US3740860A - Freeze drying method and apparatus - Google Patents

Freeze drying method and apparatus Download PDF

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Publication number
US3740860A
US3740860A US00276556A US3740860DA US3740860A US 3740860 A US3740860 A US 3740860A US 00276556 A US00276556 A US 00276556A US 3740860D A US3740860D A US 3740860DA US 3740860 A US3740860 A US 3740860A
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product
compartment
freezing compartment
pressure
freezing
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H Smith
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SMITHERM IND INC US
SMITHERM INDUSTRIES
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SMITHERM INDUSTRIES
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    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F26—DRYING
    • F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
    • F26B5/00—Drying solid materials or objects by processes not involving the application of heat
    • F26B5/04—Drying solid materials or objects by processes not involving the application of heat by evaporation or sublimation of moisture under reduced pressure, e.g. in a vacuum
    • F26B5/06—Drying solid materials or objects by processes not involving the application of heat by evaporation or sublimation of moisture under reduced pressure, e.g. in a vacuum the process involving freezing

Definitions

  • This invention relates to freeze drying and, more particularly, to novel, improved methods and apparatus for carrying out freeze drying on a continuuos basis.
  • Continuous type freeze dryers are disclosed in my prior U.S. Pat. Nos. 2,515,098 issued July I1, 1959 and 3,226,169 issued Aug. 6, 1966.
  • the material to be dried is frozen, introduced into a vacuum chamber, and deposited on one end of an endless belt conveyor.
  • moisture is evolved from it by radiant heat emitted from one or more radiators adjacent the material bearing leg of the conveyor.
  • the dried material is removed from the conveyor belt and then from the vacuum chamber.
  • the product is first converted into a frozen powder which is introduced into the vacuum vessel and spread onto the conveyor.
  • Considerable difficulty may be experienced with the loose particles bouncing or flying off the conveyor when the product is introduced into the vacuum vessel in powdered form. This can result in a build-up of powdered product within the vacuum vessel great enough to materially reduce the efficiency and/or prevent proper operation of the apparatus.
  • the layer of product must be relatively thick for the apparatus to handle an acceptable volume of material. This makes it diffucult for radiant energy to penetrate to the center of the product layer. Also, a layer of powdered material has low thermal conductivity. Because of these properties of the layer, the removal of the moisture from the product cannot be accomplished with high efficiency.
  • the formation of the product into a thin, coherent layer solved the problem of loose particles flying off the conveyor and building up inside the vacuum vessel. This also increased the drying efficiency as the layer was both reduced in thickness and made more conductive.
  • the product is introduced into what I term a freezing compartment in an evacuated vacuum vessel and is formed into a layer on an endless belt or other conveyor.
  • the conveyor is then cooled or chilled to freeze the product to it.
  • the pressure in the freezing compartment is maintained above the vapor pressure of the product so that volatiles will not evolve from it as it is being spread on and frozen to the conveyor. This also keeps the product from turning to icy or snowlike particles while it is being introduced into and spread on the conveyor.
  • the frozen product is conducted by the conveyor into and through a drying compartment where the pressure is maintained at a level much lower than that in the freezing compartment; viz., below the triple point of water.
  • the moisture is sublimed from the product by applying radiant heat to it as described in my already issued patents. Then the dried product is removed from the drying compartment and the vacuum vessel.
  • FIG. I - is a schematic illustration of a freeze drying system constructed in accord with the principles of the present invention with certain components including a vapor producing system eliminated for the sake of clary;
  • FIG. 2 is a generally diagrammatic longitudinal section through a vacuum vessel employed in the system of FIG. 1;
  • FIG. 3 is a section through the vacuum vessel taken substantially along line 33 of FIG. 2;
  • FIG..4 is a fragment of FIG. 3 to an enlarged scale, showing in more detail an arrangement for distributing a product to be dried on an endless conveyor housed in the vacuum vessel;
  • FIG. 5 is a section through part of the product distributing arrangement, taken substantially along line 5-5 of FIG. 4;
  • FIG. 6 is a section through a cooled roll-located at the discharge end of a drying compartment in the vacuum vessel.
  • FIG. 7 is a section showing an arrangement for freezing the product onto the conveyor in a freezing compartment in the vacuum vessel and is taken substantially along line 77 of FIG. 2.
  • a liquid or semiliquid product is frozen in a thin, uniform layer on a conveyor in an environment in which the pressure is high enough to keep volatiles from evolving from the product.
  • the frozen layer of product is then conveyed into a drying chamber where the pressure is below the triple point of water.
  • radiant heat is applied to the frozen product to sublime the moisture from it.
  • the dried product is cooled, removed from the conveyor, and discharged from the drying chamber.
  • FIG. 1 illustrates freeze drying apparatus 20 including a novel vacuum vessel 22 in which the foregoing steps may be carried out.
  • vacuum vessel 22 includes a shell 24 divided by an insulated, vertical partition 26 into a freezing compartment 28 and a drying compartment 30.
  • Each of the three endless conveyors includes an endless belt 38 which has material bearing and return legs 40 and 42 and is trained around rolls 44 and 46 at opposite ends of the conveyor. One or both of these rolls is driven by an appropriate drive arrangement (not shown) to effect movement of the material bearing leg through the vacuum vessel in the direction shown by arrow 48.
  • each conveyor extends through apertures 50 and 52 in partition 26.
  • Flexible seals 54 are disposed in each aperture 52 above and below the return leg 42 of the conveyor belt 38 to reduce the flow of gases between the freezing and drying compartments 28 and 30.
  • the product to be dried is introduced into vacuum vessel 22 in liquid or semiliq uid form from a receptacle 56 through a main conduit 58.
  • a valve 60 in the main conduit controls the rate at which the product flows into the vacuum vessel.
  • the product flows into one of three longitudinally extending branch conduits 61, 62, and 64. As best shown in FIG. 2, one of these conduits is located above the material bearing leg 40 of each of the three conveyors 32, 34, and 36. Valves 66, 68, and 70 in the branch conduits proportion the product among the three branch conduits.
  • transversely extending headers 72, 74, and 76 which span the material bearing legs 40 of the three conveyors, are connected to the ends of conduits 61, 62, and'64 opposite main conduit 58.
  • Formed in the lower sides of the headers are discharge holes or apertures 78 (see' FIGS. 4 and The product flows from the branch conduits into the headers and then through these apertures onto the material bearing legs 40 of the conveyor belts to form layers 80 of the product thereon.
  • layers 80 will be from one thiry-second to one-sixteenth of an inch thick. In any event, however, the number of apertures 78, their size, and the spacing between them as well as the rate of flow of the product onto the belt and the rate of movement of the latter will be coordinated to produce a layerwhich has the selected thickness and is uniformly thick across the conveyorbelt.
  • the next step in my novel process is to freeze the product to the material bearing leg 40 of the conveyor belt on which it is spread.
  • the exemplary, illustrated arrangement includes three reservoirs 82 having side walls 84 and end walls 86 and an open upper end.
  • One such reservoir is located beneath and immediately adjacent the material bearing leg 40 of each of the three conveyors 32, 34, and 36.
  • An appropriate refrigerant such as a cryohydrate, lithium chloride brine or solution is chilled in a refrigeration unit 88.
  • a refrigeration unit 88 Such units are commercially available and will, accordingly, not be described in detail herein.
  • the cold refrigerant flows through a supply line 90 into a transversely extending header 92 located in the bottom of each reservoir 82. As best shown in FIG. 7, the refrigerant then flows out of the open ends of the header and circulates into contact with the lower side of the conveyor belt material bearing leg 40, reducing its temperature and causing the product to freeze and adhere to the belt. The refrigerant then spills over the side walls 84 of the reservoir into traps 94. From these, the refrigerant is circulated through return conduits 96 (only one of which is shown in FIG. 1) to the refrigeration unit 88, where it is recooled and recirculated.
  • that employed to freeze the proudct to the conveyors need not be of the particular construction illustrated in the drawing.
  • it may be replaced with spray nozzles for projecting the refrigerant against the undersides of the material bearing legs of the conveyor belts.
  • doctor blades, squeeges, etc. may be located adjacent partition 26 to remove from the undersides of the belts any refrigerant which may adhere to them.
  • the product will be instantly reduced to particles as it flows out of the distribution headers. As discussed above, these particles will not stick to the conveyors but will accumulate on the inner surfaces of shell 24, on partition 26, and on other components in the freezing compartment, reducing the efficiency of the operation or stopping it altogether.
  • the pressure is preferably kept at the desired level in freezing compartment 28 by maintinaing an atmosphere of water vapor in it.
  • One arrangement for doing this shown in FIG. 2, includes a water reservoir 98 hav ing an open top. The reservoir is located'in the lower reaches of the freezing compartment. Water is supplied to the reservoir through line 100 and a float type control 102 of conventional construction, keeping water at a selected level in the reservoir.
  • Water is evaporated from the body of liquid in the reservoir at a controlled rate to maintain the pressure in the freezing compartment constant by a conventional resistance heater 104 in the reservoir.
  • the pressure maintained in the freezing compartment will vary, depending primarily upon' the product being dried, although it will always be well below atmospheric pressure.
  • the pressure in this compartment may be maintained at a level on the order of 5 plus mm of mercury absolute.
  • the temperature in the freezing compartment will be 36F. This is highenough to keep the product from freezing as coffee extracts typically freeze at 27-27.5F.
  • the pressure will be high enough to keep voltatiles from evolving, but not so high as to produce an unacceptable pressure differential between and flow of vapor from compartment 28 into compartment 30.
  • the particular arrangement employed to maintain the vapor pressure at the selected level in freezing compartment 28 is not critical. Alternates to the illustrated arrangement include steam jets, thermocompressor systems for compressing vapor in drying compartment 30 and returning it to the freezing compartment, etc.
  • the product frozen to the material bearing legs 40 of the three conveyors is transported by the conveyors through partition 26 into the drying compartment 30 of the vacuum vessel.
  • This compartment is maintained at a pressure below 4.6 mm of mercury absolute and typically at about 1.5 mm mercury.
  • Radiant heaters or radiators 106 and 108 are disposed on opposite sides of each material bearing conveyor leg 40 in drying compartment 30 to apply radiant heat to the product.
  • the conveyor belts can be made of metals such as stainless steel or bronze or of synthetic materials such as Mylar or the like.
  • the upper sides of the product layers will be heated by direct radiation from heaters 106. If the belts are made of metal, radiators 108 will heat the undersides of the material bearing legs by radiation, and heat will be conveyed through the latter to the product layers by conduction. 1f the belts are made of Mylar or the like, the radiant energy from heaters 108 will pass through the belts 'to the undersides of the product layers.
  • the radiators may be of any desired type such as, for example, those disclosed in my U.S. Pat. Nos. 3,262,494 issued July 26, 1966; 3,285,514 issued Nov. 15, 1966; and 3,305,011 issued Feb. 21, 1967.
  • the radiators are heated by circulating a fluid, preferably liquid, heat transfer medium through them. Suitable heat transfer liquids are disclosed in my U.S. Pat. No. 3,236,292 issued Feb. 22, 1966.
  • the system for heating and circulating the heat transfer medium will typically include a conventional liquid heater (see FIG. 1) connected to the radiators by a supply conduit arrangement indicated generally by reference character 112.
  • the heat transfer medium is returned to the heater by a conduit system similarly identified by reference character 114.
  • the dried product is cooled to harden it, separated from the conveyor, and discharged from the vacuum vessel.
  • the product may be cooled by chilling the rolls 46 at the discharge ends of conveyors 32, 34, and 36 so that heat will be conducted away from the product as the material bearing legs 40 of the conveyor belts pass around the rolls.
  • the rolls 46 employed in the exemplary system 20 each have a cylindrical shell 122 supported from a central shaft 124 as by end members 126.
  • the shaft 124 is rotatably supported in bearings 128 attached to structrual components in the vacuum vessel which are identified generally by reference character 130.
  • each roll Disposed within each roll in heat transfer relationship to its shell 122 is a spiral coil 132, which extends substantially from end-to-end of the roll.
  • a refrigerant issupplied from a refrigeration unit (which is not shown but may be of the same type as unit 88) through a supply line 134 and a rotary coupling 136 to a passage 138 in the shaft 124 of each roll. From this passage, the refrigerant flows through coil 132, a passage 140 in the opposite end of the shaft, a rotary coupling 142, and a return line 144 back to the refrigeration unit.
  • a refrigeration unit which is not shown but may be of the same type as unit 88
  • a pivoted gate 164 can be swung from the position shown in full lines to that shown in dotted lines to direct the dried product from conduit 158 into a selected one of the two hoppers.
  • the product flows through a rota pocket valve 166 or 168 or other device capable of isolating the vacuum vessel from the surrounding environment into one of two transfer conduits 170 and 172 which can be evacuated through vacuum lines 174 and 176. From the transfer conduit, the product flows through a second pocket valve 178 or 180 into a conduit 182 or 184 for transfer to a packaging or other processing station.
  • the system employed in the apparatus 20 of FIG. 1 for this purpose includes a condensor 186 connected to vacuum vessel 22 by a conduit 188 and to a vacuum pump 190 by a conduit 192.
  • Vacuum pump 188 which is also used to pump down vacuum vessel 22 when the system is started up, draws the accumulated water vapor from vacuum vessel 22 through conduit 188 and upwardly through condensor 186. Any noncondensible gases mixed with the water vapor are discharged from the system by the pump through conduits 192 and 193.
  • a cold sorbent such as lithium chloride brine is pumped into the upper end of condensor 186 through a conduit 194 and flows downwardly through it, absorbinb and condensing the vapor moving upwardly through the condensor as it does so.
  • the sorbent is diluted by the condensed water vapor and heated by the latent heat given up as the water vapor condenses. Accordingly, it is necessary to reconcentrate and cool the lithium chloride solution after it leaves the condensor.
  • the heated, dilute sorbent is therefore recirculated from condensor 186 through return conduit 196 to a brine cooler 198 to reduce its temperature before it is returned through conduit 194 to the condensor.
  • a portion of the diluted sorbent discharged from cndensor 186 is diverted from conduit 196 through conduit 200, a coil 202 in heat exchanger 204, and conduit 206 to a sorbent concentrator or reboiler 207.
  • excess water is boiled off the sorbent.
  • This vapor may be conducted to the freezing compartment 28 in vacuum vessel 22 to provide at least part of the needed water vapor therein, if desired.
  • the heat is supplied by circulating a fluid heat transfer medium through the concentrator from liquid heater 110 by way of conduits 208 and 210.
  • the concentrated sorbent flows into conduit 211 and through a coil 212 in heat exchanger 204 disposed in heat transfer relationship to coil 202.
  • the sorbent in coil 212 gives up heat to the dilute sorbent flowing through coil 202, reducing the temperature of the reconcentrated sorbent and adding sensible heat to the dilute sorbent flowing to sorbent concentrator 207.
  • the sorbent flows through conduit 214 to brine cooler 198, where it is combined with the sorbent circulated directly from condensor 186 to the cooler.
  • Freeze drying apparatus comprising: a vacuum vessel; means dividing said vacuum vessel into a freezing compartment and a drying compartment; means for evacuating said vessel; means for conveying a product to be dried from said freezing compartment into and through said drying compartment; means for introducing a liquid or 'semiliquid product to be dried into the freezing compartment and onto the conveying means in a layer, means for cooling said conveying means to freeze the product thereto; means for keeping the pressure in the freezing compartment at a selected level which is sufficiently high to prevent volatiles from evolving from'the product until it is frozen to the conveying means and to prevent the product from freezing until it is on the conveying means; means for heating the product as it is conveyed through the drying compartment to evolve water therefrom; and means for removing the dried product from the vessel.
  • the means for providing water vapor in said freezing compartment comprises a receptacle in said freezing compartment, means for supplying water to said receptacle, and means for maintaining the water in said receptacle at a temperature sufficiently high that said water will volatilize at the pressure in the freezing compartment.
  • the freeze drying appartus of claim 1, wherein the means for cooling the product conveying means comprises means for effecting the flow of a refrigerant into heat exchange relationship with said conveyor means.
  • Freeze drying apparatus wherein the product conveying means has a material bearing leg and wherein the means for cooling said con veying means comprises a reservoir beneath said material bearing leg and means for effecting a flow of said coolant into said reservoir and out the upper end thereof and into heat transfer relationship with said material bearing leg.
  • the freeze drying apparatus of claim 1 wherein the means for maintaining the pressure in the freezing compartment at the selected level is means for maintainingan atmosphere of water vapor in said freezing compartment.
  • freeze drying apparatus of claim 5 wherein there is a partition in said vacuum vessel dividing it into said freezing and drying compartments, there being apertures in said partition through which said conveyor can pass and said apparatus further including means for removing from said vacuum vessel moisture evolved from the product in the drying compartment and water vapor flowing from the freezing compartment into the drying compartment through the apertures in the partition.
  • the method offreeze drying a product comprising the steps of: introducing the product to be dried into a zone maintained at a pressure which is below atmospheric but is sufficiently high to keep volatile constituents of said product from vaporizing; spreading the product into a layer; freezing the product in said layer; reducing the pressure on the frozen product to a pressure below 4.6 mm of mercury; and heating the product to effect the sublimation of water from the product and thereby reduce its moisture content.

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  • Engineering & Computer Science (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Molecular Biology (AREA)
  • Mechanical Engineering (AREA)
  • General Engineering & Computer Science (AREA)
  • Drying Of Solid Materials (AREA)
US00276556A 1972-07-31 1972-07-31 Freeze drying method and apparatus Expired - Lifetime US3740860A (en)

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JP (1) JPS5432181B2 (nl)
AR (1) AR198847A1 (nl)
AU (1) AU454555B2 (nl)
BR (1) BR7304809D0 (nl)
CA (1) CA974445A (nl)
CH (1) CH561888A5 (nl)
DE (1) DE2337549B2 (nl)
FR (1) FR2198611A5 (nl)
GB (1) GB1384838A (nl)
IT (1) IT989775B (nl)
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Cited By (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3991772A (en) * 1973-01-05 1976-11-16 Smitherm Industries, Inc. Methods of and apparatus for expanding tobacco
US4033048A (en) * 1976-01-12 1977-07-05 Clayton Van Ike Freeze drying apparatus
US4449305A (en) * 1981-07-01 1984-05-22 Societe D'utilisation Scientifique Et Industrielle Du Froid Usifroid Freeze-drying apparatus
US5172487A (en) * 1988-03-23 1992-12-22 Danisco A/S Method for continuous drying of a material and an assembly for carrying out said method
US5269077A (en) * 1991-12-11 1993-12-14 Criofarma Di Giorgio Bruttini & C. S.A.S. Continuous freeze drying apparatus
US5688333A (en) * 1994-12-27 1997-11-18 U.S. Philips Corporation Method of bulk washing and drying of discrete components
US5822882A (en) * 1995-01-20 1998-10-20 Freezedry Specialties, Inc. Freeze dryer method and apparatus with enclosed heater and controller
US6076274A (en) * 1998-02-27 2000-06-20 Dreisbach; Bernd Vacuum drying cabinet
WO2003006904A1 (en) * 2001-07-09 2003-01-23 Perera, Horacio, Eduardo Apparatus and process for freezing produce
US20080142166A1 (en) * 2004-05-01 2008-06-19 James Kenneth Carson Drying Process and Apparatus
WO2008048115A3 (en) * 2006-10-16 2008-06-26 Agres Ltd Improvements in spray freeze drying
ES2347397A1 (es) * 2007-05-17 2010-10-28 Obschestvo S Ogranichennoy Otvetstvennostyu Instalacion para el secado al vacio.
CN110945305A (zh) * 2017-04-21 2020-03-31 基伊埃里奥菲尔股份有限公司 冷冻干燥机和用于在产品中诱导成核的方法
EP3714226A4 (en) * 2017-11-22 2021-03-03 IMA Life North America Inc. LYOPHILIZATION BY SPRAYING ON A SUBSTRATE
CN113154851A (zh) * 2021-05-07 2021-07-23 湖南康琪壹佰生物科技有限公司 一种能调理血脂血糖血压的保健食品及其制备方法
US20220125078A1 (en) * 2018-10-19 2022-04-28 Harvest Right, LLC Freeze Drying Methods
US20230324118A1 (en) * 2020-11-16 2023-10-12 Sublime Stericeuticals Corporation Continuous throughput lyophilizer-powder filler within a sterile boundary

Families Citing this family (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS49115927A (nl) * 1973-03-10 1974-11-06
JPS5630397B2 (nl) * 1973-04-18 1981-07-14
JPS55112980A (en) * 1979-02-26 1980-09-01 Nippon Oxygen Co Ltd Freezing drier
JPS5976858A (ja) * 1982-10-22 1984-05-02 Hitachi Metals Ltd Ｆｅ−Ｃｒ−Ａｌ系合金
DE3706415A1 (de) * 1987-02-27 1988-09-08 Thyssen Edelstahlwerke Ag Halbfertigerzeugnis aus ferritischem stahl und seine verwendung
JPS6411957A (en) * 1987-07-04 1989-01-17 Kawasaki Steel Co Manufacture of stainless steel having high-temperature oxidation film excellent in corrosion resistance
JP5927066B2 (ja) * 2012-07-05 2016-05-25 株式会社協真エンジニアリング 乾燥装置及び乾燥方法
US20240085106A1 (en) * 2021-01-22 2024-03-14 Ima Life North America Inc. Drying chamber for a bulk freeze drying system

Cited By (25)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3991772A (en) * 1973-01-05 1976-11-16 Smitherm Industries, Inc. Methods of and apparatus for expanding tobacco
US4033048A (en) * 1976-01-12 1977-07-05 Clayton Van Ike Freeze drying apparatus
US4449305A (en) * 1981-07-01 1984-05-22 Societe D'utilisation Scientifique Et Industrielle Du Froid Usifroid Freeze-drying apparatus
US5172487A (en) * 1988-03-23 1992-12-22 Danisco A/S Method for continuous drying of a material and an assembly for carrying out said method
US5269077A (en) * 1991-12-11 1993-12-14 Criofarma Di Giorgio Bruttini & C. S.A.S. Continuous freeze drying apparatus
US5688333A (en) * 1994-12-27 1997-11-18 U.S. Philips Corporation Method of bulk washing and drying of discrete components
US5822882A (en) * 1995-01-20 1998-10-20 Freezedry Specialties, Inc. Freeze dryer method and apparatus with enclosed heater and controller
US6076274A (en) * 1998-02-27 2000-06-20 Dreisbach; Bernd Vacuum drying cabinet
WO2003006904A1 (en) * 2001-07-09 2003-01-23 Perera, Horacio, Eduardo Apparatus and process for freezing produce
US20080142166A1 (en) * 2004-05-01 2008-06-19 James Kenneth Carson Drying Process and Apparatus
US8012313B2 (en) * 2004-05-01 2011-09-06 Agresearch Limited Drying process and apparatus
US20110016742A1 (en) * 2006-10-16 2011-01-27 Agresearch Limited spray freeze drying
AU2007313546B2 (en) * 2006-10-16 2011-07-21 Agresearch Limited Improvements in spray freeze drying
WO2008048115A3 (en) * 2006-10-16 2008-06-26 Agres Ltd Improvements in spray freeze drying
ES2347397A1 (es) * 2007-05-17 2010-10-28 Obschestvo S Ogranichennoy Otvetstvennostyu Instalacion para el secado al vacio.
ES2347397B1 (es) * 2007-05-17 2011-09-29 Obschestvo S Ogranichennoy Otvetstvennostyu Instalacion para el secado al vacio.
US11047620B2 (en) 2017-04-21 2021-06-29 Gea Lyophil Gmbh Freeze dryer and a method for inducing nucleation in products
CN110945305A (zh) * 2017-04-21 2020-03-31 基伊埃里奥菲尔股份有限公司 冷冻干燥机和用于在产品中诱导成核的方法
CN110945305B (zh) * 2017-04-21 2021-07-16 基伊埃里奥菲尔股份有限公司 冷冻干燥机和用于在产品中诱导成核的方法
EP3714226A4 (en) * 2017-11-22 2021-03-03 IMA Life North America Inc. LYOPHILIZATION BY SPRAYING ON A SUBSTRATE
US20220125078A1 (en) * 2018-10-19 2022-04-28 Harvest Right, LLC Freeze Drying Methods
US20230324118A1 (en) * 2020-11-16 2023-10-12 Sublime Stericeuticals Corporation Continuous throughput lyophilizer-powder filler within a sterile boundary
US11874060B2 (en) * 2020-11-16 2024-01-16 Sublime Stericeuticals Corporation Continuous throughput lyophilizer-powder filler within a sterile boundary
CN113154851A (zh) * 2021-05-07 2021-07-23 湖南康琪壹佰生物科技有限公司 一种能调理血脂血糖血压的保健食品及其制备方法
CN113154851B (zh) * 2021-05-07 2022-07-22 湖南康琪壹佰生物科技有限公司 一种能调理血脂血糖血压的保健食品及其制备方法

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PH9954A (en) 1976-06-14
GB1384838A (en) 1975-02-26
AU5671373A (en) 1974-10-31
BR7304809D0 (pt) 1973-10-25
CH561888A5 (nl) 1975-05-15
IT989775B (it) 1975-06-10
FR2198611A5 (nl) 1974-03-29
AU454555B2 (en) 1974-10-31
CA974445A (en) 1975-09-16
DE2337549A1 (de) 1974-02-21
AR198847A1 (es) 1974-07-24
NL7308805A (nl) 1974-02-04
JPS5432181B2 (nl) 1979-10-12
JPS4945456A (nl) 1974-04-30
DE2337549B2 (de) 1976-07-15

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