IE46022B1 - Process and device for the production of frozen granultes - Google Patents

Process and device for the production of frozen granultes

Info

Publication number
IE46022B1
IE46022B1 IE2638/77A IE263877A IE46022B1 IE 46022 B1 IE46022 B1 IE 46022B1 IE 2638/77 A IE2638/77 A IE 2638/77A IE 263877 A IE263877 A IE 263877A IE 46022 B1 IE46022 B1 IE 46022B1
Authority
IE
Ireland
Prior art keywords
liquid
cooling agent
frozen
granulates
frozen granulates
Prior art date
Application number
IE2638/77A
Other versions
IE46022L (en
Original Assignee
Boehringer Mannheim Gmbh
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Boehringer Mannheim Gmbh filed Critical Boehringer Mannheim Gmbh
Publication of IE46022L publication Critical patent/IE46022L/en
Publication of IE46022B1 publication Critical patent/IE46022B1/en

Links

Classifications

    • 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
    • F26B5/065—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 the product to be freeze-dried being sprayed, dispersed or pulverised
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23B—PRESERVING, e.g. BY CANNING, MEAT, FISH, EGGS, FRUIT, VEGETABLES, EDIBLE SEEDS; CHEMICAL RIPENING OF FRUIT OR VEGETABLES; THE PRESERVED, RIPENED, OR CANNED PRODUCTS
    • A23B4/00—General methods for preserving meat, sausages, fish or fish products
    • A23B4/03—Drying; Subsequent reconstitution
    • A23B4/037—Freeze-drying, i.e. cryodessication, lyophilisation; Apparatus therefor
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23B—PRESERVING, e.g. BY CANNING, MEAT, FISH, EGGS, FRUIT, VEGETABLES, EDIBLE SEEDS; CHEMICAL RIPENING OF FRUIT OR VEGETABLES; THE PRESERVED, RIPENED, OR CANNED PRODUCTS
    • A23B4/00—General methods for preserving meat, sausages, fish or fish products
    • A23B4/06—Freezing; Subsequent thawing; Cooling
    • A23B4/062—Freezing; Subsequent thawing; Cooling the materials being transported through or in the apparatus with or without shaping, e.g. in the form of powder, granules or flakes
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
    • A23L3/36—Freezing; Subsequent thawing; Cooling
    • A23L3/37—Freezing; Subsequent thawing; Cooling with addition of or treatment with chemicals
    • A23L3/375—Freezing; Subsequent thawing; Cooling with addition of or treatment with chemicals with direct contact between the food and the chemical, e.g. liquid nitrogen, at cryogenic temperature
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
    • A23L3/40—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by drying or kilning; Subsequent reconstitution
    • A23L3/44—Freeze-drying
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25C—PRODUCING, WORKING OR HANDLING ICE
    • F25C1/00—Producing ice
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25D—REFRIGERATORS; COLD ROOMS; ICE-BOXES; COOLING OR FREEZING APPARATUS NOT OTHERWISE PROVIDED FOR
    • F25D3/00—Devices using other cold materials; Devices using cold-storage bodies
    • F25D3/10—Devices using other cold materials; Devices using cold-storage bodies using liquefied gases, e.g. liquid air

Abstract

The device has a cooling column (1) with supply devices for coolant flows (2) and product liquid flows (3) in the centre of the upper part of the cooling column (1) and a removal opening (4) for the granulate at the lower end of the cooling column as well as discharges for gaseous coolant (7). The device serves in particular for manufacturing frozen granulates of foods and pharmaceuticals.

Description

The present invention is concerned with a process and device for the production of frozen granulates.
It is known to preserve foodstuffs, for example fish, meat and vegetables, by freezing. Drinks, for example fruit juices, coffee, tea and soups, can be converted, by freezing and drying in a frozen state, into readily soluble granulates, i.e. into so called instant powders. Pharmaceutical preparations, too, which are administered in the form of a solution but which are not stable in the solvent to be used, have, for many years, been stored in the form of lyophilisates.
In order to avoid the destruction of the structure of the solid foodstuffs or the demixing of the solutions, it is necessary to freeze these products as suddenly as possible. In the past, a large number of techniques have been developed, particularly for freezing solutions.
Thus, it is known to freeze out the solvents in cooled containers in block form and to comminute the blocks by cold grinding. According to another process, the liquid is sprayed on to a cooled, rotating cylinder or on to a cooled conveyor belt from which, after solidification, it is again removed by means of appropriate scrapers or scratchers. In the case of one variant of these apparatus, heat is removed not by cooling the substrate but by spraying on readily evaporating cooling agents, for example, carbon dioxixe, nitrous oxide and, especially, liquid nitrogen. A disadvantage common to all of these processes is that, due to the comminution or removal of 46023 - 3 the frozen product, particles are obtained of greatly varying size and shape, together with a considerable amount of fines, which makes difficult the further working up by the freeze drying (see Sehormuller, Handbuch der Lebensmittelschemie, pp. 262“266, pub. Springer-Verlag, 1974). Furthermore, frozen granulates which are readily flowable, i.e. are substantially spheroidal, are also desired for the production of porous tablets according to the process described in British Patent Specification Ho. 1,381,588 and Patent Specification No. 44571 It is known from British Patent Specification No. 1,376,972 that granulates of substantially uniform shape and size can be obtained when the solution to be frozen is sprayed through appropriate nozzles into a moving bath of a boiling fluorinated hydrocarbon, such as Freon, as cooling agent.
(Freon is a Registered Trade Mark,. The resultant granulate is normally removed discontinuously since a continuous removal requires the use of expensive apparatus. Products frozen on to parts of the apparatus, especially on to the stirrer, make it difficult to change quickly from one product to another, this only being possible after complete emptying, warming and thorough cleaning of the plant.
Therefore, the problem exists of providing a continuous process for the production of uniform, frozen granulates for freeze drying which, with the lowest possible expense for apparatus, permits a rapid change from one product to another.
According to the present invention, there is provided a process for the production of frozen granulates, wherein a liquid product solution is introduced into a moving stream of a readily evaporable liquid cooling agent and the frozen granulates of the product remaining after evaporation of the 6 0 2 2 - 4 cooling agent are separated off.
The process of the present invention results in the liquid product solution being suddenly frozen to give small, spheroidal particles. These spheroids can then easily be separated after evaporation of the gaseous cooling agent, freeze dried by known processes and further worked up. The freeze-dried granulates produced in this manner are, surprisingly very uniform, dissolve readily and can be readily worked up due to their spheroidal shape, whereas, in point of fact, non10 uniformly-formed granules or snowflake-like products of greatly varying size distribution were to have been expected.
Especially good results are achieved when the streams of liquid product solution and liquid cooling agent run in the direction of the gravitational force since an especially long15 lasting heat exchange is thereby achieved. On the other hand, by an oblique guiding of the streams from below upwardly, the result is achieved that the granules formed, on the basis of their size, drpp down from the stream of liquid cooling agent at different speeds and thus a classification or grading is achieved insofar as there are again formed granules of greatly differing size.
As liquid cooling agent, there can be used all liquid materials which evaporate at atmospheric pressure below the freezing point of the liquid product solution and which do not react with the product. By way of example, there can be mentioned nitrous oxide, alkylene oxides, ammonia, carbon dioxide, low boiling point hydrocarbons, such as butane and propane, and fluorinated hydrocarbons, such as Freon. Liquid nitrogen has proved to be especially advantageous since it is inexpensive to obtain, does not react with any of the liquid product solutions, does not cause contamination of the environ46022 - 5 msnt due to escaping gases and, because of its low boiling point, cools the product very quickly to a low temperature. In the case of products which are not sensitive to oxygen, liquid air can also be used in the same manner.
The present invention also provides a device for the continuous production of frozen granulates, comprising a cooling column, supply means for streams of liquid cooling agent and streams of liquid product solution in the centre of the upper part of the column, a removal opening for the frozen granulates of the product at the lower end of the cooling column and removal means for evaporated cooling agent.
One embodiment of the device according to the present invention is illustrated in Fig. 1 of the accompanying drawings. This device comprises a vertically standing, conically-shaped cooling column (1) which narrows in the downward direction, the upper part of the column having a centrally positioned inlet nozzle (2) for a liquid cooling agent, as well as one or more nozzles (3) for a liquid product solution and on the lower end of the column having an opening (4) for the removal of frozen granulates of the product and for the escape of evaporating cooling agent. The column (1) is preferably provided with an insulating outer mantel (5), as well as with an inner lining (6), between which evaporated cooling agent flows off, as cooling and insulating material, via a valve (7). Furthermore, for the supply of liquid cooling agent and of liquid product solution, there are provided regulatable valves (8) and (9).
The amount of gaseous cooling agent flowing off via valve (7), which serves for the cooling of the outer mantel, can be regulated by an additional over-pressure valve (10) provided in an outlet at the top of the column (1). The liquid cooling agent is fed in via a pipe (11) from a storage container (12), 6 0 2 2 - 6 the pressure in this storage vessel bringing about the conveyenc ing of the liquid qooling agent. The storage container (12) is preferably constructed with double walls and can be cooled by cooling agent removed via valves (7) and (10), through a pipe (14). The liquid product solution is taken from a storage container (13), which is preferably also constructed with double walls and can also be cooled by cooling agent removed via valves (7) and (10), through pipe (14), through a pips (15) and forced by means of a pump (16) and through valve (9) into the product nozzle (3). The product nozzle is preferably heatable in order to prevent freezing up. The frozen granulate falling out through the opening (4) due to the gravitational force can be collected in a collection container and passed discontinuously to a freeze drying plant.
Preferably, however, the granulate falling out is passed continuously on a conveyor belt (17) through a continuous freeze drying apparatus (18) and thereafter passes into a confectioning or storage station (19). For protection against anibient temperature and moisture, the conveyor belt (17) is, up to the point of entry into the freeze drying plant, also surrounded by a mantel (20), the inner space of which can also be cooled by the evaporating cooling agent. If liquid nitrogen or liquid air is not used as the cooling agent, then it is also necessary to provide a device for the collection or reliquifaction of the evaporated cooling agent.
Fig. 2 of the accompanying drawings schematically shows a cross-sectional view of an arrangement according to the present invention of 6 liquid product solution nozzles (3) with supply pipe (15) and liquid cooling agent nozzle (2).
It has proved to be advantageous to supply the liquid product solution to the nozzles with a temperature just a - 7 little above the freezing point of the solution since, in this way, the liquid cooling agent is best utilised. By variation of the diameter of the nozzles (2) and (3) and of the pressure with which the liquid cooling agent and the liquid product solution is sprayed in, the size and solids content of the granules can be varied within wide limits. The size and solids content of the granules can also be varied by the concentration and viscosity of the liquid product solution. For economic reasons, the amount of liquid cooling agent fed in is adjusted in such a manner that it just suffices to freeze the liquid product solution and to cover the heat losses to the surroundings. Depending upon the concentration of the liquid product solution, in the case of the preferred use of liquid nitrogen, the consumption of cooling agent is 2—3 kg. per kg. of liquid product solution.
Of course, numerous variations of the above-described apparatus are conceivable with which the process according to the present invention can also be carried out. Thus, for example, the columns can, of course, also be cylindrical or double-conical, instead of a simple liquid cooling agent and liquid product solution feed in, several such nozzles can also be provided and the products can, instead of being continuously passed to a freeze drying plant, also be collected in a storage tank and then used at some later time.
For the construction of the device, it is possible to use practically all materials which still have, at the temperature of the liquid cooling agent, a sufficient stability and strength, stainless steel, copper, polyethylene and the like being mentioned by way of example.
By a simultaneous spraying in, via two different nozzles, it is possible to spray components which are incompatible with one another and thus to obtain a statistically mixed granulate. (Β $ 2.2 - 8 By means of a different nozzle size or of a different spray pressure, if desired there can also be obtained a differing particle size for a particular granulate.
The following Example is given for the purpose of illustrating the present invention:Example 1. Formation of the frozen granulate.
Use was made of a cooling column (1) according to Fig. 1 of the accompanying drawings which had a height of 200 cm., a diameter of 80 cm and an outlet opening (4) with a width of 20 cm. The upper cylindrical part of the column had a length of 60 cm. and the conically-shaped part had an angle of 30° from the vertical. Pipes, valves and storage vessels were according to Fig. 1 but instead of the illustrated continuously operating freeze drying plant, there was employed a cooled storage vessel below the exit opening (4). kg. Saccharose was dissolved in 10 litres distilled water to give a 10% solution which was placed in a thermostatically controlled storage vessel (13) and kept there at a temperature of about +1°C., the freezing point of this solution being about -0.5°C.
From a second storage container (12), liquid nitrogen (LN2) was supplied via an insulated copper pipe (11) and a regulating valve (8) to the LN2 nozzle, this nozzle having an inner diameter of 8 mm. The reaction chamber (1) was precooled until, at the outlet opening (4), a temperature of about -50°C. was achieved in the outflowing stream of nitrogen.
Then, by means of pump (16), at a spraying in pressure of 1.5 bar., the saccharose solution was sprayed, via a polyethylene pipe (15), a regulating valve (9) and six product nozzles (3), into the stream of liquid nitrogen. The six nozzles, which -9.were arranged in the form of a circle at a conical angle of 60° around the LN2 stream, had an inner diameter of about 0.15 mm. The distance between the exit point of the LN2 from the LN2 nozzle and the point of mixing with the solution was 125 mm. and the distance from the product nozzle to the mixing point was 30 mm. Upon contact with the LN2 stream, the saccharose solution froze suddenly to give small spheroids, whereas the greater part of the LN2 evaporated. This gaseous, cold nitrogen was further used for cooling the reaction chamber (1) and the storage container (13).
The frozen spheroids fell downwardly in the reaction chamber (1) and were removed through the opening (4) and collected in a deep-cooled Dewar vessel. The diameter size of these spheroids was between 0.16 and 1.0 mm., the Gaussian distribution having its maximum at 0.63 mm. with 85% by weight of the particles. Over 99% of the granulate had a spheroidal shape. It flowed readily and did not stick together. In a cooled container, if can be stored practically without time limit.
The consumption of LN2 was 2.5 kg/kg. of solution (including pre-cooling of the reaction chamber and losses). 2. Freeze drying of the frozen granulate.
The frozen spheroids collected in the Dewar vessel were shaken on to a pre-cooled metal sheet (-50°C.) of a lyophilisation plant and discontinuously freeze-dried under the following conditions: (a) 13 hours at 0.2 nibar and 25°C. (b) 5 hours at 1.333 10-3 mbar and 25°C.
After lyophilisation, the particle size distribution and the spheroidal form of the granulate had not changed from that of the frozen state. Its density was calculated to be about 6 0 2 2 - 10 3 116 kg./m . The residual water content was 1.6% by weight.
The product had a homogeneous, white colour. Upon shaking up and sieving,the granulate retained its shape. It could easily be rubbed between the fingers. The electrostatic charging was 5 low. The spheroids scarcely stuck together and did not stick at all to the walls of bottles in which it was stored. The flowability was very good, the flow behaviour of the granulate resembling that of a liquid. In order again to produce the initial concentration of the 10% saccharose solution, 100 g. of granulate were added to 1 litre of distilled water. Without mechanical movement of the liquid, the dissolving time was 32 seconds.

Claims (10)

1. CIAIMS:1. A device for the continuous production of frozen granulates, comprising a cooling column, supply means for streams of liquid cooling agent and streams of liquid product solution in the centre of the upper part of the column, a removal opening for the frozen granulates of the product at the lower end of the cooling column and removal means for evaporated cooling agent.
2. A device according to claim 1, wherein the product removal opening is connected via a conveyor belt with a continuously operating freeze drying plant.
3. A device according to claim 1 for the continuous production of frozen granulates, substantially as hereinbefore described and exemplified.
4. A process for the production of frozen granulates, wherein a liquid product solution is introduced into a moving stream of a readily evaporatable liquid cooling agent and the frozen granulates of the product remaining after evaporation of the cooling agent are separated off.
5. A process according to claim 4, wherein the stream of liquid cooling agent moves downwardly in the direction of the gravitational force.
6. A process according to claim 4 or 5, wherein the size and solids content of the granules is varied by the concentration, viscosity and spray in pressure of the liquid product solution, as well as by the nozzle diameter.
7. A process according to any of claims 4 to 6, wherein the liquid cooling agent used is liquid nitrogen.
8. A process according to claim 4 for the production of frozen granulates, substantially as hereinbefore described 4 6 0 2 2 12 and exemplified.
9. Frozen granulates, whenever produced with the device according to any of claims 1 to 3.
10. Frozen granulates, whenever produced by the process 5 according to any of claims 4 to 8.
IE2638/77A 1976-12-30 1977-12-29 Process and device for the production of frozen granultes IE46022B1 (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DE19762659546 DE2659546A1 (en) 1976-12-30 1976-12-30 METHOD FOR PRODUCING FROZEN GRANULES

Publications (2)

Publication Number Publication Date
IE46022L IE46022L (en) 1978-06-30
IE46022B1 true IE46022B1 (en) 1983-01-26

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ID=5997030

Family Applications (1)

Application Number Title Priority Date Filing Date
IE2638/77A IE46022B1 (en) 1976-12-30 1977-12-29 Process and device for the production of frozen granultes

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JP (1) JPS53114783A (en)
AR (1) AR214108A1 (en)
AT (1) AT356498B (en)
AU (1) AU506746B2 (en)
BE (1) BE862370A (en)
CA (1) CA1106686A (en)
CH (1) CH625332A5 (en)
DD (1) DD133295A5 (en)
DE (1) DE2659546A1 (en)
FI (1) FI773941A (en)
FR (1) FR2375901A1 (en)
GB (1) GB1559920A (en)
IE (1) IE46022B1 (en)
IL (1) IL53695A0 (en)
IT (1) IT1089419B (en)
NL (1) NL7714401A (en)
SE (1) SE7714822L (en)
ZA (1) ZA777184B (en)

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FR2983286B1 (en) * 2011-11-24 2018-04-13 L'air Liquide,Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude DEVICE FOR COOLING BULK PRODUCTS
CN103123196B (en) * 2013-02-06 2015-08-26 邹杰 A kind of cold-storage apparatus
JP5837670B2 (en) * 2014-10-24 2015-12-24 アイエムエー ライフ ノース アメリカ インコーポレーテッド Bulk freeze drying using spray freezing and stirring drying
CN105597622B (en) * 2016-03-09 2017-11-21 苏州大学 The controllable spray chilling tower for being used to prepare micron order ice hockey particle of freezing temperature
CN106113314B (en) * 2016-08-15 2019-06-21 浙江心源科技有限公司 A kind of spray crystallization prilling granulator and its prilling process
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NL7714401A (en) 1978-07-04
GB1559920A (en) 1980-01-30
JPS53114783A (en) 1978-10-06
CH625332A5 (en) 1981-09-15
AU506746B2 (en) 1980-01-24
IL53695A0 (en) 1978-03-10
CA1106686A (en) 1981-08-11
ATA940677A (en) 1979-09-15
AR214108A1 (en) 1979-04-30
SE7714822L (en) 1978-07-01
DD133295A5 (en) 1978-12-27
IE46022L (en) 1978-06-30
FR2375901A1 (en) 1978-07-28
IT1089419B (en) 1985-06-18
ZA777184B (en) 1978-10-25
BE862370A (en) 1978-06-27
AU3192277A (en) 1979-06-28
DE2659546A1 (en) 1978-07-13
FI773941A (en) 1978-07-01
AT356498B (en) 1980-04-25

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