CN100444943C - System for preparing micro particles with hydraulic cavitation reinforcing supercritical auxiliary atomizing and its method - Google Patents
System for preparing micro particles with hydraulic cavitation reinforcing supercritical auxiliary atomizing and its method Download PDFInfo
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- CN100444943C CN100444943C CNB200710067262XA CN200710067262A CN100444943C CN 100444943 C CN100444943 C CN 100444943C CN B200710067262X A CNB200710067262X A CN B200710067262XA CN 200710067262 A CN200710067262 A CN 200710067262A CN 100444943 C CN100444943 C CN 100444943C
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Abstract
The invention discloses a system of waterpower cavitation enhanced supercritical assistant pulverization preparing particle and a method thereof, which has the following character that: (1) sieve plate is mounted in the waterpower cavitation mixer to form cavity, inanition and cavum in the miscible liquid flow of supercritical CO2 and solution to realize the rapid mixture thereof, and to make the meltage of the supercritical CO2 in the solution approach the equilibrium solubility; (2) the mixture of the supercritical CO2 and solution is sprinkled into the precipitator by nozzle to form secondary liquid drop, which is heat transfer and mass transfer with N2 to make the liquid vaporize, and then get particle; (3) the particle is collected using the sintered plate mounted on the bottom of the precipitator; (4) the mixing gas of CO2, N2 and solvent enter into the condenser, and the solvent is reclaimed and recycling. The operating condition of the invention is relative mildness, the operating process is simple, the residual of the solvent is low, and the size distribution of the product is narrow. The invention can be used for grain diminution of various of material.
Description
Technical field
The present invention relates to a kind of system and method thereof of preparing micro particles with hydraulic cavitation reinforcing supercritical auxiliary atomizing.
Background technology
The method of particulate preparation at present mainly contains mechanical crushing method, liquid anti-solvent method, spray drying process and freezing etc.Though these methods are simple to operate; but all exist some shortcoming and defect; remaining organic solvent content height in, the product big, treat that micronized solute thermal sensitivity degraded is serious etc., the most important thing is that these methods all are difficult to control the particle size of product, distribution and product pattern as organic solvent load.Though these methods still play an important role in the production of large petroleum chemicals, in recent years along with the day by day raising of people to food, pharmaceutical requirements (kind, quality), these traditional methods obviously more and more have been difficult to satisfy people's demand.
In recent years, along with going deep into of supercritical fluid technique research, utilize supercritical fluid technique manufacturing micron order, nano_scale particle to be considered to one of effective way that replaces existing particulate technology of preparing.Micronize technology based on supercritical fluid technique can be divided into 4 classes haply: (1) supercritical solution rapid expanding method (RESS); (2) the anti-solvent deposition of supercritical fluid (crystallization) method (SAS); (3) from the gas saturated solution, obtain particulate method (PGSS).The characteristic of these methods is as shown in table 1.
The comparison of the various supercritical fluid technique micronisation process of table 1
1998, Sievers etc. proposed the CO of band bubble drier
2The assisted atomization method (carbon dioxideassisted nebulization with bubble dryer, CAN-BD), supercritical CO
2Finish in threeway with solution and to mix, expand, form the microfluidic aerosol droplet, and use preheating N through flow restrictor
2Be dried to particulate.Because the key position of CAN-BD is the very little threeway of effective mixed volume, mixability is not high, and experimental repeatability is poor.2002; Reverchon and colleague thereof are improved to the saturator that has Berlsaddle with threeway; and with this technology called after supercritical auxiliary atomizing granulating technique (Supercritical fluid assisted atomization; SAA); this technology can be used for the micronize of water-soluble substances; also can be used for the micronize of liposoluble substance, scope is widely used.Though the more original CAN-BD technology of SAA technology improves to some extent, but still exist supercritical carbon dioxide and solution two alternate mass transfer velocities in saturator are crossed the problem that waits slowly, cause that mixing efficiency is low, overstand etc., cause separating out in advance of solute thus easily, influence product quality.
Summary of the invention
The system and the method thereof that the purpose of this invention is to provide a kind of preparing micro particles with hydraulic cavitation reinforcing supercritical auxiliary atomizing.
The system of preparing micro particles with hydraulic cavitation reinforcing supercritical auxiliary atomizing: CO
2Steel cylinder and filter, first cooler, first syringe pump, temperature control heating surge tank, Hydrodynamic cavitation blender, heat exchanger, second syringe pump, solution storage tank join N
2Steel cylinder and heater, settling vessel, vavuum pump, second cooler, flowmeter join, and Hydrodynamic cavitation blender and nozzle and settling vessel join, and blender links to each other with temperature controller, Pressure gauge and safety valve, and settling vessel links to each other with Pressure gauge with temperature controller.
Described Hydrodynamic cavitation blender has upper kettle, lower kettle, and upper kettle and lower kettle are by bolted on connection, and the fixing clearance rate is 10～50% sieve plate between last lower kettle, and upper kettle has CO
2Charging aperture, solution feed mouth, upper kettle top have Pressure gauge, relief valve connection, lower kettle bottom to be provided with outlet, and to join with nozzle.Described sieve plate is single hole or porous.
The method of preparing micro particles with hydraulic cavitation reinforcing supercritical auxiliary atomizing comprises following feature:
1) the fixing clearance rate is 10～50% sieve plate in the Hydrodynamic cavitation blender, makes inner hole, cavity or the cavity of producing of mixed liquor fluid of supercritical carbon dioxide and solution, realizes CO in the Hydrodynamic cavitation blender
2With the rapid mixing of solution, make meltage and the equilbrium solubility of supercritical carbon dioxide in liquid solution approaching;
2) be that 20～85 ℃, pressure are that 6～20MPa, liquid inventory are that 10～100ml/min and stream of supercritical carbon dioxide amount are under the condition of 10～250g/min in temperature, the mixed liquor of supercritical carbon dioxide and solution is that the nozzle of 50～200 μ m is injected in the settling vessel through internal diameter, the drop instantaneous expansion makes the CO that is dissolved in the drop
2Discharge rapidly, form the secondary drop, secondary drop and the N that enters in the settling vessel
2Under 50～120 ℃ of temperature, conduct heat and mass transfer, thereby liquid flux evaporates rapidly and obtains solia particle;
3) utilize the sintered plate that is installed in the settling vessel bottom, collect and obtain particulate;
4) CO
2, N
2, solvent gas enters condenser, reuse after the solvent recovery.
The present invention has adopted the hydraulic cavitation reinforcing supercritical auxiliary atomizing principle, the solubility that exists in the existing particulate technology of preparing is low, particle size distribution range is wide, operating procedure is complicated, yield is low, cost is high, residual contamination is difficult to control, end product quality is difficult to problems such as assurance to solve, it is slow excessively particularly to have solved the supercritical carbon dioxide and the solution two alternate mass transfer velocities in saturator that exist among the SAA effectively, problem such as mixing efficiency is low, overstand, solute are separated out in advance, unstable product quality.
The present invention has that operating condition is gentle relatively, operating procedure is simple, dissolvent residual is low, the product cut size narrowly distributing; the micronize that can be used for water-soluble substances; the micronize that also can be used for liposoluble substance, the characteristics such as scope that are widely used, two strands of materials are respectively high pressure compressed CO
2With the organic solvent or the aqueous solution, solute can be any in the medicine (example hydrochloric acid lavo-ofloxacin, ROX, aspirin, salbutamol etc.), polymer (as PLA etc.), pigment, inorganic salts of water-soluble or organic solvent.
Description of drawings
Fig. 1 is a preparing micro particles with hydraulic cavitation reinforcing supercritical auxiliary atomizing system architecture schematic diagram;
Fig. 2 is a Hydrodynamic cavitation mixer structure schematic diagram of the present invention.
The specific embodiment
As shown in Figure 1, in the system of preparing micro particles with hydraulic cavitation reinforcing supercritical auxiliary atomizing, CO
2Steel cylinder 1 joins N with filter 2, first cooler 3, first syringe pump 4, temperature control heating surge tank 5, Hydrodynamic cavitation blender 6, heat exchanger 7, second syringe pump 8, solution storage tank 9
2 Steel cylinder 11 joins with heater 12, settling vessel 13, vavuum pump 14, second cooler 15, flowmeter 16, and the Hydrodynamic cavitation blender joins with nozzle 10, settling vessel 13.Be the temperature and the pressure of control system, Hydrodynamic cavitation blender 6 links to each other with temperature controller, Pressure gauge and safety valve, and settling vessel links to each other with Pressure gauge with temperature controller.
System is by three material supply lines, i.e. supercritical carbon dioxide, liquid solution and preheating N
2Deng pipeline form.Liquid CO
2Take from steel cylinder, through compressor pressurizes and the hot bath laggard waterpower cavitation blender of going into that heats up, when being raised to preset value, starts pressure pressure liquid pump, throw solution into the Hydrodynamic cavitation blender, supercritical carbon dioxide and solution fully mix, and the Hydrodynamic cavitation blender is by the electrical heating temperature control.The nozzle of an adjustable size control is equipped with at Hydrodynamic cavitation mixer outlet place, and mixed liquor enters settling vessel through nozzle.N
2Through also entering settling vessel after the heat exchanger heating, with CO
2And drop forms turbulent flow in settling vessel, carries out violent heat transfer and mass transfer, thereby liquid flux evaporates rapidly and obtains particulate, and sintered plate is equipped with in the settling vessel bottom, holds back the particulate that obtains.Admixture of gas (CO
2+ N
2+ solvent vapo(u)r) enter condenser, solvent condensation separation in condenser is come out, and reclaims and recycling remaining admixture of gas (CO
2+ N
2) by its flow of spinner survey.
As shown in Figure 2, the Hydrodynamic cavitation blender has upper kettle 24, lower kettle 23, and upper kettle and lower kettle connect by bolt 20, and the fixing clearance rate is 10～50% sieve plate 21 between last lower kettle, and upper kettle has CO
2Charging aperture 17, solution feed mouth 19, upper kettle top have Pressure gauge, relief valve connection 18, lower kettle bottom to be provided with outlet 22, and to join with nozzle 10.Sieve plate is single hole or porous, and voidage is 10～50%.
In the Hydrodynamic cavitation blender, supercritical carbon dioxide and solution mixed liquor pass through sieve plate after the porch strong collision reaches first mixing, pressure reduces, because pressure is reduced to a certain critical numerical value (being generally the pressure for vaporization of water) when following, current inside forms hole, cavity or cavity, promptly produces the phenomenon of cavitation bubble.These cavitation bubbles are crumbled and fall under positive pressure, and its process that crumbles and fall only continues several microseconds, thereby produce moment HTHP and with strong shock wave and the speed per hour jet up to 400km/h at this point, and these extreme environments cause CO
2Mix with the quick secondary of solution, make the meltage of actual supercritical carbon dioxide in liquid solution can be approaching with equilbrium solubility.
Following examples are in conjunction with Fig. 1,2, and the operation of hydraulic cavitation reinforcing supercritical auxiliary atomizing device and the example of preparation particulate are described in detail in detail, but do not mean that and limit the scope of the invention.
Embodiment 1: the preparation of lavo-ofloxacin hydrochloride particulate
At first preparing an amount of concentration is the lavo-ofloxacin hydrochloride methanol solution of 2mg/ml, and with water-bath solution is preheating to 40 ℃; Nozzle inside diameter is transferred to 200 μ m; Open compressor, will heat CO in the surge tank
2Boost to 8MPa, temperature control box is heated to 40 ℃; Settling vessel is controlled temperature be made as 60 ℃, and feeding 40NL/min is preheated to 60 ℃ nitrogen.In the Hydrodynamic cavitation blender, feed 60g/minCO then
2Fluid, copper sieve plate voidage (single hole) is 1/8; The Hydrodynamic cavitation blender is boosted to 8MPa, pump into the lavo-ofloxacin hydrochloride methanol solution of 25ml/min again in the Hydrodynamic cavitation blender, the time of staying is 40～60 seconds, with the Hydrodynamic cavitation mixer pressure accurately be controlled at 8MPa (± 0.1MPa); After vaporific drop appears in jet expansion, open vavuum pump, solia particle is trapped within on the sintered plate of settling vessel bottom; Admixture of gas (CO
2+ N
2+ solvent vapo(u)r) continue to enter condenser, solvent condensation separation in condenser is come out.After treating that solution all injects the Hydrodynamic cavitation blender, close the solution compresses pump; After treating that solution all enters settling vessel in the Hydrodynamic cavitation blender, close CO
2Compression pump; After finishing, experiment closes the power supply and the hot nitrogen source of gas cylinder, water-bath and electric heater; Unload settling vessel and collect powder, analyze.Obtaining the lavo-ofloxacin hydrochloride product is white powder, through ESEM, gas chromatographic analysis: average grain diameter 1.2 μ m, size distribution 0.45～1.7 μ m, the methyl alcohol residual quantity is 0.
Embodiment 2: the preparation of PLA particulate
At first preparing an amount of concentration is the PLA dichloromethane solution of 6mg/ml, and with water-bath solution is preheating to 40 ℃; Nozzle inside diameter is transferred to 100 μ m; Open compressor, will heat CO in the surge tank
2Boost to 8MPa, temperature control box is heated to 40 ℃; Settling vessel is controlled temperature be made as 70 ℃, and feeding 40NL/min is preheated to 70 ℃ nitrogen.In the Hydrodynamic cavitation blender, feed the CO of 50g/min then
2Fluid, copper sieve plate voidage (circular holes of 8 1mm) is 0.32; The Hydrodynamic cavitation blender is boosted to 8MPa, pump into the PLA dichloromethane solution of 35ml/min again in the Hydrodynamic cavitation blender, the time of staying is 40～60 seconds, with the Hydrodynamic cavitation mixer pressure accurately be controlled at 8MPa (± 0.1MPa); After vaporific drop appears in jet expansion, open vavuum pump, solia particle is trapped within on the sintered plate of settling vessel bottom; Admixture of gas (CO
2+ N
2+ solvent vapo(u)r) continue to enter condenser, solvent condensation separation in condenser is come out.After treating that solution all injects the Hydrodynamic cavitation blender, close the solution compresses pump; After treating that solution all enters settling vessel in the Hydrodynamic cavitation blender, close CO
2Compression pump; After finishing, experiment closes the power supply and the hot nitrogen source of gas cylinder, water-bath and electric heater; Unload settling vessel and collect powder, analyze.Obtaining PLA is white powder, through ESEM, gas chromatographic analysis: average grain diameter 1.5 μ m, size distribution 0.8～2.1 μ m, the carrene residual quantity is 0.
Embodiment 3: the preparation of aspirin particulate
At first preparing an amount of concentration is the aspirin ethanolic solution of 2mg/ml, and is 60 ℃ with water-bath with the solution preheating; Nozzle inside diameter is transferred to 200 μ m; Open compressor, will heat CO in the surge tank
2Boost to 9MPa, temperature control box is heated to 60 ℃; Settling vessel is controlled temperature be made as 90 ℃, and feeding 50N L/min is preheated to 90 ℃ hot nitrogen.In the Hydrodynamic cavitation blender, feed 65g/minCO then
2Fluid, copper sieve plate voidage (single hole) is 1/10; The Hydrodynamic cavitation blender is boosted to 9MPa, pump into the aspirin ethanolic solution of 40ml/min again in the Hydrodynamic cavitation blender, the time of staying is 40～60 seconds, with the Hydrodynamic cavitation mixer pressure accurately be controlled at 9MPa (± 0.1MPa); After vaporific drop appears in jet expansion, open vavuum pump, solia particle is trapped within on the sintered plate of settling vessel bottom; Admixture of gas (CO
2+ N
2+ solvent vapo(u)r) continue to enter condenser, solvent condensation separation in condenser is come out.After treating that solution all injects the Hydrodynamic cavitation blender, close the solution compresses pump; After treating that solution all enters settling vessel in the Hydrodynamic cavitation blender, close CO
2Compression pump; After finishing, experiment closes the power supply and the hot nitrogen source of gas cylinder, water-bath and electric heater; Unload settling vessel and collect powder, analyze.Obtaining aspirin ethanol is white powder, through ESEM, gas chromatographic analysis: average grain diameter 1.5 μ m, size distribution 0.85～2.5 μ m, the ethanol residual quantity is 0.
Embodiment 4; The preparation of ROX particulate
The ROX acetone soln of at first preparing an amount of concentration and be 15mg/ml is an amount of, and is 40 ℃ with water-bath with the solution preheating; Nozzle inside diameter is transferred to 200 μ m; Open compressor, will heat CO in the surge tank
2Boost to 9.5MPa, temperature control box is heated to 50 ℃; Settling vessel is controlled temperature be made as 80 ℃, and feeding 45N L/min is preheated to 80 ℃ hot nitrogen.In the Hydrodynamic cavitation blender, feed 60g/minCO then
2Fluid, copper sieve plate voidage (single hole) is 1/10; The Hydrodynamic cavitation blender is boosted to 9.5MPa, pump into the ROX acetone soln of 45mi/min again in the Hydrodynamic cavitation blender, the time of staying is 40～60 seconds, with the Hydrodynamic cavitation mixer pressure accurately be controlled at 9.5MPa (± 0.1MPa); After vaporific drop appears in jet expansion, open vavuum pump, solia particle is trapped within on the sintered plate of settling vessel bottom.Admixture of gas (CO
2+ N
2+ solvent vapo(u)r) continue to enter condenser, solvent condensation separation in condenser is come out.After treating that solution all injects the Hydrodynamic cavitation blender, close the solution compresses pump; After treating that solution all enters settling vessel in the Hydrodynamic cavitation blender, close CO
2Compression pump; After finishing, experiment closes the power supply and the hot nitrogen source of gas cylinder, water-bath and electric heater; Unload settling vessel and collect powder, analyze.Obtaining ROX is white powder, through ESEM, gas chromatographic analysis: average grain diameter 1.3 μ m, size distribution 0.95～2.8 μ m, the acetone residual quantity is 0.
Embodiment 5: the preparation of salbutamol particulate
The salbutamol methanol solution of at first preparing an amount of concentration and be 6mg/ml is an amount of, and is 50 ℃ with water-bath with the solution preheating; Nozzle inside diameter is transferred to 200 μ m; Open compressor, will heat CO in the surge tank
2Boost to 10MPa, temperature control box is heated to 50 ℃; Settling vessel is controlled temperature be made as 70 ℃, and feeding 40N L/min is preheated to 70 ℃ hot nitrogen.In the Hydrodynamic cavitation blender, feed 50g/minCO then
2Fluid, copper sieve plate voidage (single hole) is 1/10; The Hydrodynamic cavitation blender is boosted to 10MPa, pump into the salbutamol methanol solution of 40ml/min again in the Hydrodynamic cavitation blender, the time of staying is 40～60 seconds, with the Hydrodynamic cavitation mixer pressure accurately be controlled at 10MPa (± 0.1MPa); After vaporific drop appears in jet expansion, open vavuum pump, solia particle is trapped within on the sintered plate of settling vessel bottom; Admixture of gas (CO
2+ N
2+ solvent vapo(u)r) continue to enter condenser, solvent condensation separation in condenser is come out.After treating that solution all injects the Hydrodynamic cavitation blender, close the solution compresses pump; After treating that solution all enters settling vessel in the Hydrodynamic cavitation blender, close CO
2Compression pump; After finishing, experiment closes the power supply and the hot nitrogen source of gas cylinder, water-bath and electric heater; Unload settling vessel and collect powder, analyze.Obtaining salbutamol is pale yellow powder, through ESEM, gas chromatographic analysis: average grain diameter 1.5 μ m, size distribution 0.9～2.5 μ m, the methyl alcohol residual quantity is 0.
Claims (2)
1. the device of a preparing micro particles with hydraulic cavitation reinforcing supercritical auxiliary atomizing is characterized in that, CO
2Steel cylinder (1) is connected N with filter (2), first cooler (3), first syringe pump (4), temperature control heating surge tank (5), Hydrodynamic cavitation blender (6), heat exchanger (7), second syringe pump (8), solution storage tank (9) successively
2Steel cylinder (11) is connected with heater (12), settling vessel (13), vavuum pump (14), second cooler (15), flowmeter (16) successively, Hydrodynamic cavitation blender (6) is connected with nozzle (10), settling vessel (13) successively, described Hydrodynamic cavitation blender has upper kettle (24), lower kettle (23), upper kettle (24) and lower kettle (23) connect by bolt (20), the fixing clearance rate is 10～50% sieve plate (21) between last lower kettle, and upper kettle is provided with CO
2Charging aperture (17), solution feed mouth (19), upper kettle top are provided with Pressure gauge, relief valve connection (18), the lower kettle bottom is provided with outlet (22), and join with nozzle (10).
2. the method for the preparing micro particles with hydraulic cavitation reinforcing supercritical auxiliary atomizing that installs according to claim 1 of a use is characterized in that comprising as follows:
1) the fixing clearance rate is 10～50% sieve plate in the Hydrodynamic cavitation blender, makes inner hole, cavity or the cavity of producing of mixed liquor fluid of supercritical carbon dioxide and solution, realizes CO in the Hydrodynamic cavitation blender
2With the rapid mixing of solution, make meltage and the equilbrium solubility of supercritical carbon dioxide in liquid solution approaching;
2) be that 20～85 ℃, pressure are that 6～20MPa, liquid inventory are that 10～100ml/min and stream of supercritical carbon dioxide amount are under the condition of 10～250g/min in temperature, the mixed liquor of supercritical carbon dioxide and solution is that the nozzle of 50～200 μ m is injected in the settling vessel through internal diameter, the drop instantaneous expansion makes the CO that is dissolved in the drop
2Discharge rapidly, form the secondary drop, secondary drop and the N that enters in the settling vessel
2Conduct heat and mass transfer, thereby liquid flux evaporates rapidly and obtains solia particle;
3) utilize the sintered plate that is installed in the settling vessel bottom, collect and obtain particulate;
4) CO
2, N
2, solvent gas enters condenser, reuse after the solvent recovery.
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| CN101869820B (en) * | 2009-04-23 | 2012-02-29 | 霍万鹏 | Liquid molecular bond bursting device |
| CN101838346B (en) * | 2010-05-20 | 2012-05-23 | 广西工学院 | Method for preparing chitosan |
| CN102633350B (en) * | 2012-04-23 | 2013-11-06 | 西安交通大学 | Method for recycling excessive oxygen and carbon dioxide in supercritical water oxidation system |
| CN105314805B (en) * | 2015-12-11 | 2017-11-10 | 黑龙江省科学院高技术研究院 | A kind of device, method and product that fuel oil is manufactured with sludge |
| CN109943313B (en) * | 2019-04-23 | 2021-03-12 | 中国石油大学(华东) | Equipment and method for preparing supercritical carbon dioxide microemulsion and fly ash particle compound dispersion |
| CN116042302B (en) * | 2022-05-04 | 2024-03-26 | 新纪元食品科技(佛山)有限公司 | Cavitation treatment process for complete material |
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| CN1280875A (en) * | 1999-06-30 | 2001-01-24 | 刘士群 | Process and equipment for preparing microparticles with supercritical back extractant |
| US20040178529A1 (en) * | 2001-07-02 | 2004-09-16 | Ernesto Reverchon | Process for the production of micro and/or nano particles |
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