CN101391156A - Fine particle preparation device using supercritical fluid quick expansion - Google Patents
Fine particle preparation device using supercritical fluid quick expansion Download PDFInfo
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- CN101391156A CN101391156A CNA2008102185435A CN200810218543A CN101391156A CN 101391156 A CN101391156 A CN 101391156A CN A2008102185435 A CNA2008102185435 A CN A2008102185435A CN 200810218543 A CN200810218543 A CN 200810218543A CN 101391156 A CN101391156 A CN 101391156A
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Abstract
Disclosed is an apparatus for preparing fine particles through rapid expansion of supercritical fluids, which is composed of a CO2 solvent bottle, a condensation compressor, a solvent storage tank, a high pressure pump, an extraction kettle, a nozzle, a crystallization kettle, an exhaust and collection device and a plurality of regulating and controlling valves. The apparatus adopts the connection and operation according to the following process: a CO2 solvent enters the condensation compressor from the CO2 solvent bottle by passing through a switch valve V1 and then is output to the solvent storage tank after being cooled, then is output to the high pressure pump for compression and then output to the extraction kettle through a regulating valve V2 to extract (or dissolve) materials in a material container of the extraction kettle, thereby forming a supercritical fluid which is then sprayed into the crystallization kettle via the nozzle by passing through a nozzle control valve V3, the solute in the fluid is separated out in the form of ultrafine particles after decompression expansion, and the solvent is discharged to the air via the exhaust and collection device by passing through an exhaust control valve V5. The apparatus overcomes a plurality of defects of the existing decompression expansion device, and can properly meet the requirements on process quality of the rapid expansion of supercritical solutions (RESS).
Description
Technical field
The present invention relates to a kind of device for preparing subparticle by the using supercritical fluid quick expansion process.
Background technology
Supercritical solution fast expansion (Rapid Expansion of Supercritical Solution) is called for short RESS.Be the supercritical fluid that is dissolved with solute under uniform temperature and the certain pressure, carbon dioxide normally, after the decompression of special nozzle rapid expanding, solute solubility descends rapidly and separates out with particulate, fiber and film crystal form.The shape of precipitating thing, size and distributing depends primarily on temperature, pressure drop before and after expanding, and (the general pressure of supercritical fluid is between 20Mpa～40Mpa, the rapid expanding decompression of nozzle ejection back reduces near normal pressure), various factors such as carbon dioxide flow velocity, nozzle form.
In recent years, along with the development of supercritical liquid extraction technique, both at home and abroad with the existing a large amount of reports of pharmaceutically active ingredient in the supercritical extract.The further reprocessing of active ingredient (extract), make the preparation formulation of determined curative effect, become the problem that people pay close attention to, particularly in the technological process of making solids such as capsule, tablet, granule, ointment, semisolid preparation, extract need be made graininess earlier, and the more little absorption that helps human body to active ingredient more of particle diameter.The supercritical solution fast expansion is sprayed into active ingredient (extract) process of fine particles such as particulate, fiber and film crystal exactly.Present existing using supercritical fluid quick expansion prepares the device of minuteness particle, needing directly extract to be dissolved in as solute becomes supercritical solution in the supercritical fluid, again by the nozzle puffing, form the superfine powder product, restricted to the material that is used to prepare the superfine powder product, and there are a lot of defectives in its puffing equipment, separate out the device pressure transient as decompression, the ejecta particle diameter is inhomogeneous, drying effect is poor, lack effective exhaust gas filter equipment, the mist that exhaust outlet is discharged contains salvage stores etc., can not satisfy the processing quality requirement of supercritical solution fast expansion (RESS).
Summary of the invention
The objective of the invention is to propose a kind ofly can carry out supercritical CO to the material that is used to prepare the superfine powder product
2Extraction also becomes extract dissolving supercritical solution and by the nozzle puffing, forms the superfine powder product, can better satisfy the fine particle preparation device using supercritical fluid quick expansion that the processing quality of supercritical solution fast expansion (RESS) requires.
The technical solution used in the present invention is as follows:
Designed fine particle preparation device using supercritical fluid quick expansion comprises:
One is used for CO
2Solvent is cooled to 0-5 ℃ refrigeration unit, and this refrigeration unit is made up of condensate compressor and solvent tank, and solvent tank is installed in the heat-insulated container that glycerine-aqueous mixtures is housed, and the solvent input of condensate compressor is through switch valve V1 and CO
2Solvent bottle connects, and the solvent input solvent tank after the condensate compressor refrigeration stores;
One is used for CO
2The high-pressure pump of solvent pressurization, the input of this high-pressure pump is connected with described solvent tank output, and the high pressure delivery side of pump is connected with the input of control valve V2;
One is used for the super CO that faces
2Extraction or dissolving material active ingredient become the extraction kettle of supercritical fluid, this extraction kettle is with the tank chuck outward, this tank chuck is connected with a constant temperature water tank, water in constant temperature water tank and the tank chuck circulates by circulating pump, stainless steel material tube is housed in the extraction kettle, the solvent input of stainless steel material tube is connected with the output of described control valve V2, and the supercritical fluid output on extraction kettle top is connected with the input of nozzle control valve V3;
One is used for the crystallization kettle of using supercritical fluid quick expansion, the top of this crystallization kettle is provided with nozzle, the bottom is provided with collection cylinder, be with the tank chuck outward, this tank chuck is connected with a constant temperature water tank, and the water in constant temperature water tank and the tank chuck circulates by circulating pump, is provided with the input port of dry gas in the bottom of crystallization kettle, top is provided with exhaust outlet, and the nozzle of described crystallization kettle is connected with the output of described nozzle control valve V3;
One exhaust and gathering-device, this exhaust and gathering-device are laid with dress column type in the stainless steel cylinder of steam vent by outer wall the Nylon Bag that aeration is arranged constitutes, and the sack of this column type Nylon Bag is connected with the exhaust outlet on described crystallization kettle top by gas exhausting valve V5.
The further technical measures of the present invention comprise:
(1) the buzzing alarm pressure gauge is installed above described crystallization kettle, by setting the alarm pressure parameter, test crystallization kettle internal pressure can guarantee operation continuously under the condition of constant voltage (voltage drop value is stable).
(2) a sleeving temperature display unit is installed on crystallization kettle.
The present invention carries out drying by feeding dry gas (nitrogen) to crystallization kettle to the subparticle that forms, dry gas (nitrogen) is by the input of dry gas input port, crystallization kettle bottom, and this dry gas input port is connected with nitrogen cylinder through gas switch valve V4 by gas pipeline.
Use the process route of apparatus of the present invention as follows:
Carbon dioxide → refrigeration → storage tank → pressurization → extraction → ejection → nitrogen drying → collection material → row's mist → collection material.
CO
2Solvent is by CO
2Solvent bottle enters the condensate compressor refrigeration through switch valve V1, condensate compressor control temperature is at 0-5 ℃, solvent input solvent tank through refrigeration, import the high-pressure pump pressurization again, again in control valve V2 input extraction kettle, make extraction kettle reach required pressure by control time and high-pressure pump rotating speed, material in the extraction kettle material tube is extracted (or dissolving), form supercritical fluid, open nozzle control valve V3, supercritical fluid sprays into crystallization kettle through nozzle, puffing, the solute in the fluid is separated out with the ultrafine dust form, and solvent is discharged in the air through exhaust and gathering-device by gas exhausting valve V5, pressure in the crystallization kettle can be regulated by control valve V3 and gas exhausting valve V5 switch size, obtains particle at last in collection cylinder; Open gas switch valve V4, nitrogen (dry gas) is blown into by the crystallization kettle bottom, plays the drying particulate effect.
Useful technique effect of the present invention is as follows:
1, will surpass and face CO
2Solvent imports extraction kettle material is extracted (or dissolving), both the active ingredient of material can be extracted and dissolve, and can directly dissolve solute again, has enlarged the range of application of equipment;
2, extraction kettle and crystallization kettle guaranteeing operation continuously under the condition of constant temperature (temperature value stable), and by the adjusting control to each valve, can guarantee effectively that extraction kettle and crystallization kettle move by constant temperature water tank under constant pressure;
3, nitrogen (dry gas) import is arranged on the crystallization kettle lower end, with the supercritical fluid that sprays into crystallization kettle, form two opposite each other airflow directions, the speed that the supercritical fluid ejecta is fallen slows down, prolong drying time, plays the particle effect of better drying.
3, the mist exhaust apparatus is set to exhaust and gathering-device.The supercritical solution fast expansion is a dynamic process, and mist is in exhaust condition by filter material always in its running.The filtering material of existing apparatus generally adopts conventional silicon pottery sintered plate, and this silicon pottery sintered plate divides different model and aperture, and the gaseous mixture physical efficiency is passed through, and works the fine particle effect of holding back.Along with the prolongation of operation hours, the gathering of silicon pottery sintered plate plate face fine particle, aeration reduces, and causes the obstruction of silicon pottery sintered plate, and the crystallization kettle internal pressure is increased, and the pressure drop parameter changes.The present invention adopts at the exhaust outlet on crystallization kettle top the exhaust that the Nylon Bag that aeration is arranged of dress column type in the stainless steel cylinder that is laid with steam vent by outer wall constitutes and the scheme of gathering-device is installed, and to be Nylon Bag be easy to get, easily processing, easily select the material in different apertures, aeration better as filtering material in its effect one; The 2nd, enlarged filter area, be difficult for stopping up, prolonged the equipment continuous operating time; The 3rd, Nylon Bag cleans easily; The 4th, the effect of collecting salvage stores when Nylon Bag can play the mist discharging has avoided material to discharge from exhaust outlet with mist.
4, device of the present invention has overcome existing puffing equipment and has had a lot of defectives, can make decompression separate out device and keep steady pressure, make the ejecta particle diameter even, drying effect is good, satisfies the processing quality requirement of supercritical solution fast expansion (RESS) preferably.
Description of drawings
Fig. 1 is the structure and the process flow diagram of fine particle preparation device using supercritical fluid quick expansion of the present invention.
The specific embodiment
Embodiment
As shown in Figure 1, the structure of fine particle preparation device using supercritical fluid quick expansion embodiment of the present invention is by CO
2Solvent bottle 1, condensate compressor 2, solvent tank 3, high-pressure pump 4, extraction kettle 5, nozzle 6, crystallization kettle 7, exhaust and gathering-device 8 and some adjusting control valve doors constitute; Condensate compressor 2 and solvent tank 3 constitute refrigeration unit; The described extraction kettle 5 outer tank chucks 51 that are with, this tank chuck 51 is connected with a constant temperature water tank 9, water in constant temperature water tank 9 and the tank chuck 51 circulates by circulating pump, and stainless steel material tube 52 is housed in extraction kettle, also is provided with electro connecting pressure gauge 53 on extraction kettle; The described crystallization kettle 7 outer tank chucks 71 that are with, this this tank chuck 71 is connected with a constant temperature water tank 11, water in constant temperature water tank 11 and the tank chuck 71 circulates by circulating pump, be provided with collection cylinder 72 in the bottom of crystallization kettle 7, be provided with the input port of dry gas in the bottom of crystallization kettle 7, top is provided with exhaust outlet, and buzzing alarm pressure gauge 73 also is installed above crystallization kettle 7; Described nozzle 6 is located at the top of crystallization kettle 7; Described exhaust and gathering-device 8 are laid with dress column type in the stainless steel cylinder of steam vent by outer wall the Nylon Bag that aeration is arranged constitutes.The annexation of each parts is as follows in the device: CO
2Solvent bottle 1 is connected with condensate compressor 2 by switch valve V1, condensate compressor 2 is connected with solvent tank 3, the output of solvent tank 3 is connected to the solvent input of high-pressure pump 4, the solvent input of the stainless steel material tube 52 of the solvent output of high-pressure pump 4 in control valve V2 connects into extraction kettle 5, the supercritical fluid output on extraction kettle 5 tops is connected with nozzle 6 through nozzle control valve V3, the input port of the dry gas of crystallization kettle 7 bottoms is connected with nitrogen (dry gas) bottle 10 through gas switch valve V4 by gas pipeline, and the heating of the nitrogen by 11 pairs of inputs of constant temperature water tank, the exhaust outlet on crystallization kettle 7 tops is connected by the sack of the column type Nylon Bag in gas exhausting valve V5 and exhaust and the gathering-device 8.
It is as follows to carry out the operating process that supercritical fluid prepares subparticle with this fine particle preparation device using supercritical fluid quick expansion:
1, behind the logical three phase mains, opens total power switch;
2, cooling: open condensate compressor 2, open cold circulating pump and ice chest temperature switch, 0～5 ℃ of control ice chest temperature;
3, charging: with the material stainless steel material tube 52 of packing into earlier, 5 li of the extraction kettles of again stainless steel material tube 52 being packed into will be noted the sealing of stainless steel material tube 52 and extraction kettle 5 body walls in this step, and the sealing of extraction kettle 5 headkerchieves;
4, heating: open the heater switch of extraction kettle 5 and crystallization kettle 7, and on temperature control instrument, set its temperature parameter separately;
5, air inlet: open CO
2The switch valve V1 of solvent bottle 1 allows CO
2After condensate compressor 2 refrigeration is to 0～5 ℃, enter solvent tank 3, open control valve V2 again, allow CO
2Enter extraction kettle;
6, boost: after extraction kettle 5 temperature reach setting value, open high-pressure pump 4, begin pressurization, when extracting pressure reaches required pressure, regulate the high-pressure pump rotating speed and make pressure stability on required pressure;
7, expand: open nozzle control valve V3, supercritical fluid sprays into crystallization kettle 7 and carries out the rapid expanding granulation, regulate the control valve V2 and the nozzle control valve V3 valve of high-pressure pump simultaneously, make the pressure stability of extraction kettle 5 on required pressure, (select whether to open the gas switch valve V4 of nitrogen cylinder according to the particle degree of drying);
8, discharging: after granulation is finished, close the control valve V2 and the nozzle control valve V3 valve of high-pressure pump, collect the particle in the crystallization kettle 7;
9, exhaust: close each control power supply earlier, close general supply again.Close CO
2The switch valve V1 of bottle opens extraction kettle 5 drain taps, treat the emptying of extraction kettle pressure after, open the headkerchief of extraction kettle, the extract barrel is poured out material.
Claims (3)
1, a kind of fine particle preparation device using supercritical fluid quick expansion is characterized in that comprising:
One is used for CO
2Solvent is cooled to 0-5 ℃ refrigeration unit, this refrigeration unit is made up of condensate compressor (2) and solvent tank (3), solvent tank (3) is installed in the heat-insulated container that glycerine-aqueous mixtures is housed, and the solvent input of condensate compressor (2) is through switch valve (V) and CO
2Solvent bottle (1) connects, and the solvent input solvent tank (3) after condensate compressor (2) refrigeration stores;
One is used for CO
2The high-pressure pump (4) of solvent pressurization, the input of this high-pressure pump (4) is connected with described solvent tank (3) output, and the output of high-pressure pump (4) is connected with the input of control valve (V2);
One is used for the super CO that faces
2Extraction or dissolving material active ingredient become the extraction kettle (5) of supercritical fluid, this extraction kettle is with tank chuck (51) outward, this tank chuck (51) is connected with a constant temperature water tank (9), water in constant temperature water tank (9) and the tank chuck (51) circulates by circulating pump, stainless steel material tube (52) is housed in the extraction kettle (5), the solvent input of stainless steel material tube (52) is connected with the output of described control valve (V2), and the supercritical fluid output on extraction kettle (5) top is connected with the input of nozzle control valve (V3);
One is used for the crystallization kettle (7) of using supercritical fluid quick expansion, the top of this crystallization kettle (7) is provided with nozzle (6), the bottom is provided with collection cylinder (72), be with tank chuck (71) outward, this tank chuck (71) is connected with a constant temperature water tank (11), water in constant temperature water tank (11) and the tank chuck (71) circulates by circulating pump, be provided with the input port of dry gas in the bottom of crystallization kettle (7), top is provided with exhaust outlet, and the nozzle (6) of described crystallization kettle (7) is connected with the output of described nozzle control valve (V3);
One exhaust and gathering-device (8), this exhaust and gathering-device (8) are laid with dress column type in the stainless steel cylinder of steam vent by outer wall the Nylon Bag that aeration is arranged constitutes, and the sack of this column type Nylon Bag is connected with the exhaust outlet on described crystallization kettle (7) top by gas exhausting valve (V5).
2, fine particle preparation device using supercritical fluid quick expansion according to claim 1 is characterized in that described crystallization kettle (7) top is equipped with buzzing alarm pressure gauge (73).
3, fine particle preparation device using supercritical fluid quick expansion according to claim 1 is characterized in that the input port of dry gas of the bottom of described crystallization kettle (7) is connected with nitrogen cylinder (1 θ) through gas switch valve (V4) by gas pipeline.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008102185435A CN101391156A (en) | 2008-10-22 | 2008-10-22 | Fine particle preparation device using supercritical fluid quick expansion |
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| Application Number | Priority Date | Filing Date | Title |
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| CNA2008102185435A CN101391156A (en) | 2008-10-22 | 2008-10-22 | Fine particle preparation device using supercritical fluid quick expansion |
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| CNA2008102185435A Pending CN101391156A (en) | 2008-10-22 | 2008-10-22 | Fine particle preparation device using supercritical fluid quick expansion |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104694014A (en) * | 2015-02-15 | 2015-06-10 | 广西大学 | Method and device for preparing rosin ester by coupling catalytic esterification and separation |
| CN104950960A (en) * | 2015-06-17 | 2015-09-30 | 长春工业大学 | Method for accurately controlling temperature and pressure of supercritical extraction process |
| CN105344129A (en) * | 2015-12-07 | 2016-02-24 | 江苏知原药业有限公司 | Traditional Chinese medicine extraction device |
| CN108244389A (en) * | 2018-01-30 | 2018-07-06 | 广西壮族自治区畜牧研究所 | It is a kind of using leaflet white popinac as broiler fodder of raw material and preparation method thereof |
| CN109730929A (en) * | 2019-03-11 | 2019-05-10 | 塔尔普(北京)制药技术有限公司 | A kind of medicament nano granulation combined nozzle |
| CN110478246A (en) * | 2019-08-09 | 2019-11-22 | 厦门大学 | A kind of pure medicine nano particle preparation facilities and method |
| WO2021152204A1 (en) * | 2020-01-29 | 2021-08-05 | Nanoform Finland Oyj | System and method to produce particles of organic substances |
| CN114605368A (en) * | 2022-03-27 | 2022-06-10 | 中国药科大学 | Method for preparing luteolin superfine particles by applying supercritical fluid enhanced solution dispersion technology |
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2008
- 2008-10-22 CN CNA2008102185435A patent/CN101391156A/en active Pending
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104694014A (en) * | 2015-02-15 | 2015-06-10 | 广西大学 | Method and device for preparing rosin ester by coupling catalytic esterification and separation |
| CN104950960A (en) * | 2015-06-17 | 2015-09-30 | 长春工业大学 | Method for accurately controlling temperature and pressure of supercritical extraction process |
| CN105344129A (en) * | 2015-12-07 | 2016-02-24 | 江苏知原药业有限公司 | Traditional Chinese medicine extraction device |
| CN108244389A (en) * | 2018-01-30 | 2018-07-06 | 广西壮族自治区畜牧研究所 | It is a kind of using leaflet white popinac as broiler fodder of raw material and preparation method thereof |
| CN108244389B (en) * | 2018-01-30 | 2020-09-01 | 广西壮族自治区畜牧研究所 | Broiler feed taking albizzia julibrissin as raw material and preparation method thereof |
| CN109730929A (en) * | 2019-03-11 | 2019-05-10 | 塔尔普(北京)制药技术有限公司 | A kind of medicament nano granulation combined nozzle |
| CN109730929B (en) * | 2019-03-11 | 2024-05-28 | 塔尔普(北京)制药技术有限公司 | Combined spray nozzle for drug nano-granulation |
| CN110478246A (en) * | 2019-08-09 | 2019-11-22 | 厦门大学 | A kind of pure medicine nano particle preparation facilities and method |
| WO2021152204A1 (en) * | 2020-01-29 | 2021-08-05 | Nanoform Finland Oyj | System and method to produce particles of organic substances |
| US11766650B2 (en) | 2020-01-29 | 2023-09-26 | Nanoform Finland Oyj | System and method to produce particles of organic substances |
| CN114605368A (en) * | 2022-03-27 | 2022-06-10 | 中国药科大学 | Method for preparing luteolin superfine particles by applying supercritical fluid enhanced solution dispersion technology |
| CN114605368B (en) * | 2022-03-27 | 2023-05-26 | 中国药科大学 | Method for preparing luteolin ultrafine particles by using supercritical fluid enhanced solution dispersion technology |
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Open date: 20090325 |