Dispersion method for preparing micron-sized particles

Abstract

The invention discloses a dispersion method for preparing micron-sized particles, which comprises the step of using a shearing machine for dispersion, the shearing machine comprises a tank body, a tank cover, a material injection port, a material discharge port and a shearing module, and the method comprises the following steps: (1) firstly injecting a dispersion medium into the tank body of the shearing machine through the material injection port, and starting shearing; (2) injecting a dispersion phase and a dispersion medium in proportion; (3) circularly shearing the dispersed phase in a shearing machine for more than three times; and (4) discharging the small-particle-size particles or emulsion droplets from an upper material outlet under the action of fluid injection power, and sinking the large-particle-size particles or emulsion droplets to the bottom of the tank under the action of gravity to be sheared again by a shearing machine. The problems of non-uniform shearing, poor particle morphology and excessive heat production are solved, the requirement of any required scale from small-scale production to large-scale production is met, the limitation of a batch type shearing machine and a pipeline type shearing machine is solved, the amplification effect is reduced, and the research and development cost is reduced.

Description

[0001] Cross-references to related applications

[0002] This application is a divisional application of application number 2024118696995, filed on December 18, 2024, entitled "Method for Dispersion of Micron-sized Particles," the entire contents of which are incorporated herein by reference. This application claims priority to application number 2023118648249, filed on December 29, 2023, entitled "Method for Dispersion of Micron-sized Particles," the entire contents of which are incorporated herein by reference. Technical Field

[0003] This invention relates to the field of particle dispersion technology, and more specifically to a dispersion method for preparing micron-sized particles. Background Technology

[0004] Shear emulsification equipment is widely used in the pharmaceutical, food, cosmetic, and chemical industries. Materials are sheared and dispersed by a high-speed rotating rotor to prepare products with different particle sizes, such as dairy products, emulsions, suspensions, and nano-micron granules. The particle size is usually around 0.1μm-100μm, and the particle size and particle size distribution have a direct impact on the quality of the product.

[0005] Common preparation equipment includes batch high-shear dispersers and inline high-shear dispersers. Batch high-shear dispersers are suitable for particle dispersion in laboratories or small-batch production workshops, and typically include top-mounted and bottom-mounted types. The size of the shear head and the effective shear volume of batch high-shear dispersers limit their effectiveness. After obtaining a small-scale sample that meets expectations in the early stages of research and development, it is necessary to further scale up the production, i.e., increase the reaction volume. However, increasing the reaction volume makes it difficult to ensure uniform shearing, usually requiring changes to the appropriate shear head. This involves alterations to various process parameters and a scale-up effect. Continuous process parameter adjustments require more time and cost, and there is even a risk of not being able to reproduce the small-scale results. On the other hand, it must also be considered that batch high-shear dispersers may not meet the requirements of large-scale mass production.

[0006] Inline high-shear dispersers enable continuous production, solving most issues in the transition from small-scale to large-scale product manufacturing. However, for materials with significant viscosity differences between the dispersed phase and the dispersion medium, inline high-shear dispersers often result in large clumps of material forming before it reaches the shear head, hindering uniform dispersion. Furthermore, the relatively small mixing chamber means the material is not fully homogenized before exiting the equipment, leading to large particle sizes and non-spherical shapes in the final product, failing to meet quality standards. Increasing the speed of the inline high-shear disperser from 15,000 rpm to 18,000 rpm further exacerbates the problem. The powerful suction of the equipment results in a large amount of material being discharged before being uniformly dispersed, leading to larger particle sizes and irregular product morphology.

[0007] The micrometer-sized particles are prepared by using the pipeline high-shear dispersion machine, and the rotation speed is set to 11000 rpm, 15000 rpm and 18000 rpm respectively, the prepared microparticles have large particle size, wide particle size span (Span) and uneven particle size distribution, and the particle size is not effectively reduced with the increase of the rotation speed, and the prepared microparticles have poor morphology. Moreover, the temperature of the material rises rapidly when the micrometer-sized particles are prepared by using the pipeline high-shear dispersion machine, and the temperature of the material rises by 6 ℃ after being sheared for 5 min at 15000 rpm, which is not conducive to the preparation of heat-sensitive materials. SUMMARY

[0008] The present application proposes a dispersion method for preparing micrometer-sized particles to solve the problems in the prior art. Specifically, the present application mainly includes the following contents.

[0009] The dispersion method for preparing micrometer-sized particles provided by the present application comprises the step of dispersing by using a shear machine, wherein the shear machine comprises a tank body, a tank cover, a material injection port, a material discharge port and a shearing module, and the step comprises:

[0010] (1) injecting a dispersion medium into the shear machine tank body through the material injection port first, and starting shearing;

[0011] (2) injecting the dispersed phase and the dispersion medium in proportion, wherein the injection speed of the dispersed phase is 5 mL / min to 100 mL / min, and the injection speed of the dispersion medium is 1000 mL / min to 10000 mL / min;

[0012] (3) making the dispersed phase and the dispersion medium in the shear machine circulate and shear for more than three times, so as to obtain small-particle-size particles or emulsion droplets with a volume average diameter of 0.5-30 μm; and

[0013] (4) discharging the small-particle-size particles or emulsion droplets from the upper material discharge port under the action of fluid injection, and sinking the large-particle-size particles or emulsion droplets back to the tank bottom under the action of gravity to be sheared again by the shear machine.

[0014] In some embodiments, the dispersion method for preparing micrometer-sized particles according to the present application, wherein the rotation speed of the shear machine is controlled to be 4800-7700 rpm, so as to obtain particles or emulsion droplets with a volume average diameter of 22.51-27.26 μm.

[0015] In some embodiments, the dispersion method for preparing micrometer-sized particles according to the present application, wherein the material is continuously injected into the shear machine tank body from the material injection port, and the flow rate of the material discharge port is consistent with the flow rate of the material injection port.

[0016] In some embodiments, the dispersion method for preparing micron-sized particles according to the present application, wherein the volume of the continuous injection of the material is 2L-200L.

[0017] In some embodiments, the dispersion method for preparing micron-sized particles according to the present application, wherein the bottom of the tank is connected with a support frame, and the stability of the tank is maintained by the support frame.

[0018] In some embodiments, the dispersion method for preparing micron-sized particles according to the present application, wherein the viscosity ratio of the dispersed phase to the dispersion medium is in the range of 300-7500:1.

[0019] In some embodiments, the dispersion method for preparing micron-sized particles according to the present application, wherein the shear machine comprises a driving motor arranged at the upper part of the tank, a stator assembly arranged inside the tank, and a rotor assembly, the rotor assembly comprising a rotor connecting rod and rotor blades radially arranged at the end of the rotor connecting rod, the stator assembly comprising a stator and a stator connecting cover arranged on the upper surface of the stator, the rotor assembly being inside the stator assembly, the upper part of the rotor connecting rod being connected with the driving motor through the center of the tank cover, and the rotor blades being rotated by the driving motor for cyclic shearing.

[0020] In some embodiments, the dispersion method for preparing micron-sized particles according to the present application, wherein the tank and the tank cover are sealed by an O-ring, and the tank cover and the rotor connecting rod are sealed by a double-end mechanical seal.

[0021] In some embodiments, the dispersion method for preparing micron-sized particles according to the present application, wherein the shear machine further comprises a material injection pipe, the material injection pipe comprising an outer injection pipe and an inner injection pipe for the injection of the dispersion medium and the dispersed phase, respectively.

[0022] In some embodiments, the dispersion method for preparing micron-sized particles according to the present application, wherein a lifting machine is arranged at one side of the tank, the lifting machine being connected with the tank cover and being arranged to enable the lifting of the shear machine.

[0023] The dispersion method for preparing micrometer-sized particles of the present application is suitable for preparing products with different particle size ranges and more uniform particle size distribution. In particular, the increased tank volume and bottom feeding method can obtain small particle size particles with a volume average particle size of less than 30 μm without requiring extreme rotational speed, and can meet the needs of any desired scale from small test to large-scale production without the need to replace equipment, thereby solving the limitations of batch high-shear dispersion machines and pipeline high-shear dispersion machines and reducing the scale-up effect. The method is suitable for mixing two mutually immiscible media, and is particularly suitable for use at different temperatures, where the viscosity difference between the two phases is extremely large, resulting in uneven shear and poor particle morphology.

[0024] The emulsification effect is greatly enhanced in the exemplary method of the present application, and the viscosity ratio of the dispersed phase to the dispersion medium is in the range of 300-7500:1. At the same time, the high-speed shear machine must generate heat during use, although a jacketed temperature control method is often used in actual operation to avoid excessive heating of the material. However, for batch high-shear dispersion machines, the temperature control jacket cannot effectively reduce the material temperature during long-term operation, which is not conducive to the preparation of heat-sensitive materials. In addition to jacketed temperature control, the enlarged tank volume in the present application allows continuous injection of the dispersion medium and the dispersed phase during preparation, which can continuously update the liquid in the tank and timely remove the heat generated by the high-shear dispersion machine, thereby avoiding the problem of excessive heat generation and poor heat dissipation due to the small tank volume and long-term operation of the machine. The method has good applicability to the preparation of heat-sensitive materials and non-heat-sensitive materials.

[0025] In the exemplary method of the present application, the scale-up effect of batch high-shear dispersion machines can be avoided, and the problem of uneven dispersion of two-phase materials with large property differences can be solved for pipeline high-shear dispersion machines. The method can stably prepare extremely small particle size particles or emulsion droplets without requiring extreme rotational speed, greatly improving the uniformity of the product, and maintaining the uniform characteristics of the product from small-scale test to large-scale production, meeting the production of different batches and reducing the research and development cost. BRIEF DESCRIPTION OF DRAWINGS

[0026] Figure 1 Overall structure schematic diagram of the embodiment of the shear machine with the discharge port arranged at the top of the tank body.

[0027] Figure 2 Overall structure schematic diagram of the embodiment of the shear machine with the discharge port arranged at the top of the tank body.

[0028] Figure 3 Particle morphology prepared by using a pipeline high-shear dispersion machine with a rotational speed of 11000 rpm.

[0029] Figure 4 Particle morphology prepared by using a pipeline high-shear dispersion machine with a rotational speed of 15000 rpm.

[0030] Figure 5 Particle morphology prepared using a top-entry high shear disperser on a 2 L scale.

[0031] Figure 6 Particle morphology prepared using a top-entry high shear disperser on a 2 L scale.

[0032] Figure 7 Particle morphology prepared using a top-entry high shear disperser on a 10 L scale.

[0033] Figure 8 Particle morphology prepared using a top-entry high shear disperser on a 50 L scale.

[0034] Figure 9 Particle morphology prepared using a tank high speed shear on a 50 L scale.

[0035] Reference sign list:

[0036] 100. tank body; 200. tank cover; 300. stator assembly; 310. stator; 311. dispersion slot; 320. stator connecting cover; 400. rotor assembly; 410. rotor connecting rod; 420. rotor blade; 500. motor; 600. support frame; 710. outer injection pipe; 711. outer injection pipe outlet; 712, outer injection pipe inlet; 720, inner injection pipe; 721. inner injection pipe outlet; 722. inner injection pipe inlet; 810. top discharge outlet; 820. side upper discharge outlet; 900. temperature control jacket; 910. cooling inlet; 920. cooling outlet; 930. deflector; 1000. elevator. DETAILED DESCRIPTION

[0037] Various exemplary embodiments of the present application will now be described in detail, with reference to the figures. Such description, however, is to be considered as merely illustrative of certain aspects, features and embodiments of the present application, not as limitations to the scope of the present application.

[0038] It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the present application. Additionally, for a range of values of or statements concerning a value, it is contemplated that each intervening value, to the extent that such intervening values are associated with a property that can be used to describe an aspect of the application, and each smaller range of values bounded by such value that can be described by a limit range of values above and below the stated value are also contemplated. The same applies to every statement concerning a value or a range of values. These are only examples of what is provided by this application, and in no way serve to limit the true scope of this application, since the scope of the application is defined only by the appended claims.

[0039] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. Although preferred structures and materials are described, any structure and materials similar or equivalent to those described herein can be used in the practice or testing of the present application.

[0040] The terms first, second, third, etc. are used in the description and in the claims to indicate different elements similar to one another, and are not necessarily used to describe a sequential or chronological order. It should be understood that the terms so used are interchangeable under appropriate circumstances and that the embodiments of the application described herein are capable of operating in other sequences than described or illustrated herein.

[0041] In addition, the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", and the like in the description and claims indicate the orientation or positional relationship based on the orientation or positional relationship shown in the drawings, and are only for the convenience of describing the application and simplifying the description, and do not indicate or imply that the devices or elements referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore cannot be understood as limiting the application. It should be understood that the terms so used are interchangeable under appropriate circumstances and that the embodiments of the application described herein are capable of operating in other orientations than described or illustrated herein.

[0042] The term "fixed connection" of the present application includes detachable fixed connection or non-detachable fixed connection. The detachable fixed connection includes bolt connection and the like. The non-detachable fixed connection includes welding and the like.

[0043] Embodiments

[0044] The structure of an exemplary shear machine used in the dispersion method of the present embodiment is as follows:

[0045] As shown in Figure 1 , it is a tank type high-speed shear machine, which includes a tank body 100, a tank cover 200, a stator assembly 300, a rotor assembly 400, a driving motor 500, a material injection sleeve, and a material discharge port.

[0046] A seal is provided between the tank body 100 and the tank cover 200, which can be sealed by an O-ring seal or a packing seal. The tank cover 200 and the driving part of the shear machine use a mechanical seal, which effectively maintains the sealing of the shear machine and can achieve sterile production.

[0047] The tank body 100 has a diameter-height ratio of 0.6-0.9, and the volume of the tank body 100 is 1.5L-3L. Further, a support frame 600 is provided at the lower part of the tank body 100 to maintain the stability of the tank body 100.

[0048] Further, the shearing machine is provided with a lifting machine 1000 beside the shearing machine, and the lifting function can be realized through the lifting machine 1000, so that the operation and disassembly are facilitated.

[0049] Further, the temperature control jacket 900 is arranged outside the tank body 100, the lower part of the temperature control jacket 900 is provided with a cooling inlet 910, and the upper part is provided with a cooling outlet 920. The heat exchange of the partition type is realized by the input of cold or hot fluid, so that the temperature of the material in the tank body 100 is raised or lowered to meet the expected temperature. Preferably, a heat preservation layer is arranged outside the temperature control jacket 900. The heat preservation layer can be made of high-efficiency heat preservation materials, such as polyurethane foam and phenolic foam, which can provide good insulation and heat insulation effect while ensuring heat preservation performance.

[0050] Further, a plurality of guide plates 930 are arranged in the temperature control jacket 900 to prevent dead zones in the flow and make the heat transfer uniform, thereby improving the heat transfer efficiency. The number and shape of the guide plates 930 are arranged according to the needs, and the guide plates 930 are preferably arranged at the flow direction changing positions in the temperature control jacket 900.

[0051] A sleeve is arranged at the bottom center position of the tank body 100 for material injection, and a material discharge port is arranged at the top or upper side of the tank body 100 for material discharge. The top discharge port 810 is located at the top of the tank body 100 and is connected with the tank cover 200. The upper side discharge port 820 is located on the sidewall at the upper side of the tank body 100 and is connected with the tank body 100. The position of the material discharge port can be arranged according to the needs.

[0052] The material injection sleeve arranged at the bottom center position of the tank body 100 is divided into an outer injection pipe 710 and an inner injection pipe 720, which are respectively used for the injection of two-phase medium. The two ends of the inner injection pipe 720 and the outer injection pipe 710 are respectively liquid inlets and liquid outlets, and the liquid inlets and the liquid outlets of the inner injection pipe 720 and the outer injection pipe 710 are not communicated with each other. The inner injection pipe 720 is located at the bottom center of the tank body 100, and the diameter is preferably 3mm-6mm. The inner injection pipe liquid inlet 722 is arranged at the lower part of the tank body 100, and the inner injection pipe liquid outlet 721 is arranged inside the tank body 100 and is close to the inner side of the bottom wall of the tank body 100. The vertical distance is preferably 1-5cm, and further preferably 3cm. The inner injection pipe liquid outlet 721 is very close to the bottom surface of the stator 310 of the stator assembly, and the vertical distance is preferably 0.5cm-1cm, so that the material can be dispersed more uniformly. The outer injection pipe 710 is sleeved outside the inner injection pipe 720, and the two are vertically arranged and consistent with the center line of the tank body. The outer injection pipe liquid outlet 711 is flush with the inner side of the tank body bottom wall. Preferably, in order to make the feeding and discharging speeds consistent, the diameter of the material discharge port is the same as the diameter of the outer injection pipe 710.

[0053] The structure of the downward and upward movement utilizes the medium gravity to make the small particle size particles or emulsion droplets be discharged from the upper material outlet under the dynamic action, and the larger particle size particles or emulsion droplets sink back to the tank bottom under the gravity action, and are sucked into the rotor blade rotating at the shaft center under the strong centrifugal force of the shearing machine to be sheared again, so that the shearing is more sufficient and uniform, and the emulsification effect is enhanced. Meanwhile, since the dispersion medium and the dispersed phase are continuously injected, the liquid in the tank body is always renewed, and the problems of a large amount of heat generation due to the long-time operation of the high-speed shearing machine and poor heat dissipation are avoided.

[0054] The stator assembly 300 and the rotor assembly 400 are arranged on the vertical central axis inside the tank body, the rotor assembly 400 is arranged inside the stator assembly 300, the rotor assembly 400 includes a rotor connecting rod 410 and rotor blades 420, the rotor blades 420 are arranged at the bottom end of the rotor connecting rod 410 and are radially and uniformly distributed along the circumferential direction of the rotor connecting rod 410, the upper part of the rotor connecting rod 410 is connected with the driving motor 500, and the rotor blades 420 rotate under the driving of the driving motor 500 to perform shearing. The stator assembly 300 includes a stator 310 and a stator connecting cover 320, the stator connecting cover 320 is fixed to the upper end surface of the stator 310, the stator 310 is connected with the rotor connecting rod 410 through the stator connecting cover 320, the stator 310 is in a hollow cylindrical shape, and a plurality of dispersion grooves 311 are arranged on the stator 310 and used for medium dispersion.

[0055] When working, the motor 500 drives the rotor assembly 400 to rotate at a high speed, when the rotor assembly 400 in the shearing machine rotates at a high speed, a very strong negative pressure will be formed in the area around the rotor blades 420, and the material is continuously sucked in under the strong centrifugal force, so that the material is diffused from the center to the periphery, the negative pressure generated in the shearing machine helps the material to be sucked and transported, and when the rotating speed of the motor increases, the negative pressure gradually increases, so that the material can be more easily sucked from the liquid outlet of the inner injection pipe.

[0056] The dispersion method of the embodiment is as follows:

[0057] (1) First, the dispersion medium is injected into the shearing machine tank body 100 through the liquid outlet 711 of the outer injection pipe, after the tank body 100 is filled, the shearing is started;

[0058] (2) Then, the dispersed phase and the dispersion medium are injected in proportion, the injection speed of the dispersed phase can be 5 mL / min to 100 mL / min, and the injection speed of the dispersion medium can be 1000 mL / min to 10000 mL / min;

[0059] (3) The dispersed phase and the dispersion medium are subjected to more than three times of circulation shearing in the shearing machine, so that small particle size particles or emulsion droplets with a volume average diameter of 0.5-30 μm are obtained; and

[0060] (4) Small particle size particles or emulsion droplets are discharged from the upper material outlet under the fluid injection power, and large particle size particles or emulsion droplets sink back to the tank bottom under the action of gravity and are sheared again by the shear machine.

[0061] In the third step:

[0062] The shear dispersion process of the material in the tank body mainly includes three shear processes, and the three shear processes are repeatedly circulated until the particle size is sufficiently dispersed and refined and discharged out of the tank.

[0063] The first shear process: when the dispersion starts, the material enters the tank body from the feed port, and under the action of strong centrifugal force, a very strong vortex is formed in the rotor blade 420 area. The generation of the vortex enhances the collision and friction between the dispersed phase and the dispersion medium in the material, which is beneficial to the further mixing and dispersion of the material, and the material diffuses from the rotor blade 420 area to the gap between the stator and the rotor.

[0064] The second shear process: under the action of strong centrifugal force, the material is thrown into the gap between the stator and the rotor along the radial direction from the rotor blade 420 area. The gap between the stator and the rotor is the main area where shear occurs. A large number of vortices exist therein, and at the same time, the material is subjected to forces such as centrifugal extrusion and impact, so that the material is further dispersed and mixed. In the gap between the stator and the rotor, the medium is subjected to the shearing action of the high-speed rotating rotor blade, and the particle medium rapidly collides and breaks. In the entire gap between the stator and the rotor, the material can be quickly mixed and dispersed uniformly under the combined action of strong shear stress and turbulent stress, achieving better mixing and dispersion effect.

[0065] The third shear process: the material is continuously ejected from the rotor blade 420 at high speed, part of which is ejected outside the stator 310. The smaller particles or emulsion droplets are discharged from the upper material outlet under the continuous fluid injection power, and the larger particles or emulsion droplets sink back to the tank bottom under the action of gravity and are continuously rolled into the rotor blade at the shaft center under the action of strong centrifugal force of the shear machine for shearing again. Because a certain velocity gradient is generated in the radial direction, according to Bernoulli's theorem, the pressure and velocity in the fluid are related, that is, the faster the velocity, the smaller the pressure, and the slower the velocity, the greater the pressure. At this time, because the speed in the stator 310 is fast, the pressure is small, and the speed outside the stator 310 is slow, so the pressure is large. The pressure difference will push the material to flow from the outside to the inside of the stator 310, and the backflow and suction phenomenon occurs. The medium backflowing and suctioning into the stator 310 from the tank body 100 and the medium continuously suctioned from the rotor blade 420 area converge in the gap between the stator and the rotor, forming multiple strong turbulent flows, which are continuously circulated and sheared. After several cycles of shear, the dispersion and homogenization process is completed.

[0066] After several cycles of shearing process, the medium is fully sheared, and the particle size distribution is more uniform. In particular, the increased tank volume and bottom feeding method make the shearing more sufficient, and without the need for extreme speed, small particle size particles with a volume average diameter range of 0.5-30 μm can be obtained, and without the need to replace the equipment, the demand from small test to large production scale can be met, and the limitations of batch type high shear dispersion machine and pipeline type high shear dispersion machine are solved.

[0067] Test Example

[0068] 1. Relationship between motor speed and particle size when preparing extremely small particle size particles by tank type high speed shear machine

[0069] First, fill the tank with the dispersion medium, and inject the dispersed phase and the dispersion medium through the inner injection pipe and the outer injection pipe in a certain proportion. Under the condition that other conditions remain unchanged, the target product is prepared by changing the speed of the tank type high speed shear machine. The particle size of the product is measured by a laser particle size analyzer.

[0070] Table 1

[0071]

[0072] According to the research data of Test Example 1, it can be known that the size of the particles can be adjusted by adjusting the speed, and the particle size decreases as the speed increases. The span is smaller than that of the pipeline type online homogenizer and the top-mounted high speed shear machine, and the particle size is more uniform.

[0073] 2. Relationship between material injection speed and particle size when preparing extremely small particle size particles by tank type high speed shear machine

[0074] First, fill the tank with the dispersion medium, and inject the dispersed phase and the dispersion medium through the inner injection pipe and the outer injection pipe in a certain proportion. Under the condition that other conditions remain unchanged, the target product is prepared by changing the speed of the tank type high speed shear machine. The particle size of the product is measured by a laser particle size analyzer.

[0075] Table 2

[0076]

[0077]

[0078] According to the results of Test Example 2, increasing the flow rate of the two phases has no significant effect on the particle size of the prepared product, and the particle size of the product under different flow rates is basically consistent

[0079] 3. Relationship between medium injection time and particle size when preparing extremely small particle size particles by tank type high speed shear machine

[0080] Preparation stability of the device at different scales. First, fill the tank with the dispersion medium, and inject the dispersion phase and the dispersion medium through the inner injection pipe and the outer injection pipe, respectively, at a certain ratio. Different scales correspond to different material quantities, and other process conditions remain unchanged. Prolong the injection time of the two phases to obtain products prepared at different scales. Use a laser particle size analyzer to measure the particle size of the products.

[0081] Table 3

[0082]

[0083] From the particle size results of Test Example 3, it can be seen that the particle size of the product prepared using the tank-type high-speed shearing machine is almost consistent, Figure 9 The scanning electron microscope image of the product prepared at a scale of 50L shows that the prepared particles have high roundness and good morphology. The tank-type high-speed shearing machine used in this application uses the initial volume as a template (2L in the test example), and by running for different lengths of time, different scales of materials can be continuously prepared, meeting the production batch of 2L-200L and larger scales. Economically and efficiently, the small test is expanded to the production scale, and consistent material properties can be obtained, reducing the amplification effect and reducing the research and development cost.

[0084] Comparative Example 1

[0085] This comparative example is to prepare micron-sized particles using a single shearing of a pipeline high-shear dispersion machine. The pipeline high-shear dispersion machine is used to prepare micron-sized particles, and the rotational speed is set to 11000 rpm, 15000 rpm, and 18000 rpm, respectively, to investigate the particle size and morphology of the particles prepared at different rotational speeds.

[0086] Table 4

[0087]

[0088]

[0089] From the research data of Comparative Example 1, it can be seen that as the shearing speed increases from 11000 rpm to 18000 rpm, the particle size of the prepared particles does not effectively decrease, the particle size span (Span) is wide, and the particle size distribution is not uniform. From Figures 3-5 It can be seen that the morphology of the particles does not become closer to spherical with the increase of the shearing speed, which does not meet the preparation target. On the other hand, 18000 rpm is close to the upper limit of the rotational speed of the pipeline high-shear dispersion machine used in this experiment, and long-time operation is not conducive to the service life and maintenance of the equipment.

[0090] Comparative Example 2

[0091] The comparative example is to prepare micron-sized particles using a top-mounted high-shear dispersion machine. The top-mounted high-shear dispersion machine equipment is used, and the bottom injection material is used, and by changing the volume of the tank, particles of different scales are prepared to investigate the feasibility of proportional scaling. The top-mounted high-shear dispersion machine equipment (rotor diameter 38 mm).

[0092] Table 5

[0093]

[0094] According to the particle size data of Comparative Example 2, the volume average diameter of the particles prepared at the scale of 2L-10L is less than 20 μm, and when the scale is increased to 50L, the D50 and D90 particle sizes increase significantly, indicating that the shear machine is not suitable for the current scale, and the equipment needs to be replaced and the process parameters need to be adjusted. On the other hand, from the particle size data of Comparative Example 3, it can be seen that the particles prepared at the scale of 2L have high roundness and good morphology, and a large number of strips appear at the scale of 10L-50L. The process has a scaling effect, and particles of different morphologies may affect product quality, so the use of top-mounted high-speed shear machines has the limitation of scaling effect. Figures 6-8

[0095] In summary, the dispersion method for preparing micron-sized particles proposed in the present application can avoid the scaling effect of batch high-shear dispersion machines, and improve the problem that the pipeline high-shear dispersion machine cannot disperse uniformly when the properties of the two phases are greatly different. Without extreme speed, it can stably prepare particles or emulsion droplets with extremely small particle size, greatly improve the uniformity of the product, and can maintain the uniformity of the product from small-scale test to large-scale production, meet different batch production, and reduce research and development costs.

[0096] Although the present application has been described with reference to exemplary embodiments, it is to be understood that the application is not limited to the disclosed exemplary embodiments. Various adjustments or changes can be made to the exemplary embodiments of the present application without departing from the scope or spirit of the present application. The scope of the claims should be based on the broadest interpretation to encompass all modifications and equivalent structures and functions.​

Claims

1. A pot-type high-speed shearing machine characterized by comprising: The shearing machine comprises a tank body (100), a tank cover (200), a material injection port, a material discharge port, a driving motor (500) and a shearing module, wherein the driving motor (500) is arranged on the upper portion of the tank body (100), the stator assembly and the rotor assembly are arranged inside the tank body (100).

2. A tank-type high-speed shearing machine according to claim 1, characterized in that, The rotor assembly comprises a rotor connecting rod (410) and rotor blades (420) which are radially and uniformly arranged on the end of the rotor connecting rod (410), and the stator assembly comprises a stator (310) and a stator connecting cover (320) arranged on the upper surface of the stator, wherein the rotor assembly is arranged inside the stator assembly.

3. A tank-type high-speed shearing machine according to claim 2, wherein The upper portion of the rotor connecting rod (410) penetrates through the center of the tank cover (200) and is connected with the driving motor (500), and the driving motor (500) drives the rotation of the rotor blades (420).

4. A tank-type high-speed shearing machine according to claim 3, wherein The tank body (100) and the tank cover (200) are sealed by an O-ring, and the tank cover (200) and the rotor connecting rod (410) are sealed by a double-end mechanical seal.

5. A tank-type high-speed shearing machine according to any one of claims 1 to 4, characterized in that, A sleeve is arranged at the central position of the bottom of the tank body (100) for material injection, and a top discharge port (810) or a side upper discharge port (820) is arranged at the top or the upper side of the tank body (100) for material discharge.

6. A tank-type high-speed shearing machine according to claim 5, wherein The sleeve is divided into an outer injection pipe (710) and an inner injection pipe (720), wherein the two ends of the inner injection pipe (720) and the outer injection pipe (710) are liquid inlet and liquid outlet, respectively, and the liquid inlet and the liquid outlet of the inner injection pipe (720) and the outer injection pipe (710) are not communicated with each other; the outer injection pipe (710) is sleeved outside the inner injection pipe (720), and the two are vertically arranged and consistent with the center line of the tank body (100), and the liquid outlet (711) of the outer injection pipe is flush with the inner side of the bottom wall of the tank body (100); preferably, the diameter of the top discharge port (810) or the side upper discharge port (820) is the same as the diameter of the outer injection pipe (710).

7. A tank-type high-speed shearing machine according to claim 6, characterized in that, The inner injection pipe (720) is located at the central position of the bottom of the tank body (100), and the diameter is preferably 3mm-6mm; the liquid inlet (722) of the inner injection pipe is arranged at the lower portion of the tank body (100), and the liquid outlet (721) of the inner injection pipe is arranged inside the tank body (100), and the vertical distance between the liquid outlet (721) and the bottom surface of the stator (310) of the stator assembly is preferably 1cm-5cm; the vertical distance between the liquid outlet (721) of the inner injection pipe and the bottom surface of the stator (310) of the stator assembly is preferably 0.5cm-1cm.

8. A tank-type high-speed shearing machine according to any one of claims 1 to 7, characterized in that, The bottom of the tank body (100) is connected with a support frame (600) to keep the stability of the tank body (100).

9. A tank-type high-speed shearing machine according to any one of claims 1 to 7, characterized in that, A lifter (1000) is arranged on one side of the tank body (100), and the lifter (1000) is connected with the tank cover (200) and is arranged to enable the shearing machine to be lifted.

10. A tank-type high-speed shearing machine according to any one of claims 1 to 7, characterized in that, The ratio of diameter to height of the tank body (100) is 0.6-0.9, and the volume of the tank body (100) is 1.5L-3L; further, the tank body (100) is externally provided with a temperature control jacket (900), the lower part of the temperature control jacket (900) is provided with a cooling inlet (910), and the upper part is provided with a cooling outlet (920); preferably, the temperature control jacket (900) is externally provided with a thermal insulation layer, and the thermal insulation layer can adopt high-efficiency thermal insulation materials.

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