A device and method for preparing microspheres of selectively solubilized substances

Abstract

This invention provides an apparatus and method for preparing selectively soluble microspheres, where the compound microspheres are readily soluble in a first solvent, substantially insoluble in a second solvent, and the first and second solvents are miscible. The main functional modules of the apparatus include: a real-time particle size detection module, a microsphere-liquid separation module, a concentration titration module, a centrifugal differential spheroidizing module, and a microsphere drying and separation module. This apparatus can separate the spheroidized compound and polymer materials, ensuring high sphericity of the compounds and polymer materials, preventing microsphere adhesion, and maintaining the dispersion of the compound microspheres. Simultaneously, the solvent and titration system are recycled to ensure that the particle size of the compound microspheres gradually decreases.

Description

Technical Field

[0001] This invention relates to the field of porous material preparation, and more specifically, to an apparatus and method for preparing selectively soluble microspheres. Background Technology

[0002] During crystallization, since dendrite growth is mostly along the direction of least crystallization resistance, the resulting crystals are often non-circular. This conflict between crystallization habit and morphology makes anisotropic crystallization the biggest obstacle to sphericity. Sphericification of crystals can significantly improve flowability and dispersibility. For example, the flowability index of microspheres with a sphericity >0.9 increases by 3-5 times. In addition, the release behavior of spherical microspheres is more controllable, and reducing the sharp edges of microspheres can effectively prevent breakage and thus increase mechanical stability. Current microsphere preparation processes generally struggle to achieve high sphericity, narrow particle size distribution, and process stability. Specifically, current microsphere processes use emulsion or microemulsion methods, dispersing ionic compound solutions into spherical droplets through a water-in-oil system before solidification. The drawback of this method is that aqueous droplets tend to aggregate and undergo Ostwald ripening in the continuous phase, resulting in poor sphericity and a wide particle size distribution. Strongly polar non-aqueous solvents are required, but solvent residue is difficult to control and is costly. Spray drying rapidly evaporates the solvent to form spherical particles. However, the rapid evaporation of the solvent during spray drying induces internal stress, resulting in dents and cracks. The sphericity is often <0.7. These microcracks absorb moisture during storage, leading to deliquescence and morphological collapse. Current methods to reduce the particle size of compound microspheres by decreasing the solution concentration are problematic. When a low-concentration liquid is introduced into a high-concentration liquid, the compound microspheres in the localized area of ​​the low-concentration liquid become too small or even dissolve due to the lower concentration of the surrounding solvent. Furthermore, current microsphere preparation processes lack effective means for online monitoring of microsphere sphericity, relying on offline electron microscopy sampling, which makes real-time feedback control difficult.

[0003] To address the aforementioned issues, there is a need for a device and method for preparing selectively soluble microspheres, which would reduce the problem of excessively low local solvent concentration, allow for solvent recycling, achieve high sphericity of compounds and polymers, enable the separation of spheric compounds and polymers, and allow for real-time feedback control of the sphericity of the microspheres. Summary of the Invention

[0004] The purpose of this invention is to provide an apparatus and method for preparing selectively soluble microspheres, which can separate spheroidized compounds and polymers, ensuring high sphericity of the compounds and polymers, preventing the microspheres from sticking together and ensuring their dispersibility, while recycling the solvent and titration system to ensure that the particle size of the microspheres gradually decreases.

[0005] The present invention provides an apparatus and method for preparing selectively soluble microspheres, the technical solution of which is as follows: The main functional modules of the device include: a real-time particle size detection module, a microsphere-liquid separation module, a concentration titration module, a centrifugal differential spheroidizing module, and a microsphere drying and separation module. The real-time particle size detection module is used to detect the particle size of the compound microspheres after grinding. The microsphere-liquid separation module is used to separate the concentrated liquid containing the compound microspheres from the clear liquid without the compound microspheres. The concentration titration module reduces the problem of local low solvent concentration by titrating a very small amount of two solvents and compound microspheres and by rapid stirring. The centrifugal differential spheroidizing module is used to grind the compound microspheres to achieve the set sphericity. The microsphere drying and separation module is used to dry and separate the ground compound microspheres.

[0006] The concentration titration module is used to titrate a mixture of a first solvent, a second solvent, and compound microspheres. The first solvent and the second solvent are miscible, and the compound microspheres are readily soluble in the first solvent but practically insoluble in the second solvent. The concentration titration module includes a low-boiling-point burette, a high-boiling-point burette, a stirring power source, a stirrer, a titration inlet, a titration outlet, a shut-off valve, a second peristaltic pump, and a second pump output pipe. The solution of solvent and compound microspheres entering through the low-boiling-point burette, the high-boiling-point burette, and the titration inlet is stirred by the stirrer and then flows out from the titration outlet. The concentration titration module titrates a very small amount of the two solvents and compound microspheres with rapid stirring by the stirrer. The concentration titration module can reduce the problem that when a low-concentration liquid enters a high-concentration liquid, the compound microspheres in the local area of ​​the low-concentration liquid become too small or even dissolve due to the low concentration of the surrounding solvent.

[0007] The centrifugal differential rounding module is connected to the concentration titration module via a second pump output pipe. The centrifugal differential rounding module is a device that uses centrifugal force to grind compound microspheres. It includes a rounding inlet, a horizontal spiral rounding tube, a vertical spiral rounding tube, and a rounding outlet. The solution containing the compound microspheres enters the horizontal spiral rounding tube through the rounding inlet. After being ground in the horizontal spiral rounding tube, the compound microspheres enter the vertical spiral rounding tube, where they are also ground. The ground compound microspheres and solution flow together into the rounding outlet. Current microsphere processes use emulsion or microemulsion methods. The method of dispersing ionic compound solutions into spherical droplets and then solidifying them in an oil-in-water system has the drawbacks of easy aggregation and Ostwald ripening of aqueous droplets in the continuous phase, poor sphericity and wide particle size distribution in emulsion or microemulsion methods, and the need to use highly polar non-aqueous solvents, but solvent residue is difficult to control and costly. However, the sphericity of compound microspheres created by centrifugal differential spheroidizing modules can significantly improve flowability and dispersibility. For example, the flowability index of microspheres with a sphericity >0.9 is increased by 3-5 times. In addition, the release behavior of spherical microspheres is more controllable, and reducing the sharp edges of microspheres can also effectively avoid breakage and thus increase mechanical stability.

[0008] The real-time particle size detection module is connected to the rounding outlet of the centrifugal differential rounding module via the detection inlet pipe. In the current microsphere preparation process, there is a lack of effective means for online monitoring of the roundness of microspheres. The real-time particle size detection module is used to detect the particle size of compound microspheres after grinding. The real-time particle size detection module includes a laser emitter, a diffractometer, a transmission lens, a dispersion chamber, a dispersion outlet, a dispersion inlet, a diffraction light receiver, a detection inlet pipe, and a detection outlet pipe. The compound microspheres and solution enter the dispersion inlet through the detection inlet pipe, and then enter the dispersion chamber through the dispersion inlet. The compound microspheres are irradiated by the laser emitter to the diffraction light receiver to measure the particle size. The solution containing the compound microspheres then flows out through the dispersion outlet.

[0009] The ball-liquid separation module is connected to the real-time particle size detection module via the outlet pipe after detection. The ball-liquid separation module is a device for separating concentrated liquid containing compound microspheres and clear liquid without compound microspheres. The ball-liquid separation module includes a hydrocyclone separator, a hydrocyclone separator inlet, a clear liquid outlet, a concentrated liquid outlet, a three-way reversing valve, a circulation pipe, a finished product pipe, and a first peristaltic pump. The solution containing compound microspheres flows into the hydrocyclone separator from below through the outlet pipe after detection. In the hydrocyclone separator, centrifugation is used to separate the concentrated liquid containing compound microspheres from the clear liquid without compound microspheres. The clear liquid without compound microspheres has a lower density and enters the clear liquid outlet, while the concentrated liquid containing compound microspheres has a higher density and enters the concentrated liquid outlet. The concentrated liquid containing compound microspheres that has not been properly ground enters the centrifugal differential rounding module through the circulation pipe under the action of the three-way reversing valve for further grinding. The ground liquid enters the finished product pipe under the action of the three-way reversing valve.

[0010] The microsphere drying and separation module is connected to the microsphere-liquid separation module via a finished product pipe. This module is used to dry and separate the polished compound microspheres. It includes a dryer, dryer inlet, ductwork, mixed steam outlet, mixed steam pipe, ball-spinning disc, hot air inlet, baffle plate, distributor, high-boiling-point condenser, high-boiling-point gas pipe, and low-boiling-point condenser. Air from the ductwork outlet causes the ball-spinning disc to rotate. Three hot air inlets are located at the bottom of the dryer; hot air from these inlets vaporizes the concentrated liquid flowing onto the ball-spinning disc, leaving the liquid remaining. The compound microspheres fall into the dryer. The vaporized steam exits through the mixed steam outlet located at the top of the dryer shell and enters the mixed steam pipe. The mixed steam pipe is connected to the dryer through the mixed steam outlet. After the vaporized steam enters the mixed steam pipe, the high-boiling-point steam condenses in the high-boiling-point condenser and enters the high-boiling-point liquid burette on the high-boiling-point condenser. The low-boiling-point steam condenses in the low-boiling-point condenser and enters the low-boiling-point liquid burette on the low-boiling-point condenser. The microsphere drying and separation module is connected to the concentration titration module through the low-boiling-point liquid burette and the high-boiling-point liquid burette.

[0011] The working process of the device includes the following steps: (1) The compound microspheres, and the first solvent in which the compound microspheres are easily soluble and the second solvent which are essentially insoluble, are titrated into the concentration titration module under the condition that the first solvent and the second solvent are miscible. The stirring is driven by a stirring power source to mix the compound microspheres and the two solvents to form a solution, and the mixed solution flows into the titration outlet; (2) The mixed solution flows from the titration outlet into the rounding inlet of the centrifugal differential rounding module through the second pump output pipe under the action of the second peristaltic pump. The mixed solution enters the horizontal spiral rounding tube from the rounding inlet. The compound microspheres are polished in the horizontal spiral rounding tube and then enter the vertical spiral rounding tube. The compound microspheres are also polished in the vertical spiral rounding tube. The polished compound microspheres and the solution flow into the rounding outlet together. (3) The polished compound microspheres flow into the detection inlet pipe from the rounding outlet along with the mixed solution. The polished compound microspheres flow into the dispersion inlet of the particle size real-time detection module through the detection inlet pipe along with the mixed solution. Then they flow downward into the dispersion chamber. Under the illumination of the laser emitter, the polished compound microspheres are monitored by the diffraction light receiver to see if they meet the requirements. Then the compound microspheres flow into the detection outlet pipe from the dispersion outlet along with the mixed solution. (4) The solution containing the polished compound microspheres flows into the hydrocyclone separator through the outlet pipe after detection. Under the action of centrifugal force in the hydrocyclone separator, the solution containing the polished compound microspheres is divided into a concentrated liquid containing compound microspheres and a clear liquid without compound microspheres. The clear liquid without compound microspheres enters the clear liquid outlet, and the concentrated liquid containing compound microspheres enters the concentrated liquid outlet. The solution entering the clear liquid outlet enters the concentration titration module through the titration inlet to participate in the next mixing. The solution containing compound microspheres entering the concentrated liquid outlet is driven by the first peristaltic pump. The polished compound microspheres are carried by the solution through the three-way reversing valve into the finished product pipe, and the unpolished compound microspheres are carried by the solution through the circulation pipe and polished again in the centrifugal differential rolling module. (5) After the solution containing the compound microspheres enters the finished product tube, it enters the dryer inlet of the microsphere drying and separation module. The solution containing the compound microspheres falls from the dryer inlet along the distributor onto the ball-spinning plate. Under the action of the air duct, the ball-spinning plate rotates. The hot air blown out through the drying hot air inlet vaporizes the solution containing the compound microspheres. The compound microspheres fall into the bottom of the dryer and are collected. The vaporized solution vapor enters the mixed vapor outlet. The high-boiling-point solvent vapor condenses in the high-boiling-point condenser and enters the high-boiling-point liquid burette. The low-boiling-point solvent vapor condenses in the low-boiling-point condenser and enters the low-boiling-point liquid burette. The condensed solvent enters the concentration titration module to participate in the next mixing. At this point, one cycle ends.

[0012] Compared with the prior art, the beneficial effects of the present invention are: 1. The technical solution of this invention can reduce the formation of excessively low solvent concentrations in local areas, thereby preventing the problem of excessively small particle size or even dissolution of compound microspheres due to a sudden drop in local concentration. In current methods of reducing solution concentration to reduce the particle size of compound microspheres, when a low-concentration liquid enters a high-concentration liquid, the compound microspheres existing in the local area where the low-concentration liquid is located will become too small or even dissolve due to the low concentration of the surrounding solvent. The concentration titration module of this invention reduces the formation of excessively low solvent concentrations in local areas by titrating and mixing a very small amount of two solvents and compound microspheres with an external stirrer for rapid stirring.

[0013] 2. The technical solution of this invention can achieve high sphericity of compound microspheres. Horizontal and vertical spiral rolling tubes can perform all-around grinding of the compound microspheres. When the solution flow rate is the same, the linear velocity of the solution relative to the center of the device in the tube is the same. At this time, the centrifugal force varies at different radii. This difference in centrifugal force leads to differences in the friction points between the compound microspheres and the tube wall, as well as differences in the friction points between different compound microspheres. This continuous friction process at different points ensures that the compound microspheres are continuously subjected to uniform and appropriate tangential and normal grinding. The surface edges of the compound microspheres are gradually eliminated, resulting in the compound microspheres achieving the desired sphericity. Current microsphere manufacturing processes... The emulsion or microemulsion method used in traditional processes disperses ionic compound solutions into spherical droplets through a water-in-oil system and then solidifies them. The drawbacks of this method are that the aqueous droplets are prone to aggregation and Ostwald ripening in the continuous phase. The emulsion or microemulsion method results in poor sphericity and a wide particle size distribution. The solvent must be a strongly polar non-aqueous solvent, but solvent residue is difficult to control and the cost is high. However, the sphericity of the compound microspheres created by the centrifugal differential sphericization module of this invention can significantly improve the flowability and dispersibility. For example, the flowability index of microspheres with a sphericity >0.9 is increased by 3-5 times. In addition, the release behavior of spherical microspheres is more controllable, and reducing the sharp edges of the microspheres can also effectively avoid breakage and thus increase mechanical stability.

[0014] 3. The technical solution of the present invention can recycle the solvent and titration system. The particle size of the compound microspheres after grinding is detected in real time by the particle size detection module. The insufficiently ground compound microspheres are returned to the concentration titration module to participate in the next cycle of grinding by the ball-liquid separation module, so as to ensure that the particle size of the compound microspheres gradually decreases.

[0015] 4. The technical solution of the present invention can monitor and control the roundness of microspheres online and in real time. In the current microsphere preparation process, there is a lack of effective means for online monitoring of the roundness of microspheres, which relies on offline electron microscopy sampling and is difficult to achieve real-time feedback control. The present invention uses a laser emitter to irradiate the compound microspheres to a diffraction light receiver, which can monitor the roundness of microspheres online and control them in real time.

[0016] 5. The technical solution of the present invention can achieve non-aggregation of compound microspheres, good separation of phases, and continuous production. The present invention adopts a microsphere drying and separation module. The drying hot air inlet ensures that the compound microspheres gradually lose moisture during rolling. The microsphere drying and separation module ensures that the compound microspheres do not stick together. The drying under the support of the hot air inlet ensures the dispersibility of the compound microspheres. The mixing steam pipe can export the two solvents in the form of steam after drying, so that the two solvents can be recycled to ensure continuous production. Attached Figure Description

[0017] Figure 1 This is a schematic diagram of the overall structure of the device; Figure 2 This is a front view of the device; Figure 3 This is a schematic diagram of the real-time particle size detection module; Figure 4 This is a schematic diagram of the concentration titration module; Figure 5 This is a front view of the centrifugal differential rolling module; Figure 6 This is a cross-sectional view of the centrifugal differential rolling module; Figure 7 This is a schematic diagram of the microsphere drying and separation module. Detailed Implementation

[0018] like Figure 1-7 As shown, the present invention provides a device for preparing selectively soluble microspheres, and the technical solution adopted is as follows: Using potassium nitrate (KNO3) microspheres as compound microsphere 045, deionized water as the first solvent, and anhydrous ethanol as the second solvent as an example, potassium nitrate microsphere 045 was prepared. Under standard conditions of 25℃, the solubility of potassium nitrate microsphere 045 in deionized water was 31.6 g / 100 mL, and the solubility of potassium nitrate microsphere 045 in anhydrous ethanol was 0.03 g / 100 mL. Deionized water and anhydrous ethanol are a polar-weakly polar miscible system, and the two can be completely miscible at any volume ratio.

[0019] The main functional modules of the device include: a real-time particle size detection module 01, a microsphere-liquid separation module 02, a concentration titration module 03, a centrifugal differential spheroidizing module 04, and a microsphere drying and separation module 05. The real-time particle size detection module 01 is used to detect the particle size of potassium nitrate microspheres 045 after grinding. The microsphere-liquid separation module 02 is used to separate the concentrated liquid containing potassium nitrate microspheres 045 and the clear liquid without potassium nitrate microspheres 045. The concentration titration module 03 reduces the problem of local low solvent concentration by titrating and mixing a very small amount of deionized water, anhydrous ethanol and potassium nitrate microspheres 045 and by rapid stirring. The centrifugal differential spheroidizing module 04 is used to grind potassium nitrate microspheres 045 to obtain the set sphericity. The microsphere drying and separation module 05 is used to dry and separate the ground potassium nitrate microspheres 045.

[0020] The concentration titration module 03 titrates and rapidly stirs a very small amount of deionized water, anhydrous ethanol, and potassium nitrate microspheres 045. After mixing, the mixture enters the centrifugal differential spheroidizing module 04, where centrifugal force is used to grind the potassium nitrate microspheres 045. The ground potassium nitrate microspheres 045 then enter the particle size real-time detection module 01 to detect the particle size. After that, they enter the sphere-liquid separation module 02 to separate the concentrated liquid containing potassium nitrate microspheres 045 and the clear liquid without potassium nitrate microspheres 045. The concentrated liquid containing potassium nitrate microspheres 045 enters the microsphere drying and separation module 05 for drying, thereby obtaining potassium nitrate microspheres 045.

[0021] like Figure 4As shown, in the above scheme, the low-boiling-point liquid burette 031, the high-boiling-point liquid burette 032, the stirring power source 033, the stirrer 034, the titration inlet 035, the titration outlet 036, the shut-off valve 037, the second peristaltic pump 038, and the second pump output pipe 039 together constitute the concentration titration module 03. The concentration titration module 03 titrates the mixture of deionized water, anhydrous ethanol, and potassium nitrate microspheres 045 in small increments at a titration rate of 2-5 mL / min, with each titration volume being 1 / 3 of the total system volume. %~2%, the low-boiling-point liquid burette 031 and the high-boiling-point liquid burette 032 are placed vertically at the same height. The stirring power source 033 and the lower end of the low-boiling-point liquid burette 031 are located on the same horizontal plane. The stirring power source 033 is connected to the stirrer 034, which is located inside the housing directly below the stirring power source 033. The titration inlet 035 is placed horizontally to the left of the high-boiling-point liquid burette 032. The titration inlet 035 is located at the upper part of the housing. The titration inlet 035 and the low-boiling-point liquid burette 031 and... The high-boiling-point burette 032 is located on the same vertical plane. The titration outlet 036 is placed horizontally to the right of the low-boiling-point burette 031. The titration outlet 036 is located at the bottom of the housing. The titration outlet 036, the low-boiling-point burette 031, and the high-boiling-point burette 032 are all on the same vertical plane. The shut-off valve 037 is installed on the titration outlet 036 outside the housing. Deionized water, anhydrous ethanol, and nitric acid enter through the low-boiling-point burette 031, the high-boiling-point burette 032, and the titration inlet 035. The solution of potassium microspheres 045 is stirred by stirrer 034 and then flows out from titration outlet 036. The concentration titration module 03 titrates a very small amount of deionized water, anhydrous ethanol and potassium nitrate microspheres 045 with the stirrer 034 stirring rapidly. The concentration titration module 03 can reduce the problem that when a low concentration liquid enters a high concentration liquid, the potassium nitrate microspheres 045 in the local area where the low concentration liquid is located will become too small or even dissolve due to the low concentration of the surrounding solvent.

[0022] like Figure 5 , Figure 6As shown, the centrifugal differential rounding module 04 is connected to the concentration titration module 03 via the second pump output pipe 039. The centrifugal differential rounding module 04 is a device that uses centrifugal force to grind potassium nitrate microspheres 045. The rounding inlet 041, the horizontal spiral rounding tube 042, the vertical spiral rounding tube 043, the rounding outlet 044, and the potassium nitrate microspheres 045 constitute the centrifugal differential rounding module 04. The rounding inlet 041 is directly connected to the second pump output pipe 039. The solution containing potassium nitrate microspheres 045 enters the horizontal spiral rounding tube through the rounding inlet 041. In tube 042, under the condition of a constant solution flow rate, the linear velocity of the solution relative to the center of the device is the same. At this time, the centrifugal force varies at different radii. This difference in centrifugal force leads to differences in the friction points between the potassium nitrate microspheres 045 and the wall of the horizontal spiral rolling tube 042, as well as differences in the friction points between different potassium nitrate microspheres 045. This continuous friction process at different points causes the potassium nitrate microspheres 045 to be continuously subjected to uniform and moderate tangential and normal grinding. The surface edges of the potassium nitrate microspheres 045 are gradually eliminated, resulting in the potassium nitrate microspheres 045 being able to obtain... To achieve the desired sphericity, potassium nitrate microspheres 045 are polished in a horizontal spiral rolling tube 042 and then enter a vertical spiral rolling tube 043. The microspheres 045 undergo similar polishing in the vertical spiral rolling tube 043. The horizontal and vertical spiral rolling tubes 042 together form a spherical polishing device. The polished potassium nitrate microspheres 045 and the solution flow together into the rolling outlet 044. Current microsphere technology uses an emulsion or microemulsion method, dispersing the ionic compound solution into spherical droplets through a water-in-oil system before solidification. The drawbacks of this method are that aqueous droplets tend to aggregate and undergo Ostwald ripening in the continuous phase. Emulsion or microemulsion methods result in poor sphericity and wide particle size distribution. Strongly polar non-aqueous solvents are required, but solvent residues are difficult to control and are costly. However, the sphericity of potassium nitrate microspheres 045 created by the centrifugal differential sphericization module 04 can significantly improve flowability and dispersibility. For example, the flowability index of microspheres with a sphericity >0.9 is increased by 3-5 times. In addition, the release behavior of spherical microspheres is more controllable, and reducing the sharp edges of microspheres can effectively prevent breakage and thus increase mechanical stability.

[0023] like Figure 3As shown, the real-time particle size detection module 01 is used to detect the particle size of potassium nitrate microspheres 045 after grinding. The real-time particle size detection module 01 is connected to the rounding outlet 044 of the centrifugal differential rounding module 04 through the detection inlet pipe 018. The laser emitter 011, diffractor 012, transmission lens 013, dispersion tank 014, dispersion outlet 015, dispersion inlet 016, diffraction light receiver 017, detection inlet pipe 018, and detection outlet pipe 019 constitute the real-time particle size detection module 01. Potassium nitrate microspheres 045 and solution enter the dispersion inlet 016 through the detection inlet pipe 018. The diffractor 012 is directly connected to the detection inlet pipe 018 and is located directly below the detection inlet pipe 018. The dispersion inlet 016 and the dispersion outlet 019 are connected to the detection inlet pipe 018. The dispersion outlet 015 is located above and below the interior of the diffractor 012. The transmission lens 013 and the dispersion chamber 014 are vertically placed between the dispersion outlet 015 and the dispersion inlet 016. The dispersion chamber 014 is inside the transmission lens 013. The laser emitter 011 is flush with the diffractor 012, and the emission port of the laser emitter 011 faces the diffractor 012. The diffraction light receiver 017 is flush with the diffractor 012 and parallel to the diffractor 012. Potassium nitrate microspheres 045 and the solution enter the dispersion chamber 014 through the dispersion inlet 016. The potassium nitrate microspheres 045 are irradiated by the laser emitter 011 and the diffraction light receiver 017 is used to measure the particle size. The solution containing potassium nitrate microspheres 045 then flows out through the dispersion outlet 015.

[0024] The sphere-liquid separation module 02 is connected to the real-time particle size detection module 01 via the detection outlet pipe 019. The sphere-liquid separation module 02 is a device for separating a concentrated solution containing potassium nitrate microspheres 045 and a clear solution without potassium nitrate microspheres 045. The sphere-liquid separation module 02 includes a hydrocyclone separator 021, a hydrocyclone separator inlet 022, a clear solution outlet 023, a concentrated solution outlet 024, a three-way reversing valve 025, a circulation pipe 026, a finished product pipe 027, and a first peristaltic pump 028. The solution containing potassium nitrate microspheres 045... After detection, the liquid flows from the bottom into the hydrocyclone separator 021 through the outlet pipe 019. In the hydrocyclone separator 021, centrifugation separates the concentrated solution containing potassium nitrate microspheres 045 from the clear solution without potassium nitrate microspheres 045. The concentrated solution containing potassium nitrate microspheres 045 is a mixture of deionized water and anhydrous ethanol with a large amount of potassium nitrate microspheres 045 suspended in it. The clear solution without potassium nitrate microspheres 045 is a low-concentration mixture of deionized water and anhydrous ethanol containing only a trace amount of unprecipitated potassium nitrate microspheres 045. The potassium microspheres 045 have a low density in the clarified liquid and enter the clarified liquid outlet 023 located at the top of the hydrocyclone 021. The concentrated liquid containing potassium nitrate microspheres 045 has a high density and enters the concentrated liquid outlet 024 located at the top of the hydrocyclone 021, which is lower than the clarified liquid outlet 023. The clarified liquid outlet 023 is connected to the concentration titration module 03 through the titration inlet 035. The first peristaltic pump 028 is located at the concentrated liquid outlet 024, and the circulation pipe 026 is directly connected to the concentrated liquid outlet 024. At the same time, the centrifugal differential rounding module 0... 4. The ball-liquid separation module 02 is connected through the circulation pipe 026. The three-way reversing valve 025 is located after the first peristaltic pump 028 and is also on the concentrated liquid outlet 024. The finished product pipe 027 is connected to the concentrated liquid outlet 024 at the three-way reversing valve 025. The concentrated liquid containing potassium nitrate microspheres 045 that has not been properly polished enters the centrifugal differential rolling module 04 through the circulation pipe 026 under the action of the three-way reversing valve 025 for further polishing. The polished product enters the finished product pipe 027 under the action of the three-way reversing valve 025.

[0025] like Figure 7As shown, the microsphere drying and separation module 05 includes a dryer 051, a dryer inlet 052, an air duct 053, a mixed steam outlet 054, a mixed steam pipe 055, a ball-spinning disc 056, a drying hot air inlet 057, a baffle plate 058, a distributor 059, a high-boiling-point condenser 061, a high-boiling-point gas supply pipe 062, and a low-boiling-point condenser 063. The microsphere drying and separation module 05 is connected to the microsphere-liquid separation module 02 via the finished product pipe 027. The microsphere drying and separation module 05 is a device for drying and separating the polished potassium nitrate microspheres 045. The dryer inlet 052 is located at the dryer 05. Inside the dryer 051, connected to the finished product pipe 027, a distributor 059 is located directly below the dryer inlet 052, with its upper end connected to the dryer inlet 052. A ball-spinning disc 056 is connected to the distributor 059, and its lower end is flush with the distributor 059. A duct 053 is located on the outer shell of the dryer 051, with its height flush with the dryer inlet 052. The air outlet of the duct 053 faces the ball-spinning disc 056, causing it to rotate through the airflow. Inside the dryer 051, at the bottom, are three hot air inlets 057. Hot air blown in at 057 vaporizes the concentrated liquid flowing onto the ball-spinning plate 056, leaving potassium nitrate microspheres 045 that fall below the dryer 051. The vaporized steam enters the mixing steam pipe 055 through the mixing steam outlet 054 located at the top of the dryer 051. The mixing steam pipe 055 is connected to the dryer 051 through the mixing steam outlet 054. The mixing steam pipe 055 is followed by a high-boiling-point condenser 061. A low-boiling-point condenser 063 is connected to the high-boiling-point condenser 061 through a high-boiling-point gas supply pipe 062. The standard boiling point of deionized water is 100℃, and the standard boiling point of anhydrous ethanol is... At 78.2℃, the vaporized steam enters the mixing steam pipe 055. The high-boiling-point deionized water condenses in the high-boiling-point condenser 061 and enters the high-boiling-point liquid burette 032 on the high-boiling-point condenser 061. The low-boiling-point anhydrous ethanol condenses in the low-boiling-point condenser 063 and enters the low-boiling-point liquid burette 031 on the low-boiling-point condenser 063. The condensed deionized water and anhydrous ethanol enter the concentration titration module 03 to continue to participate in stirring and mixing. The microsphere drying and separation module 05 is connected to the concentration titration module 03 through the low-boiling-point liquid burette 031 and the high-boiling-point liquid burette 032.

[0026] An apparatus for preparing selectively soluble microspheres includes: (1) Compound microspheres 045, and a first solvent in which compound microspheres 045 are easily soluble and a second solvent in which compound microspheres are essentially insoluble, are titrated into the concentration titration module 03 in very small amounts under the condition that the first solvent and the second solvent are miscible. The stirring power source 033 drives the stirrer 034 to stir rapidly so that the compound microspheres 045 and the two solvents are mixed. After mixing, the mixture flows into the titration outlet 036.

[0027] (2) The mixed solution flows from the titration outlet 036 into the rounding inlet 041 of the centrifugal differential rounding module 04 through the second pump output pipe 039 under the action of the second peristaltic pump 038. The mixed solution enters the horizontal spiral rounding tube 042 from the rounding inlet 041. Under the condition that the solution flow rate is the same, the linear velocity of the solution in the tube relative to the center of the device is the same. At this time, the centrifugal force at different radii is different. The different centrifugal forces bring about the difference in the friction points between the compound microspheres 045 and the wall of the horizontal spiral rounding tube 042, and at the same time, the friction points between different compound microspheres 045 are different. This continuous The friction process at different points causes the compound microspheres 045 to be continuously subjected to uniform and moderate tangential and normal grinding. The surface edges of the compound microspheres 045 are gradually eliminated, resulting in the compound microspheres 045 achieving the set sphericity. After being ground by the horizontal spiral rolling tube 042, the compound microspheres 045 enter the vertical spiral rolling tube 043, where they are also ground. The horizontal spiral rolling tube 042 and the vertical spiral rolling tube 043 together form a spherical grinding device. After grinding, the compound microspheres 045 and the solution flow together into the rolling outlet 044.

[0028] (3) The polished compound microspheres 045 flow into the detection inlet pipe 018 from the rounding outlet 044 along with the mixed solution. The polished compound microspheres 045 then enter the dispersion inlet 016 of the particle size real-time detection module 01 through the detection inlet pipe 018 along with the mixed solution. Afterward, they flow downward into the dispersion chamber 014. Under the illumination of the laser emitter 011, the polished compound microspheres 045 are monitored by the diffraction light receiver 017 to see if they meet the requirements. Then, the compound microspheres 045 flow into the detection outlet pipe 019 from the dispersion outlet 015 along with the mixed solution.

[0029] (4) The solution containing the polished compound microspheres 045 flows from the post-detection outlet pipe 019 through the hydrocyclone inlet 022 into the hydrocyclone separator 021. Under the action of centrifugal force in the hydrocyclone separator 021, the solution containing the polished compound microspheres 045 is divided into a concentrated liquid containing compound microspheres 045 and a clear liquid without compound microspheres 045. The clear liquid without compound microspheres 045 has a low density and enters the clear liquid outlet 023. The concentrated liquid containing compound microspheres 045 has a high density and enters the concentrated liquid outlet 024. The solution entering the clear liquid outlet 023 will enter the concentration titration module 03 through the titration inlet 035 to participate in the next mixing. The solution containing compound microspheres 045 entering the concentrated liquid outlet 024, under the action of the first peristaltic pump 028, the polished solution enters the finished product pipe 027 through the three-way reversing valve 025, and the unpolished solution enters the product pipe 027 through the circulation pipe 026 and is polished again in the centrifugal differential rounding module 04.

[0030] (5) The solution containing compound microspheres 045 enters the finished product tube 027 and then enters the dryer inlet 052 of the microsphere drying and separation module 05. The solution containing compound microspheres 045 falls from the dryer inlet 052 along the distributor 059 onto the ball-spinning plate 056. Under the action of the air duct 053, the ball-spinning plate 056 rotates. The hot air blown out through the drying hot air inlet 057 vaporizes the solution containing compound microspheres 045. The compound microspheres 045 fall into the dryer 051 and are collected. The vaporized solution vapor enters the mixed vapor outlet 054. The high boiling point solvent vapor condenses in the high boiling point condenser 061 and enters the high boiling point liquid burette 032. The low boiling point solvent vapor condenses in the low boiling point condenser 063 and enters the low boiling point liquid burette 031. The condensed solvent enters the concentration titration module 03 to participate in the next mixing.

Claims

1. A device for the preparation of selectively lysing microspheres, characterized in that, include: The system comprises a real-time particle size detection module, a microsphere-liquid separation module, a concentration titration module, a centrifugal differential spheroidizing module, and a microsphere drying and separation module. The centrifugal differential spheroidizing module and the concentration titration module are connected via a second pump output pipe. The real-time particle size detection module is connected to the spheroidizing outlet of the centrifugal differential spheroidizing module via a detection inlet pipe. The microsphere-liquid separation module is connected to the real-time particle size detection module via a detection outlet pipe. The microsphere drying and separation module is connected to the microsphere-liquid separation module via a finished product pipe. The real-time particle size detection module is used to detect the particle size of the compound microspheres after grinding. The microsphere-liquid separation module is used to separate the concentrated liquid containing the compound microspheres from the clear liquid without the compound microspheres. The concentration titration module reduces the formation of excessively low solvent concentrations in local areas by titrating the mixed solvent and compound microspheres and by rapid stirring. The centrifugal differential spheroidizing module is used to grind the compound microspheres to achieve the set sphericity. The microsphere drying and separation module is used to dry and separate the ground compound microspheres.

2. The apparatus for preparing a selective solubility microsphere according to claim 1, wherein The concentration titration module includes a low-boiling-point liquid burette, a high-boiling-point liquid burette, a stirrer, a titration inlet, and a titration outlet. The solution formed by the solvent and compound microspheres entering through the low-boiling-point liquid burette, the high-boiling-point liquid burette, and the titration inlet is stirred by the stirrer and then flows out from the titration outlet.

3. The apparatus for preparing selectively soluble microspheres as described in claim 1, characterized in that, The centrifugal differential rounding module includes a rounding inlet, a horizontal spiral rounding tube, a vertical spiral rounding tube, and a rounding outlet. The solution containing compound microspheres enters the horizontal spiral rounding tube through the rounding inlet. After being polished in the horizontal spiral rounding tube, the compound microspheres enter the vertical spiral rounding tube, where they are also polished. The polished compound microspheres and the solution flow together into the rounding outlet.

4. The apparatus for preparing selectively soluble microspheres as described in claim 1, characterized in that, The real-time particle size detection module includes a laser emitter, a diffractometer, a dispersion tank, a dispersion outlet, a dispersion inlet, a diffraction light receiver, a detection inlet pipe, and a detection outlet pipe. After grinding, the compound microspheres flow into the detection inlet pipe from the rounding outlet along with the mixed solution. The compound microspheres then flow downwards into the dispersion tank. Under the illumination of the laser emitter, the diffraction light receiver monitors whether the ground compound microspheres meet the requirements. Finally, the compound microspheres flow into the detection outlet pipe from the dispersion outlet along with the mixed solution.

5. The apparatus for preparing selectively soluble microspheres as described in claim 1, characterized in that, The microsphere drying and separation module includes a dryer, a dryer inlet, a duct, a mixed steam outlet, a mixed steam pipe, a ball-spinning disc, a drying hot air inlet, a baffle plate, a distributor, a high-boiling-point condenser, a high-boiling-point gas supply pipe, and a low-boiling-point condenser. The solution containing the compound microspheres falls from the dryer inlet along the distributor onto the ball-spinning disc. Under the action of the duct, the ball-spinning disc rotates, and the hot air blown out through the drying hot air inlet vaporizes the solution containing the compound microspheres. The compound microspheres fall to the bottom of the dryer and are collected. The vaporized solution vapor enters the mixed steam outlet. The high-boiling-point solvent vapor condenses in the high-boiling-point condenser and enters the high-boiling-point liquid burette. The low-boiling-point solvent vapor condenses in the low-boiling-point condenser and enters the low-boiling-point liquid burette. The condensed solvent enters the concentration titration module to participate in the next mixing.

6. The method for preparing selectively soluble microspheres according to claim 1 specifically includes the following steps: (1) The compound microspheres, the first solvent in which the compound microspheres are easily soluble, and the second solvent in which the compound microspheres are essentially insoluble are titrated into the concentration titration module in a very small amount under the condition that the first solvent and the second solvent are miscible. The stirring is driven by the stirring power source to stir so that the compound microspheres and the two solvents are mixed to form a solution. The mixed solution flows into the titration outlet. (2) The mixed solution flows from the titration outlet into the rounding inlet of the centrifugal differential rounding module through the second pump output pipe under the action of the second peristaltic pump. The mixed solution enters the horizontal spiral rounding tube from the rounding inlet. The compound microspheres are polished in the horizontal spiral rounding tube and then enter the vertical spiral rounding tube. The compound microspheres are also polished in the vertical spiral rounding tube. The polished compound microspheres and the solution flow into the rounding outlet together. (3) The polished compound microspheres flow into the detection inlet pipe from the rounding outlet along with the mixed solution. The polished compound microspheres flow into the dispersion inlet of the particle size real-time detection module through the detection inlet pipe along with the mixed solution. Then they flow downward into the dispersion chamber. Under the illumination of the laser emitter, the polished compound microspheres are monitored by the diffraction light receiver to see if they meet the requirements. Then the compound microspheres flow into the detection outlet pipe from the dispersion outlet along with the mixed solution. (4) The solution containing the polished compound microspheres flows into the hydrocyclone separator through the outlet pipe after detection. Under the action of centrifugal force in the hydrocyclone separator, the solution containing the polished compound microspheres is divided into a concentrated liquid containing compound microspheres and a clear liquid without compound microspheres. The clear liquid without compound microspheres enters the clear liquid outlet, and the concentrated liquid containing compound microspheres enters the concentrated liquid outlet. The solution entering the clear liquid outlet enters the concentration titration module through the titration inlet to participate in the next mixing. The solution containing compound microspheres entering the concentrated liquid outlet is driven by the first peristaltic pump. The polished compound microspheres are carried by the solution through the three-way reversing valve into the finished product pipe, and the unpolished compound microspheres are carried by the solution through the circulation pipe and polished again in the centrifugal differential rolling module. (5) After the solution containing the compound microspheres enters the finished product tube, it enters the dryer inlet of the microsphere drying and separation module. The solution containing the compound microspheres falls from the dryer inlet along the distributor onto the ball-spinning plate. Under the action of the air duct, the ball-spinning plate rotates. The hot air blown out through the drying hot air inlet vaporizes the solution containing the compound microspheres. The compound microspheres fall into the bottom of the dryer and are collected. The vaporized solution vapor enters the mixed vapor outlet. The high-boiling-point solvent vapor condenses in the high-boiling-point condenser and enters the high-boiling-point liquid burette. The low-boiling-point solvent vapor condenses in the low-boiling-point condenser and enters the low-boiling-point liquid burette. The condensed solvent enters the concentration titration module to participate in the next mixing. At this point, one cycle ends.

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