CN1035350A - Freeze-drying and freeze drying plant - Google Patents
Freeze-drying and freeze drying plant Download PDFInfo
- Publication number
- CN1035350A CN1035350A CN 88100770 CN88100770A CN1035350A CN 1035350 A CN1035350 A CN 1035350A CN 88100770 CN88100770 CN 88100770 CN 88100770 A CN88100770 A CN 88100770A CN 1035350 A CN1035350 A CN 1035350A
- Authority
- CN
- China
- Prior art keywords
- refrigeration
- hothouse
- transfer medium
- heating surface
- area
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
Images
Landscapes
- Drying Of Solid Materials (AREA)
Abstract
In freeze-drying method of the present invention, predetermined water gaging is poured on the interior refrigeration/area of heating surface of hothouse, and this surface is cooled to below 0 ℃, makes and forms one deck ice film on it.Then, the temperature of the ice film of formation is remained on below 0 ℃, fluent material is fed to ice film surface, make the frozen coating that forms one deck liquid material on the ice film surface.Under this environment, in hothouse, cause vacuum, make and under vacuum environment, frozen materials is carried out freeze drying.
Description
Freeze-drying method that the present invention relates to and device are suitable for handling such as solution, emulsion, solid suspension, slurries and similar material.
In a kind of habitual seasoning, adopt hopper-shelf-type device with dried material.Freezed to be contained in material in hopper and the similar containers and be emitted on the shelf in the vacuum chamber in the device or between the shelf, supplied with certain heat and make and freeze to have at least in the material a kind of component to produce sublimation to freezing material from these shelves.After this sublimation process is finished, feed clean air or nitrogen, then the material through lyophilization is taken out vacuum chamber together with container to vacuum chamber.
In this customary way, certain bulk article such as a kind of coffee extract, concentrates earlier, and the back is freezing.The coffee extract that freezes is 1 to 3 millimeter through the granular size after the granulation.Subsequently, in hopper, fill up the coffee extract of this granulation.For another kind of bulk article,, always adopt and evacuate drying mode such as certain soup.This evacuation drying mode is: soup is pushed out from a very thin shower nozzle, spreads to " fluorine Lyons 12 " liquid material (dicholorodifluoromethane CCl
2F
2One of trade name) put into hopper to form a kind of tiny graininess frozen substance.After this above-mentioned habitual drying means will be called prior art 1.
In the habitual freeze-drying method of another kind, there is liquid material to be dried at first to inject hopper, be seated in again on the cooling shelf or among the refrigerating chamber, the same with the great majority evacuation drying operation situation of medicine and some food, it is freezing that the liquid material is able to.After this this another kind of habitual freeze-drying method will be called prior art 2.
No matter among any prior art 1 and 2, it all is that at first sparsely large tracts of land is spread in the hopper of plate-like that material to be dried is arranged, and then stands freezing processing and freeze drying processing in advance.The overturning hopper is to draw product in subsequently.Thereby, all needing to load and unload various hoppers in either case, the surface area of each hopper is very big, and it is very big to take up an area of the space altogether, and the loading and unloading apparatus of employing is complicated or to change the labour of taking a lot.When having material to be dried to handle in must environment, just must in aseptic room, be engaged in operation in high hygiene.
Especially prior art 2, and wherein the liquid material at first injects hopper, and is freezing in hopper then, and the freezing material in the hopper can't just lean on the overturning hopper just can separate from hopper.Thereby, in this case, just need to lean on artificial or use certain automatic stripping device tool that freezing material is stripped down from hopper.Operation manually this or that peel off freezing material automatically just makes that the method for prior art 2 is complicated.These all are the inherent shortcomings of prior art 1 and 2.
In order to eliminate prior art 1 and 2, in other words, these inherent shortcomings of hopper-shelf-type device, the patent No. is a 3281956(prior art 3) and 3264745(prior art 4) United States Patent (USP) other known freeze-drying method has been proposed, wherein: the space between the tube of many upright gardens is full of liquid material to be dried, cool off the surface of these garden tubes then, form the material frost zone of desired thickness on each tube surface, garden.After this material frost zone is completed into, removing the space of the liquid material of remainder between each garden tube.Subsequently, the material frost zone is in the vacuum environment, has at least a kind of component that the distillation phenomenon takes place by tube surface, heating garden in the material to obtain the required heat of sublimation from the surface, to make simultaneously.After sublimation process is finished, under the tube sur-face peeling of garden, be collected among the product receiver that is placed in below the tube of garden dry come out material bed on the tube surface, garden through this sublimation.After this known method that above-mentioned United States Patent (USP) is set forth will be called prior art 3.More specially in the prior art 3 be, pass each garden tube a kind of heat transfer medium that circulates, make the liquid material that is held in the space between these garden tubes freeze, so that form the material frost zone of desired thicknesses at these positions at the position of pressing close to tube surface, garden.Then, from then on the liquid material remainder that freezes not yet in this space removes in the space.Then, the material frost zone is among the vacuum environment, heats gradually by means of the heat transfer medium that in the tube of garden, circulates simultaneously.Thus obtained, the dry product that comes out on the tube surface, garden with stripper under the tube sur-face peeling of garden; The riding position of stripper is moved downward by a screw rod drive in this overburden operation above the tube of garden.Product that strips down like this or dry material collection are among the product receiver.
As mentioned above, in prior art 3, the garden tube lip-deep freezing material bed be that to be attached to the garden tube lip-deep.Thereby, freezing material bed in order to separate from the garden tube, in prior art 3, adopted a kind of apparatus of peeling off, this apparatus has a plate-like stripper, and hole, many gardens is arranged above, and the diameter in each hole, garden is a bit larger tham the external diameter of each garden tube.In the overburden operation of freezing material or product, the garden tube passes through the hole, garden of plate-like stripper with slip mode, so that product is stripped down from tube surface, garden.Therefore, owing to exist the gap between hole, stripper garden and the garden tube, the thin layer of product or freezing material under can retaining on the tube surface, garden simultaneously, owing to constitute the slippage contact between the surface of garden tube that is made of metal entirely and stripper, can produce metal dust again.These all be prior art 3 intrinsic defective.
On the other hand, set forth another freeze-drying method in the prior art 4, wherein: a kind of cooling with heat transfer medium circulated in by the space outerpace between the many upright garden tube that is full of material to be dried, make and form the freezing material of one deck on the inner surface of each garden tube, this point is opposite with prior art 3, on the wherein freezing material bed outer surface that is formed on each garden tube.Address in the prior art 4: do not adopt any apparatus of peeling off, thereby in order to be easy to from garden tube inner surface products of separated or dried material, the shape of any garden tube must be straight, even and during the variations in temperature of garden tube, do not have any crooked yet.
Speak of in the prior art 4, the product that drying is come out on the tube inner surface of garden can be separated from the garden tube inner surface at an easy rate, thereby does not adopt any apparatus of peeling off.In general, freezing material can have contraction slightly when drying, so that this dry material is easy to separate from the garden tube inner surface.But, in most of the cases, relevant with freezing condition with dry two operations with material properties to be dried, being contained in the material that freezes subsequently in the tube of garden with liquid state all has the trend that is attached on the tube inner surface of garden, unless material is very thin solution.As a result, dried material just can not be separated from the inner surface of vertical garden tube fully, thereby a part of dried material still can be attached on the inner surface of garden tube.This be prior art 4 an intrinsic defective.
Among prior art 3 and 4 any, this remaining part that is attached to the dried material on the tube inner surface of garden will experience the circulation next time of liquid material freeze drying operation, And and after this repeatedly stand repeatedly thing followed circulation in same mode.If the liquid material that is contained in the work cycle process in the tube of garden is heated next time, the tube surface, garden of the remaining part of dried material is heated too and adhering to, then may dissolve the remaining part of the dried material that is attached to tube surface, garden and makes it the surface of disengagement garden tube.But, no matter in any prior art 3 and 4, the heating of liquid material all can damage the quality of product.Interrelate therewith, in freeze drying work cycle next time, remain on below 0 ℃ as the orchard drum surface temperature, be full of the liquid material that temperature is approximately 0 ℃ simultaneously, under the remaining part of the dried material that forms on garden tube surface in the then preceding primary freeze drying operation process is still retained in work cycle next time, thereby it is just more and more many to be attached to the lip-deep material of garden tube.This is another intrinsic in prior art 3 and 4 defective.
The freeze-drying method that the objective of the invention is to propose a kind of material to be dried comprises following each step to solve intrinsic above-mentioned variety of issue in the prior art: directly described material is delivered to refrigeration/area of heating surface in the hothouse that is installed in the vacuum type freeze drying plant; Described material is carried out the freeze drying operation, prevent that simultaneously described material is attached on described refrigeration/area of heating surface, so that after the described freeze drying operation of finishing described material, can easily separate from described refrigeration/area of heating surface.
According to the present invention, its objective is as follows and to realize:
At first, water be poured over Shang refrigeration/area of heating surface in the hothouse of the vacuum freezing drying device of packing into ， And refrigeration/area of heating surface be cooled to temperature below 0 ℃ so that form the ice film from the teeth outwards.After the ice film is completed into, refrigeration/area of heating surface is fully remained on 0 ℃ below the temperature.Under this condition, plate material or liquid material be placed on this material is freezed on the ice film.After this, in hothouse, cause vacuum to make such material frost zone and ice film in vacuum environment, stand freeze drying.That is, according to the method among the present invention, by forming the ice film on direct refrigeration/area of heating surface in the hothouse of vacuum type freeze drying plant the same refrigeration/area of heating surface of material frost zone to be dried is separated, in the freeze drying operation process, the ice film stands sublimation together with at least a component of material to be dried and escapes from refrigeration/area of heating surface, thereby, there be space or the gap that stays because of the distillation of ice film between the dry so same refrigeration/area of heating surface of crossing of material.Such space or gap make and might separate and collect dried material or product easily from refrigeration/area of heating surface at following of gravity or slight external force effect dried material or product.So, according to method of the present invention, might be fully dried material be taken off from refrigeration/area of heating surface, collect product satisfactoryly.
Another object of the present invention provides a kind of freeze drying plant, the user can fully be separated be frozen in the dry material of crossing of And on the tubular device table face, need not use any stripping off device, thereby prevent that any part of dried material is deposited on the surface of tubular device; Solve variety of issue intrinsic in prior art 3 and 4 whereby.
That is according to the present invention, another purpose of the invention described above is by providing the freeze drying plant that comprises following each parts to realize: a hothouse that causes the standard vacuum degree therein; Be contained in a refrigeration/heater element in the described hothouse, described refrigeration/heater element has a surface, interior border and surface, an outer border, and one of surface, described border constitutes the refrigeration/area of heating surface of material to be dried; A heat transfer medium supplying device is used for a kind of heat transfer medium is supplied with another surface, border of described refrigeration/heater element; The device that supplies water/cut off the water supply is used for supplying water equably on the described refrigeration/area of heating surface of described refrigeration/heater element; Feed/fracture device be used for to/supply with/the disconnected material that removes from the ice film that forms at the described refrigeration/area of heating surface of described refrigeration/heater element; And the aperture of door device that is arranged on described hothouse bottom.That is, in freeze drying plant of the present invention, refrigeration/the area of heating surface of refrigeration/heater element is at first cooled off by the heat transfer medium of sending into refrigeration/heater element inside, and the refrigeration/area of heating surface to the refrigeration/heater element that cooled off supplies water so that form the ice film on this surface then.After this, supply with material so that on the ice film, form liquid material frost zone to the ice film that forms.After on the ice film, being completed into this material frost zone, in hothouse, carry out the freeze drying operation of material, at least a component of material and the distillation of icing film are distilled simultaneously.As a result, owing to disappear, on the position between the refrigeration/area of heating surface of material frost zone and refrigeration/heater element, just stay space or gap through this sublimated ice film.Such space or gap make that the material frozen coating of drying can easily be separated from the refrigeration/area of heating surface of refrigeration/heater element, thereby make and might collect dried material or product easily.
Fig. 1 is the part dialysis longitudinal sectional drawing of freeze drying plant first embodiment of the present invention;
Fig. 2 is the part dialysis perspective view of freeze drying plant of the present invention first embodiment shown in Figure 1;
Fig. 3 is the latter half of transverse cross-sectional view of freeze drying plant second embodiment that got along Fig. 4 section line 3-3, of the present invention;
Fig. 4 is along Fig. 3 section line 4-4 longitudinal sectional drawing that got, freeze drying plant second embodiment of the present invention;
Fig. 5 is the latter half of transverse cross-sectional view of freeze drying plant the 3rd embodiment that got along Fig. 6 section line 5-5, of the present invention;
Fig. 6 is along Fig. 5 section line 6-6 longitudinal sectional drawing that got, freeze drying plant the 3rd embodiment of the present invention;
Fig. 7 is half principle, half schematic layout pattern of a freeze drying equipment being combined by many freeze drying plants of the present invention;
Fig. 8 is the latter half of transverse cross-sectional view of freeze drying plant the 4th embodiment that got along Fig. 9 section line 8-8, of the present invention;
Fig. 9 is along Fig. 8 section line 9-9 longitudinal sectional drawing that got, freeze drying plant the 4th embodiment of the present invention.
Among the first embodiment of the invention as illustrated in fig. 1 and 2, label 1 indicates the case shell of having determined a hothouse 2 therein, and many level boards become a vertical buttress for 3 yards in the chamber.Label 3 varies to 3-n from 3-1, and label 3-1 indicates uppermost frame plate, and label 3-n indicates from which piece frame plate of uppermost frame plate number.In first embodiment of the invention, what frame plate 3 adopted adds up to 3.Each piece frame plate 3 all is equipped with a pipeline, and a kind of heat transfer medium or refrigerant therefrom pass through.A surface of frame plate 3 constitutes a refrigeration/area of heating surface 5.
These frame plates 3 are coupled to each other along the tensile coupling mechanism (not shown) of vertical direction by one, this mechanism belong to the present patent application people, set forth to some extent among the Japanese Utility Model publication number 54-139364.In the middle of frame plate 3, uppermost one links such as the such actuator 4 of the cylinder body that surges that is contained on the case shell 1 together.As uppermost frame plate 3-1, shown in the first half of Fig. 1 raising middle flask shell 1, when pushing the uppermost position of this frame plate of top arrival to by actuator 4, three frame plates are spaced apart by predetermined spacing each other, keep level simultaneously.On the contrary, uppermost frame plate 3-1, shown in the Lower Half of Fig. 1 raising middle flask shell 1, when pushing the bottom position of this frame plate of below arrival to by actuator 4, three frame plate sign indicating numbers become a vertical buttress.A suitable aperture of door device (not shown) is housed in the front portion of case shell 1.The framework 6 of square frame shape or grill-shaped has root edge, is contained on each the piece frame plate 3 frame plate 3-1 topmost, causes framework to state the root edge place thereon and closely contacts with the refrigeration/area of heating surface 5 of each piece frame plate 3.As shown in Figure 2, framework 6 respectively is equipped with a guiding bead 7 on its opposed both sides.Guiding bead 7 is outwards outstanding from each edge side direction on framework 6 opposed both sides, is assemblied in slippingly above the guide rail that both sides had 8 of each piece frame plate 3.Therefore, framework 6 can slide along guide rail 8 front and back.
When being pushed upwardly, uppermost frame plate 3-1 arrives its extreme higher position so that nethermost frame plate 3-n when arriving at as shown in Figure 1 a certain position " A ", water supply device 9 injects water the framework 6 that is contained on the bottom frame plate 3-n, and water supply device 9 is contained in the middle of the opposed edge wall of case shell 1, and its position makes this water supply device 9 to inject the framework 6 that is contained on the bottom frame plate 3-n to water.Water supply device is furnished with water supply nozzle 10, and when each frame plate 3 arrived at above-mentioned position " A ", water injected each framework 6 that is contained on the frame plate 3 from nozzle.In this first embodiment of the present invention, water supply device 9 is fixed on the case shell 1 interior certain position.But, water supply device 9 is moved along vertical direction, if each piece frame plate 3 is fixed on each certain position that these frame plates 3 can tilt.
The operational circumstances of above-mentioned first embodiment of the present invention is as follows.
When the frame plate 3 that has framework 6 arrived at precalculated position " A ", this frame plate 3 maintained the temperature at below 0 ℃.After this, the valve open of water supply device 9, with predetermined two predetermined areas of water yield spray, these two areas are: the refrigeration/area of heating surface 5 of the frame plate 3 that centers on by framework 6, and at this refrigeration/area of heating surface 5 be contained in a area between framework 6 lower ends on the surface 5.As a result, the water of so supplying with forms the ice film and covers above-mentioned two areas with regard to freezing immediately.Under this condition, frame plate 3 still keeps chilled at 0 ℃ below the temperature.If material to be dried is a liquid, this liquid material to be dried injects the framework 6 that is contained on the above-mentioned frame plate 3 by means of a kind of fixed displacement formula water jet (not shown on the figure).At this moment, for guaranteeing the quality of dried material or product, preferably in advance this liquid material is cooled to minimum temperature near its freezing point, liquid material Reng Ran And does not freeze under this minimum temperature.But, even liquid material to be dried pours into when keeping at room temperature in the operation at it, aspect quality assurance also without a doubt, as long as ice film and above-mentioned two areas, be the refrigeration/area of heating surface 5 of frame plate 3 and the area between this surface 5 and framework 6 lower ends, all pass through the fully words of cooling.If the speed of pouring into is not too low, the liquid material that so pours into can scatter along horizontal aspect.On the other hand, if material to be dried is the flat solid material as chump, then many such solid materials just lie in framework 6 the insides that are loaded on the frame plate 3 equably, so as frame plate 3 freezing/freeze above the area of heating surface 5.At this moment, these sheet materials have avoided cold excessively because of the existence of ice film, and set up the uniform thermal conducting phenomenon between the refrigeration/area of heating surface 5 of sheet material and frame plate 3.As a result, have in the material to be dried, generate many ice crystals, the sheet stock material is freezed with evenly upright needle-like in any a slice.At this moment, owing to do not have the air gap that constitutes remarkable impedance in the conduction of heat between the refrigeration/area of heating surface of sheet material and frame plate 3, the temperature of frame plate 3 that might be by placing sheet material to be dried above the accurate control is controlled the growth rate of ice crystal.That is, might control the diameter of each ice crystal.Sheet material finish freezing after, in hothouse 2, cause essential vacuum.Under such condition, the temperature of frame plate 3 is adjusted the sheet material that has freezed with drying.The sheet material drying operation incipient stage of carrying out on the refrigeration/area of heating surface 5 of frame plate 3, sheet material closely contacts with the refrigeration/area of heating surface 5 of frame plate 3 by the ice film.Thereby the temperature of frame plate 3 should remain on the certain level, the heat that sheet material is needed at least a component each sheet material that distils from 5 acquisitions of refrigeration/area of heating surface.In general, when 50 to 60% of each sheet material obtains drying (although this percentage becomes with the character and the drying condition of material to be dried), because steam is escaped from the crack of dry material, the ice film can distil; These cracks produce in the freezing operation process of material.As a result, the ice film is through distillation and disappear, and makes the distillation of dry material because additional the distillation also taken place in the bottom of material has become easily.From beginning this additional distillation, the temperature of frame plate 3 just raises to strengthen these sublimations gradually.After sublimation process is finished, send into clean air or nitrogen to eliminate vacuum wherein to hothouse 2.After this, the aperture of door device (not shown) of hothouse 2 is opened, one the receiver 11 of dried material or product successively with each piece frame plate 3 contact.When product receiver 11 during by last frame plate 3, the framework 6 that is contained on the frame plate 3 is pulled out forward, dried material or product are collected in 11 li of product receivers.At this moment, as mentioned above, in most of the cases,, in the collection operation process of product, will be fragmented into many small pieces because dried material or product have many crack ， And volume contraction in framework 6.After the collection operation was finished, framework 6 was slided go back to its origin-location, perhaps temporarily took out from drying box chamber 2.In above-mentioned first embodiment of the present invention, be lower than water spray on refrigeration/area of heating surface 5 of 0 ℃ and these two areas of another similar surfaces and form the ice film to temperature.But, also can at first form moisture film and cover above-mentioned area, the ice film that freezes subsequently so to form is to constitute the ice film.
Fig. 3 and 4 shows the second embodiment of the present invention, and wherein: label 15 indicates the case shell of hothouse 16, and heat transfer medium container 17 is housed in the chamber, is adorning two pipelines 20 and 21 on its limit wall, and heat transfer medium circulates via pipeline.Container 17 also is equipped with a upper head plate and a bottom plate, is fixedly mounting a refrigeration/heater element 18 that is made of many pipes therebetween.Peripheral space 19 is round refrigeration/heater element 18.Hothouse 16 connects by 22 same vavuum pump (not shown)s of a suction line.Heat-conduction medium container 17 by the steam jacket 23 with bung flange shape round.23 same feed pipes of vapour jacket 24 couple together, and heat-conduction medium or refrigerant flow into vapour jacket 23 via this feed pipe, therein circulation.Refrigeration/heater 18 can be made by an independent pipe.
Heat transfer medium container 17 has a lower end perforate.As shown in Figure 4, a lower end port lid 25 is equipped with in the bottom of container.Can swing to open and closely to close perforate.Also adorning a feed tube 26 and a discharging tube 27 on the container 17 lower edge walls.Feed tube 26 alternately is communicated with water supply tank 28 and feed tank 29.Discharging tube 27 is guided the liquid of discharging into Drainage tank 30.
The operational circumstances of second embodiment of the invention with said structure is as follows.
At first, be cooled to temperature and infeeded peripheral space 19 between refrigeration/heater element 18 and the garden tubular heat transfer medium container 17 by pipeline 20 and 21 at the heat transfer medium below 0 ℃, And walks circulation in peripheral space 19 and these two pipelines 20 and 21.Then, supply water to refrigeration/heater element 18 from water supply tank 28 by feed tube 26, the water level of the water that is held in device 18 reaches a certain position of device 18 upper ends.The inwall ， And that the water that is held in the device 18 touches refrigeration/heater element 18 begins to freeze and forms the ice film 31 that covers device 18 inwalls, as shown in Figure 4.When the thickness of ice film 31 reaches below 1 millimeter, when preferably reaching 0.5 millimeter, the water in refrigeration/heater element 18 is emitted from device 18 by discharging tube 27.
In this case, when refrigeration/heater element 18 undercoolings, the water that wherein holds will freeze too fast.As a result, because it is longer in the time that stayed in the device 18 before device 18 drainings than the water that resides in device 18 other parts to reside in the water of device 18 bottoms, so the thickness of the ice film 31 that forms in device 18 bottoms just becomes excessive.Excessive for the thickness of anti-stagnant ice film 31, passing through feed tube 26 before refrigeration/heater element 18 supplies water, refrigeration/heater element 18 will be cooled to temperature from-10 ° to-15 ℃.So, the ice film 31 of formation will keep that its thickness is constant, volume is very little.
After the ice film 31 that covers refrigeration/heater element 18 inwalls was completed into, device 18 was just fully cooled off.Subsequently, be contained in feed tank 29 Nei And and in jar 29, be cooled to the liquid material of temperature about its freezing point and be injected into refrigeration/heater element 18, reached the position that is lower than ice film 31 height slightly up to the liquid level of the liquid material of injection device 18.As a result, on ice film 31, be formed uniformly liquid material frost zone 32, as shown in Figure 4, ice film 31 covered fully.That is liquid material frost zone 32 is that the central axis towards the every pipe that constitutes refrigeration/heater 18 radially inwardly increases.When liquid material frost zone 32 has a certain suitable thickness, the every pipe that constitutes device 18 can be possessed when realizing the necessary centre gangway of liquid material freeze drying operation, the liquid material that does not freeze as yet is discharged in the Drainage tank 30 by these passages and discharging tube 27 and goes.In this second embodiment of the present invention, feed tube 26 is same as water inlet pipe, and discharging tube 27 is same as drainpipe.But, also can separately set up water inlet pipe and drainpipe.Naturally be cooled to the freezing point of liquid material owing to reside in the do not freeze liquid material in the borderline region between the remaining part of material of liquid material frost zone 32 Buddhist monks, be collected in liquid material temperature in the Drainage tank 30 and obviously equal to be contained in liquid material temperature in the feed tank 29.The liquid material that is collected in the Drainage tank 30 returns feed tank 29 so that reuse in the circulation next time of freeze drying operation.But, as described below, if the And connection uses many hothouses Zhong liquid material freeze drying Zuo Ye, can be returned to the liquid material of collecting in another feed tank that is communicated with another hothouse of use in the circulation next time and go.In this case, also can be equipped with an independent shared feed tank that is communicated with many hothouses.
In the operating process, temperature just infeeds chuck 23 to carry out cooling operations for-40 to-70 ℃ heat transfer medium or refrigerant after any seat valve door of aqueduct and transfusion pipe material is closed, and the while is caused essential vacuum by means of the vavuum pump (not shown) so that refrigeration/heater element 18 is among the vacuum environment in hothouse 16.At this moment, heat transfer medium infeeds peripheral space 19 between refrigeration/heater element 18 and the heat transfer medium container 17 by pipeline 20 and 21, realizing that the needed heat of liquid material frost zone 32 freeze drying operations supplies with ice film 31 and material frost zone 32, its sense of propriety is any among both of the unlikely thawing ice film 31 of this heat and liquid material frost zone 32.
In the incipient stage of freeze drying operation, liquid material frost zone 32 is attached to above the ice film 31 of covering refrigeration/heater element inwall, so that the phenomenon that distils occurs on the Free Surface of liquid material frost zone 32, and this Free Surface is around the central axis of the every pipe that constitutes device 18.In this case, ice film 31 can finally disappear by the sublimation of self, and liquid material frost zone 32 is separated from refrigeration/heater 18 inwalls.For the liquid material frost zone 32 that prevents to separate drops down from device 18 inner surfaces, the back side of lower end port lid 25 has the frost zone 32 that support member 33 is separated with support.In second embodiment of the invention shown in Figure 4, support member 33 is made by wire netting or wire rod assembly.
After the freeze drying operation was finished, clean air or nitrogen were admitted to hothouse 16, make the internal pressure of hothouse 16 equal atmospheric pressure.After this, be connected the following end And of hothouse 16 and the lower end port lid 25 that can swing is arranged downwards by hinge 34, allow the above-mentioned liquid material frost zone of separating 32, that is be kept at the dry products 32 in the hothouse, fall into product receiver 35, carry out the collection operation of product 32.In collecting operation process, when the lower end port lid was opened, the amount of wandering of product 32 depended on the deadweight of product.Product 32 in the last product receiver 35 and then fall into the following product receiver 36 that the bottom of the same product receiver 35 couples together.Because freeze drying becomes the product 32 of garden tubular very crisp, be several centimetres fragment so when this garden tubular product 32 is subjected to colliding, just be broken into many sizes in its collection operation process.Naturally, when breaking, garden tubular product 32 also can produce a small amount of fine powder of product 32 in product receiver 35.This fine powder trends towards being deposited on product receiver 35 domatic.But, because product receiver 35 is closed fully in liquid material freeze drying operation process, product receiver 35 fine powder on domatic can enter hothouse and to send into the liquid material of drying box chamber 16 in circulating with the freeze drying operation mixed in together next time so needn't worry to be attached to, and therefore just needn't worry that also fine powder can make the debase of product 32.
Fig. 5 and Fig. 6 have shown third embodiment of the invention, and it is the improvement of top second embodiment, thereby, although structurally slightly different between them, as broad as long basically on its function.In Fig. 5 and Fig. 6, for similar parts adopted with Fig. 3 and Fig. 4 in the same label.
Difference on the third embodiment of the invention and second example structure is as follows:
In third embodiment of the invention, form the refrigeration/heater element 40 of ice film 31 and liquid material frozen coating 32 on it all in hothouse 15, but not in hot transfer medium container 41 (label is 17 among second embodiment, sees Fig. 4).In addition, opposite with the refrigeration/heater element 18 of second embodiment of the invention shown in Figure 4, the bottom of refrigeration/heater element 40 of the 3rd embodiment is sealed.As shown in Figure 6, the hot transfer medium container 41 of the 3rd embodiment is positioned on the hothouse 15, also has a plurality of hot transfer medium feed conduits 42 simultaneously.Each manages 42 spaced-apart and be inserted in refrigeration/heater element 40 to form double-wall pipe.
During operation, third embodiment of the invention and second embodiment except following different, basically as broad as long: in the 3rd embodiment, ice film 31 and liquid material frozen coating 32 form on the outer round surface of refrigeration/heater element 40, because water and liquid material are fed in the space of refrigeration/heater element 40 outsides.
In the of the present invention the 3rd and second embodiment, liquid material is delivered to the surface of refrigeration/ heater element 18,40 from fluid supply tank 29, and partly gets back to case 29, uses so that continue in the fluid foods lyophilization cycle afterwards.
Therefore, the present invention the 3rd and second embodiment are suitable for producing continuously single product.Just in these embodiments, liquid material is always near the partly circulation in the case of sealing and pipeline of the temperature bottom of its freezing point.Freezing point is the uncongealable minimum temperature of this liquid material, so that stop bacterium to increase sharply.Opposite with second embodiment with the present invention the 3rd, the first embodiment of the invention shown in Fig. 1 and 2 is suitable for multi-varieties and small-batch periodically produces, and does not give rise to trouble because first embodiment can change liquid material in each lyophilization cycle.
Fig. 7 has shown a kind of freeze drying complete set of equipments that is made of a plurality of second embodiment of the invention.Wherein, replaced a big capacity hothouse 16 to 16-n, so that reduce the time of staying of liquid material in hothouse 16 with a plurality of little volume hothouse 16-1.The ading up to of low capacity hothouse " n ".The same with the situation of frame plate 3 used in the first embodiment of the invention shown in Fig. 1 and 2: in Fig. 7, label 16,28,29,30 and 36 all changes.For example, to hothouse 16, label 16 is changed into from 16-1 to 16-n, and label 16-1 represents first hothouse, and label 16-n then represents n hothouse.
In operation, as shown in Figure 7, the liquid material of getting back to the first fluid discharge case 30-1 is sent to the second fluid supply tank 29-2.If in Fig. 7 equipment 6 groups of hothouses 16 are arranged, finishing a lyophilization cycle required time is 12 hours, at this moment, the quantity of 12 hours fluent material of stop only is 2/100 with the ratio of total output 32 in hothouse, promptly 2%, if deliver to refrigeration/heater element 18 liquid material 52% get back to fluid discharge case 30.
In equipment shown in Figure 7, each unit of hothouse 16 is by the predetermined space sequential working.At first, liquid material is delivered to this equipment from common source 50, then the predeterminable quantity of liquid material is delivered to the first fluid supply tank 29-1.Afterwards, another predeterminable quantity of liquid material is sent to the second fluid supply tank 29-2.By this way the predeterminable quantity of liquid material is delivered to each fluid cassette for supplying 29 of equipment.
On the other hand, the water of scheduled volume is delivered to refrigeration/heater element 18 of the first hothouse 16-1 from water tank 28-1, on the surface of refrigeration/heater element 18 of the first hothouse 16-1, to form one deck ice film 31, then the water that does not freeze is discharged from the first hothouse 16-1.Afterwards, the liquid material of receiving in first fluid supply tank is sent to first hothouse, on the ice film 31 of the refrigeration/heater element 18 that covers the first hothouse 16-1, to form the liquid material frozen coating 32 of predetermined thickness, then, the liquid material that does not freeze is discharged to the first fluid discharge case 30-1 from first hothouse.The liquid material of collecting among the first fluid discharge case 30-1 was delivered to the second fluid supply tank 29-2 by a pump (not shown) again in two hours, mix with liquid material from liquid material common source 50.Like this, liquid material partly cycles through equipment shown in Figure 7, and n the collected liquid material of fluid discharge case 30-N got back to the first fluid supply tank 29-1 again.As a result, behind device start in 12 hours, can be every two hours sequentially from product receiver 36-1,36-2 ..., collect dry good material 32 among the 36-N.
In the equipment shown in Figure 7, can use one or more public fluid supply tanks, one or more fluid discharge casees, one or more common pump, and the sum of these common devices can change on demand.That is to say that the sum of the common device that uses in the equipment can be less than the sum of the hothouse 16 in the equipment.
Fig. 8 and Fig. 9 have shown the fourth embodiment of the present invention, and it is the further improvement to the second and the 3rd embodiment.Therefore, in Fig. 8 and Fig. 9, used with Fig. 3 in Fig. 7 identical label representing identical part, so that the difference of it and front (the second and the 3rd) embodiment is described below.
Fourth embodiment of the invention only shows down on any with the second and the 3rd embodiment difference structurally: different with the second and the 3rd embodiment, in the 4th embodiment, refrigeration/heater element 45 is to constitute by some flat boxes rather than by some pipes.Therefore, the working method of fourth embodiment of the invention is identical with second embodiment.
From the explanation of above embodiment, can know and recognize that the present invention has following advantage:
(1) different with the charging tray/shelf system that has earlier, do not need to hold the container of charging tray one class of fluent material to be dried among the present invention.That is, by the present invention, material to be dried directly is fed on refrigeration/area of heating surface in the hothouse of the present invention.After the freezing dry process of material to be dried finishes,, handle and the mechanism of cleaning container the space of so just saving these mechanisms and being occupied so can save because can be directly from hothouse of the present invention, collect dried material.Can save the space greatly like this;
(2) material to be dried directly contacts with refrigeration/area of heating surface by the ice film, so needn't worry material to be dried generation non-uniform freezing.In addition, cool off under the situation of refrigeration/area of heating surface circulating by hot transfer medium, the heat transfer coefficient between hot transfer medium and refrigeration/area of heating surface is 600 to 700Kcal/m
2Between h ℃ and very stable, and in charging tray/shelf system, the heat transfer coefficient between container and refrigeration/area of heating surface basically 60 to 70Kcal/m
2Between h ℃ and unstable.Therefore, in charging tray/shelf system, the heat conversion between hot transfer medium and material to be dried is subjected to back one coefficient (promptly 60 to arrive 70Kcal/m
2H ℃) influence very big, that is, and the speed average out to 60Kcal/m that heat transmits to material from hot transfer medium
2H ℃.On the other hand, in the present invention, when the ice film thickness is 0.5mm, be stabilized in 400Kcal/m to the heat transfer speed of material from refrigeration/area of heating surface
2About h ℃.Therefore, in an embodiment of the present invention the chilling rate of material to be dried than fast several times of the chilling rate in charging tray/shelf system;
(3) because material to be dried evenly freezes on the film at ice just beginning under the only cold situation, thus in the material pipkrake crystal equably along the direction growth vertical, so that form the material frost zone with the initial chilled surfaces of material.The formation of this pipkrake crystal all is beneficial to heat conversion and steam effusion, carries out freeze drying easily equably.If do not contain ice crystal in the material to be dried, material just can not freeze in its freezing point.As a result, material is by cold excessively, forms one deck freeze adhesion layer on refrigeration/area of heating surface thereby water wherein crystallizes into the microlite of insulation rapidly.Because in the material freezing dry process, this adhesion layer that freezes is easy to fusing, thereby it is evenly dry to influence material;
(4) in addition when the thickness of the lip-deep ice film 31 of refrigeration/heater element quite thin, approximately during 0.5mm, the pore size on the porous layer 32 of its thickness and drying is compared also enough greatly, the size of these micropores is between 0.1mm and 0.01mm.Therefore, the distillation of the ice film 31 on refrigeration/area of heating surface takes place by the crackle that forms in the material that is dried in the material freezing dry process.After the distillation of ice film 31 was finished, the distillation of at least a component of the material that is dried produced at two offsides of material again, thereby strengthened the freeze drying of material, and prevented that the material frozen crust from melting in freezing dry process;
(5) in the time need carrying out the freeze drying operation of material with the container that puts the material that is dried, above-mentioned advantage (1) and (2) have not existed.Yet when icing film when inner surface of container forms, above-mentioned two other advantage (3) and (4) still can obtain.In addition, in this case, the ice film that forms on inner surface of container makes collects dried material or product becomes easily from container, and also needn't clear up container after each lyophilization cycle is finished.
By way of parenthesis, increased the workload that makes the ice film generate and distil among the present invention.Yet this additional work amount is 5% to 10% also littler than the workload of the freeze drying work of the material that is dried, because the moisture in every square metre of material is at least 10Kg/m
2, and the moisture of ice film is about 0.5Kg/m
2Therefore, above-mentioned additional work amount does not almost constitute any shortcoming, because the above-mentioned advantage of the present invention (2) has been saved the energy significantly.
In addition, second, third arrives the present invention (5) advantage with the 4th embodiment above-mentioned except that having (1), also has following advantage;
(6) according to the present invention, material to be dried obtains handling in freezing dry process all the time in the locking device of 0 a ℃ of following temperature and a sealing, and this process operation is simple, and it comprises: automatic valve opens/closed operation in the pipeline; Pump open/stop operation; With opening/closed operation that bottom end cover and hothouse bottom are pivotably connected.In addition, the locking device of the present invention's sealing no longer includes any other movable member except outside the above-mentioned parts (being automatic valve, pump and bottom end cover).Therefore, in the dry materials process, the present invention can realize the environment of high hygiene;
(7), can from vacuum chamber of the present invention or hothouse, remove any movable member according to the present invention.In addition, can automatically deliver to hothouse to material to be dried, automatically dried material or product be collected the product receiver by the action of bottom end cover again then by being arranged in the pipeline automatic valve of carrying material to be dried and the action of pump;
(8) be dried after the frozen coating 32 of liquid material forms, remaining not frozen materials is discharged in hothouse.As a result, the front portion of the acicular crystal of material frozen coating 32 is in vacuum environment basically in freezing dry process, and is not covered by the concentrated noncrystalline film of liquid material or eutectic attitude film.In other words, because it is thin especially to cover the concentrated noncrystalline film of densification of liquid material frozen coating 32 in the present invention, steam can be overflowed from the frozen coating surface of material at an easy rate, strengthen the distillation of frozen coating 32
Up to the present, in order to remove this liquid material film that has concentrated from the surface of frozen coating 32, one deck nylon wire is added in the liquid material surface, the freezing back of liquid material is removed this layer net from frozen coating 32 surfaces; Perhaps on frozen film 32 surfaces, sprayed cold or the water of temperature up to 0 ℃ to water down the concentration that covers the concentrated film on the liquid material frozen coating 31.Afterwards, the material frozen coating that obtains broken into pieces become to be of a size of 1 to 3mm particulate, take in then in the container such as charging tray that in refrigerating process, uses.The liquid material that covers material frozen film 31 surfaces concentrates film and hinders material frozen coating 31 distillation reposefully.In addition, can't prevent that material from concentrating film and breaking suddenly, this will cause dried material or product quality to degenerate.The present invention has overcome these shortcomings.
Because second, third has above-mentioned advantage with the 4th embodiment the present invention, can produce high-quality concentrated liquid material with them.This production is to realize by the freezing dry process that interrupts liquid material before finishing in the distillation of frozen coating 31.In evaporation and concentration, the effusion speed of the velocity ratio that the volatile substances in the liquid material is overflowed from liquid material water vapour wherein is fast, so the volatile substances of liquid material forfeiture is more a lot of than the washiness of forfeiture in evaporation and concentration.Yet, in the distillation of freezing dry process, because the volatile substances in the liquid material is partially absorbed by the concentrated liquid phase of liquid material, so the not loss basically of the volatile substances in the liquid material.After distillation is finished, just obtain dry porous material or product, in standing drying operation, a part of volatile substances and moisture have been lost together.Be the prior art of using during with part freeze drying operation concentrated liquid material above.Yet the shortcoming of this technology is: at first, the manipulation of charging tray is very complicated; The second, in refrigeration operation, generate uneven ice crystal, these crystal hinder frozen materials dry reposefully, and cause local overdrying, make the volatile substances significantly sacrificing in the material.The loss volatile substances can make the dry material or the debase of product.These shortcomings have been overcome by the present invention.
Though at large disclose embodiment preferably of the present invention for illustrative purposes, can affirm that the various changes and modifications of disclosed each embodiment comprise and rearrange its part, all will fall within the scope of the present invention.
Claims (6)
1, a kind of freeze-drying method, comprise the following steps: the water of predetermined quantity is fed on refrigeration/area of heating surface in the vacuum type freeze drying plant hothouse, this refrigeration/area of heating surface is cooled to below 0 ℃ to form an ice film that predetermined thickness arranged thereon; The temperature of this refrigeration/area of heating surface is remained on below 0 ℃; Under these conditions, material to be dried being fed to this ice film surface makes this material freezing on this ice film; With in this hothouse of this vacuum type freeze drying plant, cause vacuum, make distillation of this ice film and the material on it freezing.
2, a kind of freeze drying plant comprises: a hothouse of making vacuum therein; Be arranged vertically the refrigeration/heater in this hothouse, this refrigeration/heater has an inner surface and an outer surface, and one of them forms refrigeration/heating surface and another forms the back side of this refrigeration/heating surface; A hot transfer medium feeding mechanism that hot transfer medium is fed to this back side of this refrigeration/heater; One is fed to this refrigeration/area of heating surface of this refrigeration/heater and confession/drainage arrangement that water is discharged from this hothouse basically equably to scheduled volume water; One is fed to liquid confession/arranging device on the ice film that forms on the refrigeration/area of heating surface of this refrigeration/heater to liquid to be dried; With a lid that is positioned on this hothouse bottom.
3, freeze drying plant as claimed in claim 2, wherein: this hothouse has a hot transfer medium container that has a hot transfer medium confession/row portion; This refrigeration/heater is made of a hollow tube that is arranged in this hot transfer medium container, and this hollow tube has upper shed portion and the under shed portion that connects with this hothouse, and this hollow tube constitutes the inner circumferential surface of this refrigeration/area of heating surface in addition.
4, freeze drying plant as claimed in claim 2, wherein: a hot transfer medium container that has a hot transfer medium confession/row portion is installed in the top of this hothouse; This refrigeration/heater is made of a hollow tube, and its upper shed portion communicates with the hot transfer medium discharge portion of this hot transfer medium container, and this hollow tube also has a bottom of shutting and an outer circumference surface that constitutes refrigeration/area of heating surface; With a hot transfer medium feed conduit, the bottom of its opening is inserted above-mentioned hollow tube and is formed a double-wall pipe, and the hot transfer medium feed portion of the top of this hot transfer medium feed conduit and this hot transfer medium container communicates.
5, freeze drying plant as claimed in claim 2, wherein: this refrigeration/heater is made of a flat boxes, and its external peripheral surface constitutes this refrigeration/area of heating surface.
6, freeze drying plant as claimed in claim 2, wherein: this liquid confession/arranging device is cooled with the pipeline that is connected it and this refrigeration/heater, and the temperature of liquid remains on about 0 ℃ so that this is dried, preferably up to 0 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 88100770 CN1006327B (en) | 1988-02-16 | 1988-02-16 | Freeze dry process and freeze drier |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 88100770 CN1006327B (en) | 1988-02-16 | 1988-02-16 | Freeze dry process and freeze drier |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1035350A true CN1035350A (en) | 1989-09-06 |
| CN1006327B CN1006327B (en) | 1990-01-03 |
Family
ID=4831502
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 88100770 Expired CN1006327B (en) | 1988-02-16 | 1988-02-16 | Freeze dry process and freeze drier |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1006327B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108571862A (en) * | 2017-03-07 | 2018-09-25 | 成都青山利康药业有限公司 | A kind of freeze-drying stripping means of film |
| CN110749162A (en) * | 2019-10-28 | 2020-02-04 | 迪茗（上海）智能科技有限公司 | Suspension freeze drying method for traditional Chinese medicine patch |
| CN116294446A (en) * | 2023-05-17 | 2023-06-23 | 泰州永兴合金材料科技有限公司 | Graphene alloy powder preparation drying equipment |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100455963C (en) * | 2006-04-18 | 2009-01-28 | 沈阳大学 | Method for fast freezing liquid material used for freezing drying technique |
-
1988
- 1988-02-16 CN CN 88100770 patent/CN1006327B/en not_active Expired
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108571862A (en) * | 2017-03-07 | 2018-09-25 | 成都青山利康药业有限公司 | A kind of freeze-drying stripping means of film |
| CN110749162A (en) * | 2019-10-28 | 2020-02-04 | 迪茗（上海）智能科技有限公司 | Suspension freeze drying method for traditional Chinese medicine patch |
| CN116294446A (en) * | 2023-05-17 | 2023-06-23 | 泰州永兴合金材料科技有限公司 | Graphene alloy powder preparation drying equipment |
| CN116294446B (en) * | 2023-05-17 | 2023-08-11 | 泰州永兴合金材料科技有限公司 | Graphene alloy powder preparation drying equipment |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1006327B (en) | 1990-01-03 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US4802286A (en) | Method and apparatus for freeze drying | |
| CN1086802C (en) | Freezing apparatus and method | |
| US5090132A (en) | Method and apparatus for freeze drying | |
| KR20190016903A (en) | Freezing installation | |
| CN204678810U (en) | The temperature controlled vacuum freeze drier of a kind of band | |
| CN111742977A (en) | Thawing apparatus for marine products | |
| CN1006327B (en) | Freeze dry process and freeze drier | |
| CN114719575A (en) | Contact heat transfer type freeze-drying equipment | |
| CN104949473A (en) | Vacuum freeze drying method and vacuum freeze dryer | |
| CN1392384A (en) | Freeze drying device for food and medicine and so on | |
| WO1998000031A1 (en) | A method and a system with a release thawing station for the production of frozen confectioneries, in particular edible ice bodies | |
| CN2888373Y (en) | Freezing-drying machine with liquid nitrogen to assist refrigerate | |
| US3281954A (en) | Freeze-drying apparatus | |
| NZ254174A (en) | Method and apparatus for preparing frozen foodstuffs; products are cooled by a refrigerating assembly before passing through a freezing tunnel on an endless belt | |
| CN115711515A (en) | Freeze drying device is used in preparation of yolk supernatant liquid powder | |
| CN211903512U (en) | Freeze dryer with automatic feeding and discharging system | |
| CN211903511U (en) | Vacuum freeze dryer freeze-drying bin without plate | |
| CN214841894U (en) | Energy-saving constant-humidity fruit and vegetable ice-temperature fresh-keeping warehouse | |
| CN212488259U (en) | Thawing apparatus for marine products | |
| KR910001699B1 (en) | Method and apparatus for freeze drying | |
| CN201704085U (en) | Cryolite rotary steel belt cooling machine | |
| CN2231861Y (en) | Continuous conveying type quick-freezing device | |
| US3516398A (en) | Apparatus for melting a frozen food product | |
| Hay | The vacuum contact‐plate dehydration of foodstuffs. II.—equipment | |
| CN217321655U (en) | Recycled plastic storage bin |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C06 | Publication | ||
| PB01 | Publication | ||
| C13 | Decision | ||
| GR02 | Examined patent application | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C15 | Extension of patent right duration from 15 to 20 years for appl. with date before 31.12.1992 and still valid on 11.12.2001 (patent law change 1993) | ||
| OR01 | Other related matters | ||
| C19 | Lapse of patent right due to non-payment of the annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |