CN1907553A - Method for preparing microsphere with nitrogen aid and apparatus thereof - Google Patents
Method for preparing microsphere with nitrogen aid and apparatus thereof Download PDFInfo
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- CN1907553A CN1907553A CN 200610036589 CN200610036589A CN1907553A CN 1907553 A CN1907553 A CN 1907553A CN 200610036589 CN200610036589 CN 200610036589 CN 200610036589 A CN200610036589 A CN 200610036589A CN 1907553 A CN1907553 A CN 1907553A
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Abstract
The invention relates to a method for preparing nitrogen auxiliary micro ball and a relative device, wherein it comprises: material and high-pressure nitrogen enter into ejector via two channels; the material is atomized via high-pressure air in ejector to enter into collecting room to form micro particles; the device has the units for transmitting gas and liquid, for forming particles and controlling and displaying; the gas transmitter has nitrogen pot, back pressure valve, high-pressure air meter, air compressor and buffer pot; the liquid transmitter has material groove, high-pressure liquid pump, solution coil tube and check valve; the particle former has ejector, particle collecting room, solvent recycle cold well, and vacuum pump; the controlling displaying part has air constant-temperature device, material temperature controller, pressure meter, temperature screen, and high-pressure air meter; using ultra-critical N2 and non-ultra-critical CO2, using coaxial dual-channel ejector to process the fusion material, with simple operation.
Description
Technical field
The present invention relates to a kind of ultrafine dust material, especially relate to a kind of microsphere with nitrogen aid preparation method and device thereof.
Background technology
The ultrafine dust material is owing to there is special physicochemical character, is a focus in the current new and high technology, and it has important use to be worth in fields such as material, chemical industry, light industry, metallurgy, electronics, medical science and biologies, and has been used widely.It is a new granulation technique of just actively researching and developing both at home and abroad in recent ten years that supercritical fluid prepares the ultrafine powder technology, compare with grinding, solution crystallization and chemical reaction etc. as mechanical crushing with traditional particle formation method, this method has product purity height, geometry homogeneous, narrow diameter distribution, manufacturing process is simple, operating temperature is low and avoid with an organic solvent waiting many tangible advantages, and especially impact sensitivity, thermo-responsive, structural instability and the processing that is easy to the system of chemical breakdown have clear superiority.
Through 20 years of development, emerge in large numbers multiple use supercritical fluid in the world and prepared the technology of microparticle, wherein, relatively Tu Chu several technology are respectively: supercritical solution fast expansion (Rapid Expansion of SupercriticalSolutions, RESS), the anti-solvent recrystallization process of gas (The Supercritical Anti-solvent Process, SAS/GAS) and gas saturated solution particulate form technology (Particles from Gas Saturated Solutions, PGSS) etc.
The SAS method has comprised a lot of improved methods again in the above-mentioned technology, and SEDS (the Solution Enhanced Dispersion by Supercritical fluid) method of continued operation process is arranged near industrialized method at present.It is newer a kind of that PGSS is that supercritical fluid prepares in the ultrafine powder technology, the applicant is (referring to Li J for this reason, Matos H A, Gomes deAzevedo E.Modeling of particle formation from a gas-saturated solution process, Proceedings ofthe Sixth International Symposium on Supercritical Fluids, Versailles (France), 2003) process of PGSS experimental study and simulation have been carried out, and the atomization process of PGSS process set up model, the drop size that nozzle exit liquid atomizes mutually and produces is discussed.Thereafter (referring to: Li J, Matos H A, Gomes de Azevedo E.Two-PhaseHomogeneous Model for Particle Formation from Gas-Saturated Solution Processes, J.ofSupercritical Fluids, 2004, (32): 275-286) considered the fusion-crystallization mechanism of PGSS process again, various operating conditions are inquired into the influence of microparticle size, have spherical and irregular crystal shape, multimodal distribution of particles yet analog result does not reflect the variation of particulate pattern, particularly experimental result.So further (referring to: Li J, Rodrigues M A, Matos H A, Almeida A, Gomes de Azevedo E.Modeling of the PGSS process by Crystallization and Atomization, AIChE J, 2005,51 (8), 2345-2357) fusion-crystallization and atomization mechanism combination are paid attention to, can produce the particulate of RESS mechanism, the particulate of fusion-crystallization and the particulate of atomized drop correspondence simultaneously; Their quantity, size and pattern are different and different with operating condition, thereby can simulate the mechanism of the particle correspondence of multimodal distribution of particles and sign different-shape, and atomizing produces spheroidal particle, and crystallization produces irregular crystal.
Used supplementary means all is to adopt supercritical CO in the aforementioned supercritical fluid micronize technology
2The solvent that fluid, it and required micronized solute or be used to dissolve solute has good compatibility, so can utilize crystallization mechanism to obtain micro-nano particle.Yet inquire into as can be seen from above-mentioned mechanism, atomization process tool in such as PGSS and SEDS plays a very important role, and atomization process often can obtain more intact spheric granules.
Summary of the invention
The object of the present invention is to provide a kind of microsphere with nitrogen aid preparation method and device thereof.
The technical solution adopted in the present invention is on the basis according to the above-mentioned theoretical research of carrying out, based on PGSS and SEDS technology, to use overcritical N
2Replace supercritical CO
2Material is carried out micronize, eliminate solution crystallization, obtain single atomizing particle, and designed corresponding micronize technology.
Microsphere with nitrogen aid preparation method of the present invention the steps include:
1) required material to be processed is pumped into high-pressure system with pump from a passage, enter nozzle;
2) high pressure nitrogen enters nozzle from another passage, and atomizing enters the particulate collecting chamber to material through gases at high pressure in nozzle, forms microparticle in the indoor curing of particulate collecting (comprising the volatilization of organic solvent).
Described material can be the material of fusion or the material of being furnished with organic solvent.
Microsphere with nitrogen aid preparation facilities of the present invention is provided with gas transport portion, liquid supplying part, particulate forms with collect part and control display part.
The gas transport portion is used for forming and collection part supplying nitrogen to particulate, the gas transport portion is provided with nitrogen storage tank, counterbalance valve, gases at high pressure flow meter, gas compressor and surge tank, nitrogen storage tank connects the backflow output of gas compressor input and counterbalance valve respectively through stop valve (being designated as the 1st stop valve) and filter, and the backflow input of gas compressor output and counterbalance valve connects surge tank through gases at high pressure flow meter.
Liquid supplying part is used for forming and collection part delivering liquid material to particulate, liquid supplying part is provided with material trough, pressure liquid pump, solution coil pipe and check (non-return) valve, the outlet of material trough connects the import of pressure liquid pump, and the highly pressurised liquid delivery side of pump connects the import of check (non-return) valve behind the solution coil pipe.
Particulate forms and collects formation and the collection that partly is used for particulate, particulate forms with collection unit and is arranged with nozzle, particulate collecting chamber, solvent recovery cold-trap and vavuum pump, the 1st channel entrance of nozzle is connected with the outlet of surge tank through stop valve (being designated as the 2nd stop valve), the 2nd channel entrance of nozzle is connected with the outlet of check (non-return) valve, the outlet of nozzle connects the particulate collecting chamber, the outlet of particulate collecting chamber connects the solvent recovery cold-trap through filter, and the solvent recovery cold-trap is connected to the inlet of vavuum pump.
The control display part is used for the constant temperature and the pressure of air and material, the demonstration of temperature and flow, the control display part is provided with the air thermostat, the material temperature controller, Pressure gauge, temperature indicator and gases at high pressure flow meter, surge tank, nozzle, the particulate collecting chamber, the solution coil pipe, stop valve and check (non-return) valve etc. are located in the air thermostat, the material temperature controller is connected with thermocouple in the material trough with the control material temperature, Pressure gauge is connected with surge tank, the thermocouple that is connected with temperature indicator is installed on nozzle inlet, and gases at high pressure flow meter is connected with the import of surge tank.
Described nozzle adopts coaxial double-channel spray nozzle.
Maximum characteristics of the present invention are to use overcritical N
2But not supercritical CO
2, because overcritical N
2Be easy to realize (critical-temperature 126.2K, critical pressure 3.4MPa) that therefore the present invention compares with the SEDS technology with PGSS on the technology, does not all need to have processing CO
2Fluid system (mainly being the high pressure refrigeration system), and only need a compressor to get final product; Different with the PGSS technology, the present invention has adopted coaxial double-channel spray nozzle; Compare with the SEDS technology, the present invention but can conveniently handle fused materials.In operation, because overcritical N
2The inertia characteristics, do not have saturated mixed problem with required material to be processed and different with PGSS and SEDS process, need not to worry the problem of saturation time, thereby operation and control are simplified greatly.On the result, the particulate pattern difference that obtains, promptly the PGSS process often produces the particle of multiple pattern, and the SEDS process also can form the particle of multiple pattern owing to the crystallization before the nozzle and the atomizing behind the nozzle, and the present invention forms single atomizing spheric granules.
The handled object of the present invention can be the material (fat, medicine, macromolecule etc.) of fusion and the material that can dissolve in organic solvent.Prepared particulate is mainly used in fat-soluble or water soluble drug, medicinal compound type, discharges but especially be applied to the induction type controlled delivery of pharmaceutical agents.Because the particulate of preparation mainly occurs with the single shape of microballoon (containing bulky grain low bulk density microballoon), other medicines particulate pattern is more suitable for sucking and entering lung relatively.And the most important thing is to control the particle size distribution range of product easily at 1～5 μ m.
Description of drawings
Fig. 1 is that microsphere with nitrogen aid preparation facilities example structure of the present invention is formed and process flow diagram.
Fig. 2 is the polyethylene glycol polymer particulate of the present invention's preparation.In Fig. 2, from top to bottom, from left to right be followed successively by 2a, 2b, 2c, 2d, 2e, 2f.
Fig. 3 is the myristic acid laurate particulate of the present invention's preparation.In Fig. 3, from top to bottom, from left to right be followed successively by 3a, 3b, 3c, 3d.
Fig. 4 is the medicine Co-Q10 particulate of the present invention's preparation.In Fig. 4, from left to right be followed successively by 4a, 4b.
The specific embodiment
Referring to Fig. 1, microsphere with nitrogen aid preparation facilities of the present invention is provided with gas transport portion, liquid supplying part, particulate forms with collect part and control display part.The gas transport portion is used for forming and collection part supplying nitrogen to particulate, the gas transport portion is provided with nitrogen storage tank A, gas compressor B, counterbalance valve C, gases at high pressure flow meter D and surge tank E, nitrogen storage tank A connects the backflow output of gas compressor B and counterbalance valve C respectively through the 1st stop valve V1 and the 1st filter LF1, and the backflow input of gas compressor B and counterbalance valve C meets surge tank E through gases at high pressure flow meter D.Liquid supplying part is used for forming and collection part delivering liquid material to particulate, liquid supplying part is provided with material trough J, pressure liquid pump I, solution coil pipe H and the check (non-return) valve VC of band temperature controller TC, the outlet of material trough J connects the import of pressure liquid pump I, and the outlet of pressure liquid pump I connects the import of check (non-return) valve VC behind solution coil pipe H.Particulate forms and collects formation and the collection that partly is used for particulate, particulate forms and is arranged with coaxial double-channel spray nozzle F, particulate collecting chamber G, solvent recovery cold-trap L and vavuum pump M with collection unit, the 1st channel entrance of nozzle F is connected with the outlet of surge tank E through the 2nd stop valve V2, the 2nd channel entrance of nozzle F is connected with the outlet of check (non-return) valve VC, the outlet of nozzle F meets particulate collecting chamber G, G outlet in particulate collecting chamber meets solvent recovery cold-trap L through the 2nd filter LF2, and solvent recovery cold-trap L is connected to the inlet of vavuum pump M.The control display part is used for the constant temperature and the pressure of material, the demonstration of temperature and flow, the control display part is provided with air thermostat K, material temperature controller TC, Pressure gauge P, temperature indicator T and gases at high pressure flow meter D, surge tank E, nozzle F, particulate collecting chamber G, solution coil pipe H, the 2nd stop valve V2 and check (non-return) valve VC etc. are located in the air thermostat K, thermocouple in material temperature controller TC and the material trough J is connected, Pressure gauge P is connected with surge tank E, the pairing thermocouple of temperature indicator T is connected with the inlet of nozzle, and gases at high pressure flow meter D is connected with the import of surge tank E.
The jet hole of coaxial double-channel spray nozzle F adopts the stainless steel thin slice of laser boring to make, the diameter of jet hole is 80～120 μ m, coaxial double-channel spray nozzle is 6mm (logical gases at high pressure) with external diameter respectively, and interior cover external diameter is that the high pressure stainless steel tube of 3mm (logical high-pressure solution) is made.Operating pressure (the pre-bulbs of pressure): 4～15MPa, operating temperature (pre-expansion temperature): 293～343K, solution flow rate: 1～7mL/min, organic solution (acetone+Macrogol 6000) concentration: 0.04～0.4g/mL handles material: material of fusion (for example fat, medicine, macromolecule etc.) and the material that can dissolve in organic solvent (for example acetone etc.).
Before the operation, the air-tightness of testing fixture, each road heat tracing situation and instrument show and the control situation, confirms no problem after, design and control well temperature (expansion temperature in advance) in the air thermostat.The pretreated liquid (putting into if solid material can melt then in advance, if solution is directly put into) of packing in the material trough J, logical then outsourcing heating tape keep steady temperature also to guarantee the whole fusions of target medicine or for liquid.Open nitrogen steel cylinder and the 1st stop valve V1 then,, nitrogen is pressed into surge tank E with gas compressor through the 1st filter LF1.Set the control experimental pressure (the pre-bulbs of pressure) of counterbalance valve C.After reaching requirement, opens temperature and pressure the 2nd stop valve V2.Can start pressure liquid pump I (setting flow in advance) this moment, and with raw material input nozzle F, the high pressure nitrogen that contains material is in the laggard particulate collecting chamber G of going into of nozzle F atomizing step-down.When processing contained the solution material of organic solvent, particulate collecting chamber G placed in the air thermostat K, and the temperature of particulate collecting chamber G is consistent with system temperature, and aspirates out organic solvent by vavuum pump M, is recovered in the solvent recovery cold-trap L.When the material of handling was melt liquid, particulate collecting chamber G was placed on outside the air thermostat, collected with room temperature condition and solidified particulate, did not need vacuum system this moment, directly logical atmosphere.
Embodiment 1: the microsphere with nitrogen aid technology prepares the polyethylene glycol polymer particulate.
Macrogol 6000, chemical pure, Shanghai chemical reagent purchasing and supply station provide (bulk, the about 2mm of average diameter, as Fig. 2 a); Ordinary nitrogen, purity 〉=98%, Xiamen system nitrogen factory provides; Acetone is analyzed pure AR, purity 〉=99.5%, and Chemical Reagent Co., Ltd., Sinopharm Group provides.Below provide the result's (comprising different acetone soln concentration, different solutions flow, different particulate collecting room temperatures, the different pre-bulbs of pressure, different spray nozzles) under the different operating condition.
(1) the pure Macrogol 6000 of fusion, nozzle diameter 80 μ m, pre-expansion temperature 323K, particulate collecting chamber control temperature 293K (room temperature), the pre-bulbs of pressure are 12MPa, fluid flow is less than 1mL/min, the particle (spherical, average diameter 80 μ m) of preparation is shown in Fig. 2 b.
(2) the acetone soln concentration 0.4g/mL of Macrogol 6000, nozzle diameter 80 μ m, pre-expansion temperature 323K, particulate collecting chamber control temperature 293K (room temperature), the pre-bulbs of pressure are 12MPa, fluid flow is less than 1mL/min, and the particle of preparation (hollow spheres, average diameter 33 μ m) is shown in Fig. 2 c.
(3) the acetone soln concentration 0.04g/mL of Macrogol 6000, nozzle diameter 80 μ m, pre-expansion temperature 323K, particulate collecting chamber control temperature 323K, the pre-bulbs of pressure are 10MPa, liquid inventory 2mL/min, and the particle of preparation is (spherical, average diameter 2 μ m, Particle Distribution is between 0.5～5 μ m) shown in Fig. 2 d.
(4) the acetone soln concentration 0.04g/mL of Macrogol 6000, nozzle diameter 80 μ m, pre-expansion temperature 323K, particulate collecting chamber control temperature 323K, the pre-bulbs of pressure are 4MPa, liquid inventory 2mL/min, and the particle of preparation is (spherical, average diameter 4 μ m, Particle Distribution is between 1～7 μ m) shown in Fig. 2 e.
(5) the acetone soln concentration 0.04g/mL of Macrogol 6000, nozzle diameter 120 μ m, pre-expansion temperature 323K, particulate collecting chamber control temperature 323K, the pre-bulbs of pressure are 10MPa, liquid inventory 2mL/min, and the particle of preparation is (spherical, average diameter 2 μ m, Particle Distribution is between 0.5～5 μ m) shown in Fig. 2 f.
(6) the acetone soln concentration 0.04g/mL of Macrogol 6000, nozzle diameter 120 μ m, pre-expansion temperature 323K, particulate collecting chamber control temperature 323K, the pre-bulbs of pressure are 10MPa, liquid inventory 7mL/min, the particle of preparation (spherical, average diameter 4 μ m, Particle Distribution is between 1～8 μ m).
Embodiment 2: the microsphere with nitrogen aid technology prepares myristic acid fat particulate.
Myristic acid, chemical pure, purity 〉=98%, Chemical Reagent Co., Ltd., Sinopharm Group provides (bulk, the about 200 μ m of average diameter).Ordinary nitrogen, purity 〉=98%, Xiamen system nitrogen factory provides.Below provide the result's (comprising the different pre-bulbs of pressure, different pre-expansion temperatures, different spray nozzles) under the different operating condition.
(1) the pure myristic acid of fusion, nozzle diameter 100 μ m, pre-expansion temperature 333K, particulate collecting chamber control temperature 293K (room temperature), the pre-bulbs of pressure are 10MPa, fluid flow is less than 1mL/min.Raw material and prepared particle (spherical, average diameter 10 μ m) are shown in Fig. 3 a.
(2) the pure myristic acid of fusion, nozzle diameter 100 μ m, pre-expansion temperature 333K, particulate collecting chamber control temperature 293K (room temperature), the pre-bulbs of pressure are 12MPa, fluid flow is less than 1mL/min.Raw material and prepared particle (spherical, average diameter 7 μ m) are shown in Fig. 3 b.
(3) the pure myristic acid of fusion, nozzle diameter 80 μ m, pre-expansion temperature 333K, particulate collecting chamber control temperature 293K (room temperature), the pre-bulbs of pressure are 15MPa, fluid flow is less than 1mL/min.Raw material and prepared particle (spherical, average diameter 2 μ m, Particle Distribution is between 1～4 μ m) shown in Fig. 3 c.
(4) the pure myristic acid of fusion, nozzle diameter 80 μ m, pre-expansion temperature 343K, particulate collecting chamber control temperature 293K (room temperature), the pre-bulbs of pressure are 15MPa, fluid flow is less than 1mL/min.Raw material and prepared particle (spherical, average diameter 4 μ m, Particle Distribution is between 1～6 μ m) shown in Fig. 3 d.
Embodiment 3: medicine Co-Q10 microsphere with nitrogen aid technology prepares the laurate particulate.
Co-Q10, Qualitas Sa (Portugal) company provides (bulk, the about 35 μ m of average diameter).Ordinary nitrogen, purity 〉=98%.Below provide the result under the different pre-expansion temperatures.
(1) the pure Q10 of fusion, nozzle diameter 100 μ m, pre-expansion temperature 328K, particulate collecting chamber control temperature 293K (room temperature), the pre-bulbs of pressure are 7MPa, fluid flow is less than 1mL/min.The particle (spherical, average diameter 15 μ m) of preparation is shown in Fig. 4 a.
(2) the pure Q10 of fusion, nozzle diameter 100 μ m, pre-expansion temperature 338K, particulate collecting chamber control temperature 293K (room temperature), the pre-bulbs of pressure are 7MPa, fluid flow is less than 1mL/min.The particle (spherical, average diameter 20 μ m) of preparation is shown in Fig. 4 b.
Claims (4)
1. the microsphere with nitrogen aid preparation method is characterized in that the steps include:
1) required material to be processed is pumped into high-pressure system with pump from a passage, enter nozzle;
2) high pressure nitrogen enters nozzle from another passage, and atomizing enters the particulate collecting chamber to material through gases at high pressure in nozzle, at the indoor microparticle that solidify to form of particulate collecting.
2. microsphere with nitrogen aid preparation method as claimed in claim 1 is characterized in that described material is the material of fusion or the material of being furnished with organic solvent.
3. the microsphere with nitrogen aid preparation facilities is characterized in that being provided with gas transport portion, liquid supplying part, particulate forms and collects part and the control display part;
The gas transport portion is used for forming and collection part supplying nitrogen to particulate, the gas transport portion is provided with nitrogen storage tank, counterbalance valve, gases at high pressure flow meter, gas compressor and surge tank, nitrogen storage tank connects the backflow output of gas compressor and counterbalance valve respectively through stop valve and filter, and the backflow input of gas compressor and counterbalance valve connects surge tank through gases at high pressure flow meter;
Liquid supplying part is used for forming and collection part delivering liquid material to particulate, liquid supplying part is provided with material trough, pressure liquid pump, solution coil pipe and check (non-return) valve, the outlet of material trough connects the import of pressure liquid pump, and the highly pressurised liquid delivery side of pump connects the import of check (non-return) valve behind the solution coil pipe;
Particulate forms and collects formation and the collection that partly is used for particulate, particulate forms with collection unit and is arranged with nozzle, particulate collecting chamber, solvent recovery cold-trap and vavuum pump, the 1st channel entrance of nozzle is connected with the outlet of surge tank through stop valve, the 2nd channel entrance of nozzle is connected with the outlet of check (non-return) valve, the outlet of nozzle connects the particulate collecting chamber, the outlet of particulate collecting chamber connects the solvent recovery cold-trap through filter, and the solvent recovery cold-trap is connected to the inlet of vavuum pump;
The control display part is used for the demonstration of constant temperature and pressure, temperature and the flow of air and material, the control display part is provided with air thermostat, material temperature controller, Pressure gauge, temperature indicator and gases at high pressure flow meter, surge tank, nozzle, particulate collecting chamber, solution coil pipe, stop valve and check (non-return) valve etc. are located in the air thermostat, the material temperature controller is connected with thermocouple in the material trough, Pressure gauge is connected with surge tank, the pairing thermocouple of temperature indicator is connected with nozzle entrance, and gases at high pressure flow meter is connected with the import of surge tank.
4. microsphere with nitrogen aid preparation facilities as claimed in claim 3 is characterized in that described nozzle is coaxial double-channel spray nozzle.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101362064B (en) * | 2008-09-12 | 2010-06-02 | 周建业 | Spherical granules forming device |
| CN101444709B (en) * | 2008-12-05 | 2010-06-02 | 厦门大学 | Method for obtaining solid particles from water solution by utilizing supercritical carbon dioxide |
| CN101862266A (en) * | 2010-06-01 | 2010-10-20 | 中国人民解放军第三〇九医院 | Monodispersity gel microsphere forming device |
| CN107537412A (en) * | 2016-06-27 | 2018-01-05 | 通用电气公司 | Prepare the method and system of polymer microballoon |
-
2006
- 2006-07-20 CN CNB2006100365896A patent/CN100478062C/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101362064B (en) * | 2008-09-12 | 2010-06-02 | 周建业 | Spherical granules forming device |
| CN101444709B (en) * | 2008-12-05 | 2010-06-02 | 厦门大学 | Method for obtaining solid particles from water solution by utilizing supercritical carbon dioxide |
| CN101862266A (en) * | 2010-06-01 | 2010-10-20 | 中国人民解放军第三〇九医院 | Monodispersity gel microsphere forming device |
| CN101862266B (en) * | 2010-06-01 | 2012-10-10 | 中国人民解放军第三〇九医院 | Monodispersity gel microsphere forming device |
| CN107537412A (en) * | 2016-06-27 | 2018-01-05 | 通用电气公司 | Prepare the method and system of polymer microballoon |
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