DE2025999A1 - Freeze dryer - Google Patents

Description

PHW. 4101,

wij / hv.

Dr. Herbert Sek. J,

l'ateatanwalt

Register NYPhilips' Gloeilampenfabriektn
^FileNa PHN- 4101

from the,

Freeze dryer.

The invention relates to a freeze-drying system, the at least one vacuum freezing dryer with a condenser connected to it, in general operation a lower temperature prevails as in the Vakuuakaaaer »and a KUte-sucking device contains sub ideas from KSlte to the named Kaaaern, whereby means, under which there is a heating device to regulate the operating temperature of the vacuum capacitors.

In a known freeze-drying system, the KUte sucking device through an evaporation-condensation-Kohlaasohine formed »whereby a gas duroh one or more coapressors on high Pressure is compressed, then condensed in a condenser and expands in one or more crossroads. Liquid mediua

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becomes an evaporator located in the condenser chamber supplied, vo it by the fact that the condenser chamber will lose heat, evaporates and buk compressor surfok flows. On the other hand becomes liquid Medium fed to a wide evaporator, which is in heat exchange with a liquid in a closed line system, there gives off its cold to this liquid and flows in the gas phase again sum compressor surüok. The liquid can circulate and by means of a pump device incorporated in the closed line system

Cold coming from the wide evaporator in one part of the pipe system the vacuum chamber, which exchanges heat with another part of the pipe system. Veiter, there is a healing device in the closed pipeline system with whose help the temperature of the cooled liquid and therefore the temperature of the Vacuum chamber is adjustable. The vacuum chamber is evacuated by means of a vacuum pump device connected to the condenser chamber.

The mode of operation of this known freeze-drying system is further as follows. Water-containing preparations that are outside the Gell freeze-drying plant, for example at ⁰ C -5o frozen are brought into the vacuum chamber, which is previously cooled to 0, for example, -50 *. Thereafter, the vacuum chamber is evtJraiest wtd by the fact that the vacuum chamber is supplied with warmth via the liquid in the closed conduit. It is ensured that the ice present in the preparation sublimates into water vapor. Water vapor is % u% con & aas & gate chamber with a lower Τ «« ρ®: ρ »Φι» sucked off »sebll ^ t © iela äag-äa wIqüqs and freezes on the cold surface« amv I @ ad «ncAtorkßi» er _e

Maohdem some · batches of Prfipar & tes. wai the · ® wise are freeze-dried, there is a large amount in the food chamber

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Eie Deposed what a defrosting Kondensatorkaamer before the freeze * can be repeated trooknungeproseas necessary; aaoht.

Ia general, cooling is the Kondensatorkaaaer to temperatures of about -80 · · C while the temperature of the vacuum chamber of + 30 ^# C to -30 ⁰ C or -40 · 0 is controlled.

This known freeze-drying system has some disadvantages.

The facility is relatively involved. On the one hand, this is due to the fact that in order to achieve cooling temperatures down to -80 "C, at least one low pressure and one high pressure compressor maintain a high pressure Komprassions / Kxpansionsdruckverh & ltnlssee de «gases · are necessary.

An additional difficulty with this is that special door precautions are required to prevent the compressors coming from and from compressed gas BU lead back lubricating oil carried over from these compressors.

On the other hand, the system is necessary because of the separate auxiliary line system filled with liquid (for example glycol) is involved in regulating the temperature of the yakuum chamber.

Because of the temperature requirements mentioned above, there is only a slight look! of gases can only be used in the evaporative condensation cooling unit. The choice is further enhanced, among other things, by the characteristics of the compressors, which because of their dimensions make one Require a certain minimum suction pressure * The suctioned gas is stirring from the vaporizers mentioned, in which the liquefied gas vaporizes. At the same time, it is desirable that the condenser of the cooling machine can be cooled with cooling water, which further restricts the choice of the Gases means.

Another »eighth1 is that the usable gases, at- 009849 / UU

PHN. 4101

epieleweiee the medium known under the brand name Freon 22®, bsi yer proportionally at low temperatures have a vapor pressure »that is less than 1 atm. That means that because of the fact »that the gas pressure In the pipeline system, therefore, the atmospheric pressure is lower, light Can leak air into it, with all the concomitant consequences (efficiency reduction wrestling, pollution, Kosrroeioa) »

Next is the the AbtaOTuag of erforderlich® look in the condensation & torkaaner ice formed very long time, "This is in © reter instance its cause in the fact _β that Abtauuhg at vertilltnism & seig low temperatures carried BItIeS ₁ because eomaft dor uasds>" ek la pipe system would become inadmissibly high, »In the Fs-asis, the defrosting with water of, for example, 40 ⁰ O ₀ boron water only heats up to the outside (the ice for the most part surrounds the evaporator arranged in the condensetosis aiaHex ⁴ ) »Has another unfavorable®» ΕΙμΓΙμθβ on the time.

The invention b @ üw @ ckt ₉ one

greatly simplified construction ssu 0 © haffen _s when parts are turned off · The
does this have the license plate? deso
a gas & ltera machine formed iot ₉
system is available, the one side
Heat exchange with the Gaekiltemaschirae
arranged in the condenser chamber
see in this system a "liquid" Mi © ia © finds, with a second®
on either side of the first

aa ioo osot®

StW

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attached to it and a third one arranged in the vacuum chamber Heat exchanger is located, with the same in »wide line system Liquid is located and there is a short base line that is on both sides of the third heat exchanger is connected to the wide pipe system and a second pumping device is present, which together with the heating device in one part of the second line »

system, which lies between the two connection points of the short base line to this system and which part also contains the third heat exchanger and with one or more control valves in the second line system or the short base line to regulate the flow of liquid through this system or this line, wherein the first line system is further set up in such a way that in a position of said control cocks in which the short-circuit line is almost completely closed and only the second pump device is in operation, the liquid essentially only through the second line system and that part of the first line system which lies between the connection points of the second line system and contains the second heat exchanger, flows.

In this way a freeze-drying system is obtained, which offers a great "advantage" over the known system.

By using the gas cooling machine together with liquid in the piping systems, it is possible to use simple, quick and »The vacuum chamber as well as the condensate chamber are absolutely essential to bring her · desired · temperature.

In order for the liquid to run around in the line systems, nearby circulation pumps can suffice * The line systems and heat exchangers can no longer be contaminated by SohmierSl because

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SohmierSlkreis now part of the independently working gas refrigeration machine forms. By using liquid in the piping system, the risk of air being leaked is no longer there, and it is a good one Heat transfer between this liquid and the cold or warm Places "where it is guided along" guaranteed

Is a separate auxiliary line system in the known device with liquid required) which is only used to regulate the temperature of the vacuum chamber by ErwSrsswig in this system.

F running liquid can be used, the liquid present in the system according to the invention is now also used to defrost the condenser chamber. The fact that the liquid mash is led through the second heat exchanger in the second pipe system significantly shortens the defrosting time of the ice precipitated in the condenser chamber _t be high without the risk of au noh @ m pressure in the pipes. The ice cream is defrosted from the inside here. «Awserdeii ist @ ® KBgIiCh ₉ water is also higher

| Temperature su users, among other things, remove the üüaamassa again from the Auseenseit®.

Because © ® ©, ia second WsaesiiatÄiaseiier gawS & lt becomes _p the one essential low © r®n StreHtaagswiflcaKstQadl lat as dos first® ¥ Srmeaustawscher or dadwrahi »ä & m baäs ^ iolonois® Αΐϊορ © Σ? 5.? Ο1 © αορ © Σ? 5.? Ο1 © αορ © Σ? 5? dea both sites of ermb & m Leitengssyat ®mß _ΰ die sw £ o © bora sioQ first @ n auata, u * eh «r wad de»
gnnoiiloasen ¥ # * d®Bt »becomes

when the warm · F3.fli3elgkei$@ISSteuchtea dns @ i &<äie »weife is pumped, this liquid» β ts «» completely eäes mzMmm ytBIM & dvreh den

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second heat exchanger goes and not close or not at all duroh the first heat exchanger · The split liquid flow is therefore to » Defrosting process available, which is because of a maximum VIraetransport the liquid is favorable for rapid defrosting, Ba wane The liquid does not pass the cold spot of the gas refrigerator Side benefit has been obtained that unnecessary heating of the gas refrigerator is avoided. During the defrosting period, the machine will keep its low operating temperature and is still ready for use

In the case of an inexpensive design, the freeze-drying form plant according to the invention is at least one of the line systems with connected to a liquid expansion tank in which there is a gaseous medium above the liquid under such a pressure that boiling of this liquid is avoided at any operating temperature of the liquid. This creates a strong evaporation of the and a vapor * The formation of bubbles in the liquid in the line systems is avoided, which ensures good heat transfer between the liquid and the heat exchanger. Daduroh that the Druok of the shaped Medium · is chosen in the expansion tank hooh enough, it is mSglioh, a Cause the liquid to rise in the boiling point, which occurs when the The moisture trap chamber is advantageous · The liquid can then pass through the heater can be heated to an extra high temperature without Risk of boiling phenomena.

Another favorable embodiment of the freeze-drying system according to the invention, where the operating temperature of the vacuum chamber is regulated within the area of about -3O * C to + 3O * C and the The operating temperature of the moisture trap kawmer is about -60 ° C the indicator that the liquid RIi (trichloromonofluoromethane

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CCl-Γ) iet »The use of this well-known liquid offers several advantages. First of all, the viscosity of this liquid (boiling point 23.8 * C) Sieialioh constant in the effective temperature range «That means that in the A good heat transfer between fluids and heat exchangers is maintained in the relevant temperature range. Senn the danger that the normally turbulent fluid flow in the piping systems Relatively low temperatures of the liquid because of the increased viscosity decreases and changes into a® laminar flow P does not exist here

Because of verh & ltsiiem & SSIG low viscosity low pumping action may be sufficient "w hretid dadur © _fe} DAM® oil © viscosity remains siotslioh constant effective temperature range, have the pumps lamer one naheiu constant load. This and that enables the use of small, relatively cheap pumps, the constant load having a favorable effect on the service life.

The use of R 11 also enables the liquid to be kept at a relatively high temperature when defrosting the moisture trap chamber, while at the same time the pressure in the expansion tank and the pipe systems can be comparatively low ₉ so that thin-walled and light pipes can be used , BII at a pressure of 2 _t 5 atm in the piping system, heat up to 60 * C au, without calibrating the risk of boiling «

A embodiment of the invention is shown in the drawing and is in the following ώΠ "^ ε> drive. It soaps

Fig. Ie, a seh®QQtits <g! SG not aaesger & ohte representation of a Design of the erfi »taigee®B & eeen freeze-drying system,

Fig. Ib and Io a

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tion system according to Fig. Ta on the right side of the line I-I.

In FIG. 1 a, the reference number 1 indicates a first closed line system in which, on the one hand, a heat exchanger 2 is added, which with the cold cap 3 of a gas refrigerator 4 in There is heat exchange and, on the other hand, a heat exchanger 5 »which is arranged in a condenser chamber 6. You condenser chamber 6 is on the one hand

Connected via a line 7 to a vacuum freeze-drying chamber 8 and, on the other hand, via a line 9 to a vacuum pumping device 10. It is also provided with a water supply 6 * and a water discharge 6 ″. At points A and B, there is a second line system 1 on the first line system 1 Connected line system 11, in which a heat exchanger 12 is added, which is arranged in the vacuum freeze drying chamber 8.

At the point C and S there is the second line system 11 a short-circuit line 13 is connected, in which a controllable shut-off element 14 is located. In the first line system 1 there is a pumping device 13, while in the second line system there is also a controllable shut-off element 16, a heating device 17 and a pumping device

18 are included. At the point E, the first line system 1 is a with a valve 20 provided expansion tank 19 connected.

They pipe systems are filled with a liquid that for example H 11 can be. Above the liquid in the expansion tank

19 is a gas under pressure, for example nitrogen.

The heat exchanger 2 has a flow resistance which is significantly greater than that of the heat exchanger 5.

The way your system works is as follows.

The condenser chamber 6 is cooled by »that file» iigkeit in line «« yet · «1 by means of the pumping device 15 in the alt g®« -

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The direction indicated by the drawn arrows is pumped around. The cold absorbed by the liquid in the case of the cold cap 3 of the cooling machine 4 in the heat exchanger 2 is released again in the heat exchanger 5 of the condenser chamber. In order to cool the vacuum freeze-drying chamber 8, part of the liquid flow which is led along the gas refrigeration machine is tapped at A and filtered through the fuel supply unit 18 in a direction also indicated by arrows through the second line system 11 and the pressure reservoir 12. Ib «üeseia ureas exchanger ■ - the liquid gives off its cult® of the · VokuuBgefriGfurockmasagskammer θ. During the cooling of the vacuum ^{freezing room 1} Θ, the heating device 17 is out of operation and the dispenser relay 14 is partially open. Am part of the © FlS®sigkeItos4roE @ Q _s dos? originates from Wiraeauet similarher 12, will then enter the Siaj? s0 @ | iiiassl®itung 15 at Stell® B and aa the Stell® G ait <ä © s from -Abspor ^ elsaent 16 durelagelassenera cold F? JIs3igkeito £ 3 ^ g @ Q
der Flileaigkeit © rfiaifea wls? d _e

12 herrühreadea FlSBslgkaitest ^ oaeB steiat aa © h B narad iaiseSit see there with the WSreeattetaeaeher 5 terrEte @ ad © a Fll @ 8igk @ itsstr © Ei _e through the passages® of the Ab @ p © rrelee © at © @ 16 tew ₀ 14 ksara di ©

a temperature »the hSlaep is set as Uq ₅ to ö © i © ka di®» ¥ @ aa ä®m TMsE! ®cmabcma © hQK 12 much ISlt® sageflte ^ must, the AbspsssGloa © ^ 114 ßOD @ Ioil © s! 3 © ss uos? äoa ₉ q® fiaos iä © from the Puiapvorriofeteag Hi ^ osfeSaid 372, ioGigIs © lftonosags sraa F «act E from there sua WaxmsaöB'SaiQoefosE 'S fläooolso

! © © Mets ii © ^ Qismffic ^ ofeaos ^ ifQQtoiiiaiagofeeaEiog · wmä üio je iteo Esteaofeo ^ ongoscoiuo? ossoä © iat SacälioaD uosslGia cBiooo Eicmzosm

ORIGINAL INSPECTED

P ..; : ■■■ ■■; -...; ■■ -.

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evacuated by means of the associated Takuuapumpvorrichtung 10 and the actual freeze-drying of the preparations can take place. Daiu will the fell! device 17 is installed, which is the ium heat exchanger 12 the flowing liquid stream supplies as much heat as required around the ice present in the preparations present in the vacuum freeze-drying chamber θ sublimate water vapor, as well as water vapor condenses and freezes in the condenser anmer 6 with a lower temperature. After a few batches of preparations have been freeze-dried in this way, there is a large quantity in the condenser room Ice deposited, essentially on the outside of the heat exchanger 5. You can now defrost the condenser camper quickly and easily Way done as follows. The pumping device 15 is switched off. The shut-off element 14 is closed and the shut-off element 16 is completely opened. Duroh the pumping device 18 is now the liquid that by the heating device 17 to a comparatively high temperature is heated, pumped around by the path indicated by dashed arrows. The warm liquid is generally available from the water exchanger Ice in the condenser cup is losing its heat. In Tergleioh tan Terfihren There are two main differences when it comes to cooling. First, thermosetting air the flow of liquid during the warming-up process the pumping device 15 and the heat exchanger 5 in a direction the same as that in the cooling process is opposite. This is not a problem with circulation pumps. Secondly the flow of liquid is almost impossible or not at all continuous Wtrmeaustauscher 2. This has its cause in the already mentioned l'atsaohe that the flow resistance of the Wtraeauatauaohers 2 is much greater than that of the W & raeauatgleichhera 5t ao daas the Lüaaigkeitaatroa the easiest way through the latter heat exchanger chooses. Sa iat aelbatveratlndlieli also aSglieh, a liquid

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ORiGiNAL INSPECTED

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flow through the heat exchanger 2 by means of in the line sections xvisehen de «heat exchanger 2 and points A and E included To inhibit shut-off elements.

Since no liquid or almost no liquid flows through the second heat exchanger, the entire liquid flow is available for heat transport from the heating device 17 to the condenser chamber 6, which is a thing promotes rapid defrosting. The liquid will be on a proportionate basis heated high temperature, a gas in the expansion tank 19 above the liquid under pressure, for example nitrogen, for this ensures that the liquid does not start to boil. If the operation "Temepratur the vacuum chamber ungeffthr in the temperature range from -30 to + 30 * 0 * 0 and amounts to the operating temperature of Kondensatorkaaser -70 ⁰ C to -80 * C, so, when using R11 as a liquid at a pressure of 2 , 5 atm in the expansion tank and the pipe systems, the H 11 can be heated to 60 ° C without boiling. During normal operation of the system, the pressure can then fluctuate between 1 and 1.5 atm. Should the pressure in the line systems rise so sharply during operation, the valve 20 will open. This mass can also be defrosted from the outside by means of high temperature water being fed into the condenser chamber via the inlet 6 '. Melt water can flow out of the condenser chamber via the outlet 6 " so the parking Kalt · the gas refrigerator. the · supplied by this machine Kute is not lost. Are in Fig. 1a two shut-off by 16 and 14 present in the line 11 or the fforzschlusslsitung 15 "in fig · 1b and 1a

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it is shown that it is also possible to use a mixing valve 21 BSW. a Use distribution valve 22 see below. For the rest, the mode of action is that of the in fl. 1a plant shown the same. From the above it should be it will be evident that the invention provides a simple and well-functioning freeze-drying system.

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Claims (3)

-14- PHH. 4101. PATENT CLAIMS! 1.J Freeze-drying system, which has at least one vacuum freeze-drying chamber with an associated condenser chamber in which the temperature in operation is lower than that in the vacuum chamber, and contains a refrigerating device for supplying refrigeration to said chambers, means, including a heating device, being present for regulating the operating temperature of the vacuum chamber thereby k characterized in that the cold generating © device is formed by a gas chiller, a first closed line system being present, which on the one hand contains a first heat exchanger for exchanging heat with the gas chiller and on the other hand a second in the Condenser chamber arranged heat exchanger, wherein in this system there is a liquid and a first pumping device, wherein further a second pipe system is present, which is located on both sides of the first heat exchanger »connects to the rste pipe system and in which is a third heat exchanger arranged in the vacuum chamber is located, with the same liquid being in the second pipe system * and a short-circuit line is present, which connects to the second line system on both sides of the third heat exchanger and a second pump device is present, which, together with the heating device, enters one part of the second line system between the two connection points of the short-circuit line this system is located, is included, and which part also contains the third heat exchanger, and where one or more Hegelhähaua are present in the second line system or the course closing line for regulating the flow of liquid through this system or this line ₀ with the first line system @rart eira $ ®riehtet 1st that get one 009 849 / UU -15- PHK. 4101 Position of the rules mentioned, in which the Kurteohluaaleitung almost is completely closed, and in operation only the «wide pumping device, the liquid generally through the second line system and that part of the first line system! the one between the Ansohlusstellen of the “wide pipe system is due to this, and whichever part contains the“ wide heat exchanger, it flows. 2. Freeze-drying system according to claim 1, characterized in that at least one of the line systems is connected to a liquid expansion tank in which you can see above the liquid gaseous medium is located and «was under such a pressure that boiling of this liquid is avoided at any operating temperature of the liquid. 3. Freeze-drying plant naoh Anapruoh 2, with the operating temperature of the vacuum chamber within the range of about -30 * 0 is regulated to about + 30 * 0 and the operating temperature of the condenser chamber is about -80 * 0, characterized in that the liquid RII (Triohlormonofluoromethane - CCl-F) is. 009849 / UU Blank page