle 4 from the bottom from the dispersant storage tank 12. The dispersed phase is sprayed into the granulation kettle 4 through the nozzle to form microsphere particles with uniform particle size under the surface tension of the continuous phase and the dispersant. Since the density of the dispersed phase is less than that of the continuous phase, the dispersed microsphere particles will move from bottom to top, and further polymerization reaction will occur at the same time. When the microsphere particles complete stable polymerization in the granulation kettle and reach a non-sticky state, they are pumped into the curing kettle 1, and after curing in the curing kettle 1, they are pumped to the solid-liquid separation device 13 for separation to obtain polymer microspheres; the continuous phase moves from top to bottom to the bottom of the granulation kettle 4 and is discharged from the continuous phase outlet at the bottom.
[0062] The constant pressure device of the present invention allows the dispersed phase to pass through the nozzle at a constant pressure. The nozzle is funnel-shaped, and the spray holes on the spray plate are arranged as concentric circles. The size of the polymer particles is adjusted by controlling the size and distribution of the apertures on the polymerization kettle spray plate and the feed rate. The dispersed phase enters the funnel-shaped nozzle at a constant pressure. The nozzle is filled with spherical particles to further buffer the dispersed phase pressure and ensure that the dispersed phase passes through each aperture on the spray plate at a constant pressure. Under constant pressure, the dispersed phase enters the granulation kettle after passing through the spray holes with the same aperture, and is dispersed into microsphere particles with uniform particle size under the action of the surface tension of the continuous phase and the dispersant. At the same time, the microsphere particles undergo further polymerization reaction in the granulation kettle. When the microsphere particles complete stable polymerization and reach a non-sticky state, they enter the curing kettle. After curing in the curing kettle, they are pumped to the solid-liquid separation device for separation to obtain polymer microspheres with uniform particle size.
[0063] The production capacity of the device of the present invention can be adjusted by changing the pressure and the number of nozzle holes on the nozzle. The particle size of the polymer microspheres can be adjusted by changing the pressure and the diameter of the nozzle holes on the nozzle. The particle size produced by the device of the present invention is controllable, and the yield is above 98%. The continuous phase of the device of the present invention can be repeatedly recycled, which greatly reduces the production cost and reduces the discharge of sewage.
Claims
1. A device for preparing polymer microspheres with uniform particle size, characterized in that: It comprises a dispersed phase storage tank (6), a prepolymerization kettle (7), a dispersant storage tank (12), a nozzle (8), a constant pressure device, a granulation kettle (4), a continuous phase storage tank (3) and a curing kettle (1); The outlet of the dispersed phase storage tank (6) is connected to the inlet of the prepolymerization kettle (7), the outlet of the prepolymerization kettle (7) is connected to the inlet of the nozzle (8) through a constant pressure device, the outlet of the nozzle (8) is connected to the bottom inlet of the granulation kettle (4), the outlet at the top of the granulation kettle (4) is connected to the inlet of the curing kettle (1), the outlet of the continuous phase storage tank (3) is connected to the continuous phase inlet at the top of the granulation kettle (4), the bottom of the granulation kettle (4) is also provided with a continuous phase outlet (9), and the dispersant storage tank (12) is connected to the dispersant inlet (5) at the bottom of the granulation kettle (4); The granulation kettle (4) is arranged in an S shape; the continuous phase outlet (9) at the bottom of the granulation kettle (4) is also connected to the inlet of the continuous phase storage tank (3); It also comprises a solid-liquid separation device (13), wherein the material outlet of the solidification kettle (1) is connected to the inlet of the solid-liquid separation device (13), and the liquid phase outlet at the bottom of the solid-liquid separation device (13) is connected to the inlet of the continuous phase storage tank (3).
2. The device for preparing polymer microspheres with uniform particle size according to claim 1, characterized in that: The prepolymerization kettle (7) is funnel-shaped, with the large end of the prepolymerization kettle (7) facing upward as an inlet and the small end of the prepolymerization kettle (7) facing downward as an outlet.
3. The device for preparing polymer microspheres with uniform particle size according to claim 1, characterized in that: More than two curing kettles (1) are provided. When in use, when one curing kettle (1) is filled with polymer microspheres, during the curing period, another curing kettle (1) is used to continue receiving the polymer microspheres.
4. The device for preparing polymer microspheres with uniform particle size according to claim 1, characterized in that: A jacket (14) is arranged outside the granulation kettle (4); a hot fluid inlet (15) is arranged at the lower end of the jacket (14), and a hot fluid outlet (16) is arranged at the upper end of the jacket (14); the jacket (14) is also arranged in an S shape, and the S-shaped direction of the jacket (14) is consistent with the S-shaped direction of the granulation kettle (4).
5. The device for preparing polymer microspheres with uniform particle size according to claim 1, characterized in that: The granulation kettle (4) is composed of a plurality of spherical structures connected in series.
6. The device for preparing polymer microspheres with uniform particle size according to claim 1, characterized in that: The nozzle (8) comprises a nozzle barrel and a spray plate, the nozzle barrel comprises a large end and a small end, and the spray plate is mounted on the large end of the nozzle barrel; the large end of the nozzle barrel is connected to the inlet of the granulation kettle (4), and the nozzle barrel is filled with granules.
7. The device for preparing polymer microspheres with uniform particle size according to claim 1, characterized in that: The constant pressure device comprises a pressure sensor, a piston booster (10), a frequency converter (11), a central controller (17) and a dispersed phase delivery pump; The outlet of the prepolymerization kettle (7) is connected to the feed port of the piston booster (10) via a dispersed phase delivery pump; the discharge port of the piston booster (10) is connected to the inlet of the nozzle (8); The pressure sensor collects the pressure of the dispersed phase in the piston booster or the nozzle (8) and transmits it to the central controller (17). The central controller (17) controls the speed of the dispersed phase delivery pump according to the pressure of the dispersed phase to make the dispersed phase pressure in the nozzle constant; The central controller (17) transmits a control instruction to the frequency converter according to the pressure of the dispersed phase, and the frequency converter adjusts the voltage according to the control instruction to control the output of the piston booster so that the dispersed phase pressure in the nozzle is constant.
8. A method for preparing polymer microspheres with uniform particle size, characterized in that: Based on the device described in any one of claims 1 to 7, the dispersed phase enters the prepolymerization kettle (7) from the dispersed phase storage tank (6), the dispersed phase is prepolymerized in the prepolymerization kettle (7), and then is pumped into the nozzle (8) by a constant pressure device at a constant pressure, and then sprayed into the granulation kettle (4) by the nozzle (8), and at the same time, the continuous phase enters the granulation kettle (4) from the top from the continuous phase storage tank (3), and the continuous phase moves from top to bottom to the bottom of the granulation kettle (4) and is discharged from the continuous phase outlet at the bottom; The dispersant enters the granulation kettle (4) from the dispersant inlet at the bottom of the granulation kettle (4), moves from bottom to top to the top of the granulation kettle (4), and is discharged from the curing kettle; the dispersed phase forms microsphere particles under the action of the surface tension of the continuous phase and the dispersant, and the microsphere particles move from bottom to top and further undergo a polymerization reaction, and are discharged from the top of the granulation kettle (4) and sent to the curing kettle (1), and are cured in the curing kettle (1) to obtain polymer microspheres.
Citation Information
Patent Citations
Technology for preparing monosphere resin by means of jetting method
CN110172117A
Device for preparing polymer microspheres with uniform particle size
CN215234088U
