CN101441030B - Integrated atomizing freeze drying equipment - Google Patents
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- CN101441030B CN101441030B CN200810189058XA CN200810189058A CN101441030B CN 101441030 B CN101441030 B CN 101441030B CN 200810189058X A CN200810189058X A CN 200810189058XA CN 200810189058 A CN200810189058 A CN 200810189058A CN 101441030 B CN101441030 B CN 101441030B
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Abstract
The invention relates to an integrated atomizing freeze drying equipment belonging to novel solid dispersoid preparation technique. The equipment comprises a freeze drying chamber with a freeze device for cooling, the freeze drying chamber is provided with a vacuum pumping opening, a liquid outlet, a sprayer and a refrigerant inlet, and the sprayer is connected with a liquid material source. The freeze drying chamber is formed by a mutual communicated freeze grain accommodation chamber and a freeze chamber, and the freeze grain accommodation chamber is provided with a collector and a space adjustment device. An atomizing freeze device and a freeze drying device are integrated by the integrated atomizing freeze drying equipment of the invention, so that an atomizing freeze process and a freeze drying process can be automatically executed in the same equipment, after the atomizing freeze process, the freeze drying process can be executed without manually transferring the freeze grains, thereby realizing operation integration and automation. The whole operation flow is easy and simple, which facilitates users as well as reduces the operation danger, strengthens the occupational safety protection, and enables industry automation to be realized.
Description
Technical field
The present invention relates to atomizing freeze drying equipment, belong to new solid dispersions technology of preparing, be mainly used in high added values such as slightly water-soluble medicine, biotechnology goods product.
Background technology
At present, the solid dispersions technology of preparing is widely used in the drug research field.This technology is to wait by crystalline form, particle diameter, porosity and the specific area that changes material grains to realize.Traditional solid dispersions technology of preparing comprises fusion method, solvent method, polishing, freeze-drying and spray drying process etc.Fusion method need form supersaturated solution, solvent method needs solvent volatilization fast in a large number, and spray drying process needs wink-dry medicine carrying drop, these three kinds of temperature that method is all had relatively high expectations, can quicken the degraded of medicine, and the volatilization of organic solvent can cause environmental pollution again, so be not suitable for the medicine of handling thermal sensitivity.Polishing is common mechanical micronization method, and fricative heat effect in the grinding and mechanism can cause the degraded of part effective ingredient too.Though freeze-drying has been got rid of the problem of being heated and rubbing, its preparation is the slow refrigerating process of a large amount of feed liquids, the not ideal enough and easy crystallization of the dispersity of the powder particle of formation, influence prescription effect.
The main process of general spray chilling technology is gases at high pressure to be become drug solution very little drop and enters rapidly in the spray tank or container that refrigerant (liquid nitrogen) or halocarbon refrigerant (chlorofluorocarbon, fluorocarbon) are housed through sprayer ejection, atomizing.Because rate of heat transfer in low temperature environment is very high, and droplet was solidified in moment (Millisecond), finish spraying after, need carry out vacuum freeze drying and obtain end product.Above when spraying, sprayer can be arranged in the freezing liquid liquid level or be dipped in freezing liquid, be dipped in sprayer in the freezing liquid and will install the solution solidifies that an attemperator prevents to flow through additional and stop up sprayer.When spray process carried out, refrigerant constantly volatilization reduced, and needed constantly to replenish, particularly in the spray process of long, large volume.In using liquid coolant, need constantly to stir, condense into bulk to prevent the new frozen particles that forms with magnetic stirring apparatus.Because the atomizing freeze drying technology is to carry out in low temperature environment, cooling time is very short, so can reduce to greatest extent biological products, as the isostructural destruction of protein, and can form stable solid-state structure fast; On the other hand, because the characteristic of atomizing freeze drying technology makes the product particle have characteristics such as porous, particle diameter is little, specific area is big, therefore can improve the stripping and the bioavilability of part insoluble medicine (as BCSII class medicine).
Present atomizing freeze drying technology can be divided three classes substantially: normal pressure circulation atomizing freeze drying, halohydrocarbon atomizing freeze drying and liquid nitrogen spraying freeze drying.Normal pressure circulation atomizing freeze drying is the industrial technology that relatively is fit to, its process is that the medicine carrying feed liquid is sprayed into the fluid bed that contains dry ice is freezing rapidly, the dry cold air of bottom constantly is blown into to make and solidifies the very fast distillation of solvent, and, be blown into dry cold air by continuous repetitive cycling and obtain final desciccate except that desolvating by Cryo Equipment recovery distillation gas.People such as Briggs and Maxwell has invented halohydrocarbon steam spray Freeze Drying Technique, use chlorofluorocarbon (CFC) or fluorocarbon as cooling agent, the shortcoming of this method is to use CFC to damage ozone layer, though use HFA 134 and HFA 227 can not cause environmental problem, but they can dissolve a part of medicine, the effect of influence prescription.Owing to use halohydrocarbon to have many problems, the researcher changes into and uses liquid nitrogen as cooling agent, has obtained good effect.
Relevant patent about atomizing freeze drying is existing, and these patented technologies have all designed the process of diverse ways realization spray chilling respectively.As U.S. Pat 5475984, it is arranged on the top of instrument with dissimilar feed liquid sprayers, is used to spray the freezing zone of liquid nitrogen stroke around four liquid nitrogen nozzles around it, frozen particles is collected carried out freeze-drying in the container at last.U.S. Pat 5922253 has used a plurality of sprayers to be used for the spraying of feed liquid and liquid nitrogen equally, different is that this inventor uses than relatively large liquid nitrogen, form gathering of liquid nitrogen in the bottom, frozen particles can well be kept in the liquid nitrogen and have agitator to stir and prevent to be condensed into piece.U.S. Pat 7007406, this invention is arranged at the outside with refrigerating chamber, and whole spray chamber is surrounded, and at refrigerating chamber a plurality of circulating refrigerant openings is set and constitutes refrigeration source.The feed liquid drop solidifies in the process that falls and forms frozen particles, collecting granules and freeze-drying at last.
By consulting patent and relevant research in the past, we are not difficult to find, their common drawback is exactly not design and second step---the freeze drying that how reasonably to realize atomizing freeze drying is discussed.And at long-term atomizing freeze drying technological learning with in using, we think that these technological difficulties do not lie in the process which kind of form to realize spray chilling with, and this process can be used different spray chilling technology according to different demands.As being that the feed liquid of solvent is easy to freeze with water, can use the sprayer unit of circulating type, use the not so good or cheap cold-producing medium of refrigeration, to reduce the cold-producing medium consumption, save cost; And, need to use the device that directly sprays in the liquid nitrogen with the feed liquid of pure organic solvent as solvent, reach rapidly and freeze.
After but spraying was finished, the transfer of the particle safety that also has residual refrigerant how will collect and freeze-drying were problems that is worth thinking.The user also will collect frozen particles after finishing spray chilling in the past, volatilized or remove freezing liquid, and the particle of collecting is sent to freeze drying.This process is very loaded down with trivial details, wastes time and energy, and is unfavorable for that the atomizing freeze drying technology is applied to the production of heavy industrialization; Handling and mobile freezing liquid,, easily the user is being caused somatic damage as liquid nitrogen etc., and the accident that easily meets accident.It is a kind of new that this just requires us to develop, whole atomizing freeze drying equipment and technology, spray chilling and freeze drying are integrated as a step, realize integrated, the automation of operation, reduce operational hazards when making things convenient for the user, strengthened the employment security protection, made to be applied to industrial automation and to become possibility.
Summary of the invention
The objective of the invention is in order to solve the existing problem of present atomizing freeze drying equipment, the integrated atomizing freeze drying equipment of a kind of spray chilling and the two-in-one type of freeze drying is provided, can reduce manually-operated, strengthen the employment security protection and be the suitability for industrialized production condition that facilitates.
To achieve these goals, the present invention has adopted following technical scheme: integrated atomizing freeze drying equipment is provided, comprise the freeze drying chamber that cools off by refrigerating plant, this freeze drying chamber is provided with vacuum pumping opening and liquid outlet, and constitute by the frozen particles container cavity and the freezing chamber that are interconnected, described frozen particles container cavity is provided with sprayer and liquid refrigerant inlet, and this sprayer links to each other with the feed liquid source; Wherein, also be provided with in the described frozen particles container cavity be used for the splendid attire liquid refrigerant and collect the collection container of frozen particles and regulate the liquid refrigerant surface of this collection container and sprayer between the adjusting device of distance; Described collection container adopts stainless steel material to make, and its outer wall is connected with the linker of the liquid level that is used to observe the liquid refrigerant in this collection container; Described frozen particles container cavity is made of upper strata sealing plate, lower floor's sealing plate and sealed wall, forms dismountable being tightly connected between the each several part; Described liquid refrigerant inlet comprised be formed on the opening on the sealing plate of described upper strata or this upper strata sealing plate of dismantling after the opening that forms, liquid refrigerant can manually add from above-mentioned opening part; Also be provided with in the described frozen particles container cavity and be used for agitator that the liquid refrigerant in the described collection container is stirred,, guarantee that the particle decentralization is good to prevent that frozen particles is condensed in the spray process; One end of described vacuum pumping opening leads to downwards in the described freezing chamber with being provided with, stops up vavuum pump to prevent some powder that suck the frozen particles container cavity.
This sprayer also can link to each other with high-pressure air source to realize spraying function, and high-pressure air source can be provided by devices such as gas cylinder or air compressors.Refrigerant is a liquid phase, and selecting preferably is to adopt volatilizable free of contamination liquid gases such as liquid nitrogen or liquid carbon dioxide.Described liquid refrigerant inlet also can comprise the spout of automatic input refrigerant, and this spout can link to each other with refrigerant source by the refrigerant pump, the refrigerant pump can adopt self pressure-type refrigerant pump, reciprocating type refrigerant pump or centrifugal refrigerant pump etc.
The indoor ambient parameter inductor that preferably also is provided with of described freeze drying, this ambient parameter inductor is converted into signal of telecommunication input computer with signals such as temperature, pressure, humidity, by computer software build environment parameter-time diagram, be used for observing cryodesiccated process whether normally to carry out.
Described refrigerating plant can adopt ultra low temperature freezer, and the adjustable minimum temperature of this ultra low temperature freezer should reach-110 ℃ at least to guarantee to freeze most of organic solvents.
Above-mentioned integrated atomizing freeze drying equipment is integrated spray chilling device and freeze drying plant, spray chilling process and freezing dry process can automatically be carried out in same set of equipment, need not after the spray chilling process finishes frozen particles shifted and to carry out freezing dry process, realized the integrated and automation of operation, the whole operation flow process is simple, reduce operational hazards when making things convenient for the user, make the possibility that becomes of industrial automation.
To achieve these goals, the present invention is based on identical inventive concept, another integrated atomizing freeze drying equipment also is provided, the frozen particles container cavity of splendid attire liquid refrigerant and the freezing chamber that is communicated with it have been comprised, described frozen particles container cavity is provided with sprayer, described freezing chamber is cooled off by ultra low temperature freezer, and be provided with vacuum orifice and liquid outlet, wherein, described frozen particles container cavity also is provided with liquid refrigerant inlet, spiral agitator and ambient parameter inductor, and the frozen particles that forms behind spray chilling directly rests in the frozen particles container cavity; Described frozen particles container cavity is positioned at the left side of described freezing chamber, and this frozen particles container cavity is connected with described freezing chamber by the connected entrance on its right side.
Description of drawings
Fig. 1 is the structural representation of the embodiment of the invention one;
Fig. 2 is the structural representation of the embodiment of the invention two;
Fig. 3 is the structural representation of the embodiment of the invention three;
Fig. 4, Fig. 5, Fig. 6 are the schematic diagram of three kinds of different spray methods of the present invention.
The specific embodiment
Embodiment one
Fig. 1 is embodiments of the invention one structural representations.The freeze drying chamber of present embodiment is cooled off by refrigerating plant 11, and this freeze drying chamber is made of frozen particles container cavity 30 that is interconnected and freezing chamber 40, and frozen particles container cavity 30 is positioned at the top of freezing chamber 40.Frozen particles container cavity 30 is provided with sprayer 1 and refrigerant inlet 5.Feed liquid source 15 links to each other with sprayer 1 by pipeline 23, by peristaltic pump 14 feed liquid is pumped into sprayer 1, peristaltic pump 14 can adopt the MASTER flex L/S of Cole-ParmerInstrument company, this peristaltic pump 14 can use the flexible pipe of different thicknesses, adjustable flow rates is big, it is stable to flow, and pulse is not obvious; Simultaneously, high-pressure air source 18 connects sprayer 1 and provides spraying required gases at high pressure for it by gases at high pressure conveyance conduit 21, use pressure limiting valve 17 to regulate the atomisation pressure size, gases at high pressure can adopt high-pressure nitrogen bottle to provide, and also can use air compressor.Sprayer 1 can adopt two fluid spray devices on the spray-drying instrument B-290 of similar B ü chi company, this sprayer 1 has two ad hoc interfaces, link to each other with hot water circuit device 13 by pipeline 24, to guarantee that sprayer 1 keeps higher temperature and not frozen obstruction in whole spray process.Feed liquid source 15, high-pressure air source 18 and hot water circuit device 13 are respectively by pipeline and sprayer 1 constitute one separately.
Frozen particles container cavity 30 is made of upper strata sealing plate 3, lower floor's sealing plate 9 and sealed wall 25, each several part is made by the organic plastics of anti-vacuum pressure, and be and removably connect, the material of good seal performance such as the junction use rubber of upper strata sealing plate 3, lower floor's sealing plate 9 and sealed wall 25 is airtight, can smear vaseline to strengthen airtight effect.Two spiral agitators 2 are installed on upper strata sealing plate 3, constantly stir to stop the cohesion of particle in the spray process, and spiral agitator 2 can use OST 20 digital of IKAWerke company.Ambient parameter inductor 4 is fixed in the bottom of upper strata sealing plate 3, is connected with computer by data wire, derives signal and build environment parameter-time diagrams such as temperature, pressure, humidity.Freezing liquid pump 19 and frozen liq jar 20 insert in the frozen particles container cavity 30 by pipeline 22 and freezing liquid import 5, freezing liquid pump 19 and frozen liq jar 20 can adopt AirLiquid TP35 from pressure low-temperature storage jar, by increasing pressure freezing liquid are pumped in the collection container 6.Collection container 6 adopts corrosion resistant stainless steel material to make, its outer wall connects a linker 7 observing what of freezing liquids in the collection container 6 at any time, and height adjuster 8 can be regulated the distance between the interior freezing liquid surface of sprayer 1 and collection container 6 easily.
Ultra low temperature freezer 11 is positioned at the bottom of complete equipment, the freeze drying after finishing that is used to spray of the freezing chambers 40 in the ultra low temperature freezer 11.In lower floor's sealing plate 9, be provided with connected entrance 31 and vacuum orifice 10, connected entrance 31 is communicated with frozen particles container cavity 30 with freezing chamber 40, one end of vacuum orifice 10 is positioned at freezing chamber 40 downwards, prevent that some powder that suck frozen particles container cavity 30 from stopping up vavuum pump 16, the other end links to each other with vavuum pump 16 by pipeline.Freezing chamber 40 bottoms are provided with liquid outlet 12, wash the solvent that is frozen in the freezing chamber 40 after freeze-drying is finished, and are discharged by liquid outlet 12.The design temperature of ultra low temperature freezer 11 should be able to reach-110 ℃, can freezing rapidly most of organic solvent, and ultra low temperature freezer 11 and fluid pipeline should be made by the metal material of organic solvent-resistant corrosion.
Adopt the spray-freezing drying method of above-mentioned atomizing freeze drying equipment as follows:
One, preparation feed liquid.Feed liquid is made of effective ingredient and mixed solvent, and can add various excipient substances.Effective ingredient comprises range protein, peptide class and chemical synthetic drug; Mixed solvent can be made up of one or more mixing of following solvent: water, ethanol, toluene, ethyl acetate, DMSO, DMF, methyl alcohol, acetonitrile, n-butanol, the tert-butyl alcohol or other organic or inorganic solvents; Excipient substance comprises: other polymer such as the polysaccharide of various molecular weight, polypeptide, polyester, polyanhydride, polyethers, polyglycolide (PLGA), PLA (PLA), PCL (PCL), polyethylene glycol (PEG), polyvinylpyrrolidone (PVP) and shitosan.
At first should seek suitable solvent or mixed solvent according to the character of compound used therefor or albumen, as water-ethanol, water-ethanol-n-butanol or various cushioning liquid etc.Preparation concentration suitable solution is the key that the spraying sample is prepared, and the too big or solution of concentration is thickness too, is unfavorable for spray chilling, and caking phenomenon easily takes place; The too little solvent of wasting again of concentration consumes freezing liquid.In general, solution should be clarified, and could guarantee the solid frozen particles stable homogeneous that spray chilling obtains like this, finally obtains the good solid dispersions of dispersity.Unless compound or albumen are difficult to molten or can not find appropriate organic solvent, generally do not recommend to use suspension, before the formulated suspension, solid particle should be able to be crossed 200 mesh sieves.
Two, the operating procedure of atomizing freeze drying equipment.
1. connect each pipeline, connect instrument power source, open 13 pairs of sprayers of hot water circuit device 1 earlier and carry out preheating, temperature transfers to 60 ℃, can reach in general 5-10 minute.In preheating, open freezing liquid pump 19, the freezing liquid pump 19 in the frozen liq jar 20 is gone in the collection container 6 of frozen particles container cavity 30, observe liquid level, treat that freezing liquid is added to suitable height and closes freezing liquid pump 19 by linker 7.The distance of using height adjuster 8 to regulate between sprayer 1 and the freezing liquid level is generally 10-15cm.
2. open high-pressure air source 18, adjust pressure limiting valve 17,, get final product between the pressure 0.5-3bar for general settled solution to suitable atomisation pressure.After feeding gases at high pressure, regulate peristaltic pump 14 and spiral agitator 2 to proper speed and startup, feed liquid is ejected into the freezing liquid from sprayer 1 immediately, and moment is frozen into solid particle and is in the continuous stirring to prevent cohesion.In the process of spraying, note observing the height of liquid level in the linker 7, if liquid level is lower than scale, then should in time opens freezing liquid pump 19 and add freezing liquid.
3. after the spray chilling of feed liquid is finished, close peristaltic pump 14, high-pressure air source 18 and hot water circuit device 13, extract sprayer 1, open ultra low temperature freezer 11 when closing the switch of freezing liquid import 5, regulate temperature (should be lower than the solvent for use fusing point).After treating that most of residual freezing liquid volatilizes,, open vavuum pump 16 and bleed with the circular hole of plug jam-pack insertion sprayer 1.Whether ambient parameter inductor 4 is transferred to computer with signals such as the temperature measured, pressure, humidity, observe pressure and show and normally descend then answer shutdown inspection where to leak gas as undesired decline.Under the normal condition, the decline that pressure (is generally less than 30 minutes) through after a while can be stable at low numerical value (normally being lower than 100pa).
4。Through freeze drying after a while, the solvent in the frozen particles distils under the vacuum and low temperature condition and is condensed into solid again in freezing chamber 40 bottoms, remaining dry good powder particle in the collection container 6, thus realize separating between solvent and the active ingredient.Close vavuum pump 16 and ultra low temperature freezer 11, slowly open the switch venting of vacuum orifice 10, take out collection container 6 and collect dried powders, to make the solvent melts that is condensed into solid be liquid and discharged by liquid outlet 12, cleans freezing chamber 40 at last.
Embodiment two
Fig. 2 is embodiments of the invention two structural representations, and external equipments such as vavuum pump, high-pressure air source, frozen liq jar, peristaltic pump and hot water circuit device no longer describe in detail with embodiment one herein.
As shown in Figure 2, the freeze drying chamber of present embodiment is made of frozen particles container cavity 50 that is interconnected and freezing chamber 60, and frozen particles container cavity 50 is positioned at the left side of freezing chamber 60.Sprayer 1, spiral agitator 2, ambient parameter inductor 4 and freezing liquid import 5 are arranged in frozen particles container cavity 50, and collaborative work realizes the spray chilling of feed liquid with embodiment one.And being provided with the connected entrance 51 that is communicated with freezing chamber 60 on the right side of frozen particles container cavity 50, freezing chamber 60 is equally by ultra low temperature freezer 11 coolings, and is provided with vacuum orifice 10 and liquid outlet 12 is used to the freeze drying later of spraying.
Embodiment three
Fig. 3 is embodiments of the invention three structural representations, and external equipments such as vavuum pump, high-pressure air source, frozen liq jar, peristaltic pump and hot water circuit device no longer describe in detail with embodiment one herein.
As shown in Figure 3, present embodiment is that spray chilling chamber 70 and freeze drying chamber 80 are separated with the maximum difference of embodiment one, two, and the connected entrance place between them is provided with such as baffle plate 26 valvings such as grade, but still one step of operation is finished, and is simple.Sprayer 1, spiral agitator 2 and freezing liquid import 5 are arranged in spray chilling chamber 70 and carry out spray chilling, and ambient parameter inductor 4 is installed in the freeze drying chamber 80, and this moment, baffle plate 26 was closed.After spraying is finished, two baffle plates 26 are removed, frozen particles and residual a small amount of liquid nitrogen since the effect of gravity flow into automatically in the freeze drying chamber 80, it is after 80s to treat to enter freeze drying chamber fully, close baffle plate 26, open ultra low temperature freezer 11, vacuum orifice 10 and liquid outlet 12 and carry out freeze drying, utilize ambient parameters such as 4 pairs of temperature of ambient parameter inductor, pressure, humidity to monitor in real time in the freezing dry process.
Fig. 4, Fig. 5 represent three kinds of different Sprayables of the present invention respectively with Fig. 6: the freezing liquid internal spraying, spray and spray around freezing liquid in the freezing liquid top.Wherein, Fig. 4 carries out spray chilling by regulating how much making in the sprayer 1 immersion freezing liquid 27 of height adjuster, sprayer height or freezing liquid; Fig. 5 carries out spray chilling by the liquid level top that how much makes sprayer 1 be positioned at freezing liquid 27 of regulating height adjuster, sprayer height or freezing liquid; Among Fig. 6, the both sides of sprayer 1 are respectively freezing liquid nozzles 28, are used for the freezing liquid ejection, make the formation of whole spray chilling chamber and reach a lower temperature, and the freezing liquid of ejection and the frozen particles of condensing flow in the freezing liquid 27 of bottoms along funnel 29.
Claims (2)
1. integrated atomizing freeze drying equipment, comprise the freeze drying chamber (30,40) that cools off by refrigerating plant (11), this freeze drying chamber (30,40) is provided with vacuum pumping opening (10) and liquid outlet (12), and by frozen particles container cavity (30) that is interconnected and freezing chamber (40) formation, it is characterized in that: described frozen particles container cavity (30) also is provided with sprayer (1) and liquid refrigerant inlet (5), and this sprayer (1) links to each other with feed liquid source (15);
Wherein, also be provided with the adjusting device of distance between collection container (6) that is used for the splendid attire liquid refrigerant and collects frozen particles and the liquid refrigerant of regulating this collection container (6) surface and the sprayer (1) in the described frozen particles container cavity (30), described collection container (6) adopts stainless steel material to make, and its outer wall is connected with the linker (7) of the liquid level that is used to observe the liquid refrigerant in this collection container (6);
Described frozen particles container cavity (30) is made of upper strata sealing plate (3), lower floor's sealing plate (9) and sealed wall (25), forms dismountable being tightly connected between the each several part; Described liquid refrigerant inlet (5) has comprised that being formed on being used on the described upper strata sealing plate (3) manually adds the opening of liquid refrigerant or dismantle this upper strata sealing plate (3) opening that is used for manually adding liquid refrigerant of formation afterwards;
Also be provided with in the described frozen particles container cavity (30) and be used for agitator (2) that the liquid refrigerant in the described collection container (6) is stirred;
One end of described vacuum pumping opening (10) leads to downwards in the described freezing chamber (40) with being provided with.
2. integrated atomizing freeze drying equipment, the frozen particles container cavity (50) of splendid attire liquid refrigerant and the freezing chamber (60) that is communicated with it have been comprised, described frozen particles container cavity (50) is provided with sprayer (1), described freezing chamber (60) is cooled off by ultra low temperature freezer (11), and be provided with vacuum orifice (10) and liquid outlet (12), it is characterized in that: described frozen particles container cavity (50) also is provided with liquid refrigerant inlet (5), spiral agitator (2) and ambient parameter inductor (4), the frozen particles that forms behind spray chilling directly rest in the frozen particles container cavity (50); Described frozen particles container cavity (50) is positioned at the left side of described freezing chamber (60), and this frozen particles container cavity (50) is connected with described freezing chamber (60) by the connected entrance (51) on its right side.
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| CN200810189058XA CN101441030B (en) | 2008-12-16 | 2008-12-16 | Integrated atomizing freeze drying equipment |
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| CN200810189058XA CN101441030B (en) | 2008-12-16 | 2008-12-16 | Integrated atomizing freeze drying equipment |
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Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2012018320A1 (en) | 2010-08-04 | 2012-02-09 | Ima Life North America Inc. | Bulk freeze drying using spray freezing and stirred drying |
| US9945611B2 (en) | 2010-08-04 | 2018-04-17 | Ima Life North America Inc. | Bulk freeze drying using spray freezing and agitated drying |
| CN104771417A (en) * | 2015-04-10 | 2015-07-15 | 深圳市多微生保健食品有限公司 | Probiotics powder and production method thereof |
| CN106268503B (en) * | 2015-06-29 | 2020-01-17 | 南京邮电大学 | Liquid nitrogen spray freezing granulation vacuum drying device and working method |
| CN105664513B (en) * | 2016-02-02 | 2017-11-14 | 安徽农业大学 | A kind of spray chilling lyophilization machine |
| CN106722503B (en) * | 2017-02-15 | 2020-06-16 | 大兴安岭中北农业科技股份有限公司 | Preparation method of blueberry powder |
| CN108651937B (en) * | 2018-04-20 | 2021-12-24 | 大连工业大学 | Method for producing soup-stock seasoning powder based on ultrasonic spray freeze drying |
| CN108709369A (en) * | 2018-04-20 | 2018-10-26 | 大连工业大学 | A kind of ultrasonic atomization freeze drying plant |
| CN109771701A (en) * | 2019-02-11 | 2019-05-21 | 赵延延 | A kind of preparation method of soft biological 3D printing material |
| CN110523096B (en) * | 2019-07-24 | 2022-03-04 | 天津科技大学 | Large-scale drying device and method capable of shortening probiotic feed liquid freeze-drying time |
| CN113289549A (en) * | 2021-05-17 | 2021-08-24 | 西安工业大学 | Spray freeze drying instrument capable of controlling particle size of nano powder |
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