AU593499B2 - Creación de Inventos y Patentes con Inteligencia Artificial

AU593499B2 – Device for the controlled freezing of viscous liquids
– Google Patents

AU593499B2 – Device for the controlled freezing of viscous liquids
– Google Patents
Device for the controlled freezing of viscous liquids

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Publication number
AU593499B2

AU593499B2
AU14047/88A
AU1404788A
AU593499B2
AU 593499 B2
AU593499 B2
AU 593499B2
AU 14047/88 A
AU14047/88 A
AU 14047/88A
AU 1404788 A
AU1404788 A
AU 1404788A
AU 593499 B2
AU593499 B2
AU 593499B2
Authority
AU
Australia
Prior art keywords
liquid
container
bath
frozen
freezing
Prior art date
1987-04-02
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.)

Ceased

Application number
AU14047/88A
Other versions

AU1404788A
(en

Inventor
Jurgen Buchmuller
Gunther Weyermanns
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)

Messer Griesheim GmbH

Original Assignee
Messer Griesheim 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.)
1987-04-02
Filing date
1988-03-31
Publication date
1990-02-08

1988-03-31
Application filed by Messer Griesheim GmbH
filed
Critical
Messer Griesheim GmbH

1988-10-06
Publication of AU1404788A
publication
Critical
patent/AU1404788A/en

1990-02-08
Application granted
granted
Critical

1990-02-08
Publication of AU593499B2
publication
Critical
patent/AU593499B2/en

2008-03-31
Anticipated expiration
legal-status
Critical

Status
Ceased
legal-status
Critical
Current

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Classifications

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

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

A23L3/361—Freezing; Subsequent thawing; Cooling the materials being transported through or in the apparatus, with or without shaping, e.g. in form of powder, granules, or flakes

A—HUMAN NECESSITIES

A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES

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

A23L3/361—Freezing; Subsequent thawing; Cooling the materials being transported through or in the apparatus, with or without shaping, e.g. in form of powder, granules, or flakes

A23L3/362—Freezing; Subsequent thawing; Cooling the materials being transported through or in the apparatus, with or without shaping, e.g. in form of powder, granules, or flakes with packages or with shaping in form of blocks or portions

C—CHEMISTRY; METALLURGY

C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING

C12N—MICROORGANISMS OR ENZYMES; COMPOSITIONS THEREOF; PROPAGATING, PRESERVING, OR MAINTAINING MICROORGANISMS; MUTATION OR GENETIC ENGINEERING; CULTURE MEDIA

C12N1/00—Microorganisms, e.g. protozoa; Compositions thereof; Processes of propagating, maintaining or preserving microorganisms or compositions thereof; Processes of preparing or isolating a composition containing a microorganism; Culture media therefor

C12N1/04—Preserving or maintaining viable microorganisms

Abstract

A device for the controlled deep freezing of viscous liquids by means of a low boiling liquified gas is used for producing drops from the liquid, which are frozen to pellets in a liquid nitrogen bath. The device includes a container arranged above the bath to hold the liquid to be frozen. The bottom of the container consists of two drip plates which can be moved in relation to each other and are provided with bores.

Description

2- Form COMMONWEALTH OF AUSTRALIA PATENTS ACT 1952-69 COMPLETE SPECIFICATION
(ORIGINAL)
Class Application Number: Lodged: I t. Class Complete Specification Lodged: Accepted: Published: «Priority Related Art: 593499- This documecnt coiitaiins the faineidrnents mnade Wider QSection 49 arid is correct for.
printig.
0 Name of Applicant: Address of Applicant: 6Aotual Inventor.
Address for Service: MESSER GETESHEIM GMBH Hanauer Landstrasse 330, 6000 Frankfurt/Main, Federal.
Republic of Germany JURGEN BUCKMULLER and GUNTHER WEYERMANNS EDWD. WATERS SONS, 50 QUEEN STREET, NIELBOURNE, AUSTRALIA, 3000.
Complete Specification for the invention entitled: DEVICE FOR THE CONTROLLED FREEZING OF VISCOUS LIQUIDS The following statement is a full description of this invention, including the best method of performing it known to -2- DEVICE FOR THE CONTROLLED FREEZING OF VISCOUS LIQUIDS Bacgon of the Invention Liquids can be preserved when they are frozen in bags or bottles made of plastic material and, if necessary, are vacuum dried. When these are sensitive liquids with organic components, freezing must take place as quickly and uniformly as possible, in other words, controlled to prevent cold damage. Thi~s applies, in particular, when these organic components are living cells, for example, bacteria suspensions. When freezing is uncontrolled, the wall of the cell and cellular tissue may be destroyed as a result of a severe ice crystal formation.
Such a bacteria suspension consists, for example, of 95% water an~d 5% bacteria. With iincontrolled freezing, the survival rate of these cells may drop to an unacceptable low degree. But liquids with other organic components, for *too% example, albumen solutions, vitamin solutions and vaccines foe* may be damaged by uncontrolled freezing. A proven method of freezing such liquids for the purpose of preservation is to freezing by means of a low boiling liquified gas, as a rule nitrogen. With liquid nitrogen as refrigerant, the liquid, for example, in bags or ampules can be cooled very quickly to the desired freezing temperature so that there is, for example, little time for an extensive ice crystal But some time is needed to freeze such a liquid specimen from the outside to the inside so that to some degree inevitable cold damage and concentration of components in the core of the liquid occur.
British Pat. No. 1,376,972 discloses a device 30which provides for a very gentle freezing of such a liquid, namely, liquid egg. With this device, drops of liquid egg are produced, led into a bath consisting of a low-boiling liquified gas from which they are removed in the form of frozen pellets. The liquid can be deep frozen extremelyt to the target tempei ‘ature because the drop has a small volume. This is still enhanced by the direct heat exchange between liquid and cooling medium since separating r 1 drops results, moreover, in a ratio of liquid surface to volume which is optimum for uniform freezing. The drops are produced with a peristaltic pump by a periodic compression of flexible tubes filled with the liquid to be frozen so that drops of the liquid are expelled from the flexible tube and through nozzles are led into the refrigeration bath.
This type of drops production is cumbersome. The peristaltic pump is a relatively complicated and trouble-prone machine which requires a constant monitoring.
Since it is placed in the immediate vicinity of the cooling medium bath, there is the risk that the nozzles ice up.
When a certain pellet diameter must be abFolutely 15 maintained, there are also problems since with the known device only pellets having a somewhat same diameter can be produced. A controlled freezing or sensitive liquid requires, however, drops and pellets having a uniform size f because identical and, therefore, controlled freezing r’r’ conditions can only be realised with such uniform sizes.
The known device also has only limited possibilities, for example, for varying the size of the drops via the throughput. But when different liquids having a different viscosity are to be frozen to pellets, it is often desirable i that a certain pellet size is associated with a certain c 25 liquid.
Summary of the Invention The invention is based on the objective of providing a device for the controlled deep freezing of 30 viscous liquids to frozen pellets which makes the production 0, possible of pellets having almost the same diameters, the k t r variation of the pellet size and is simple, rugged and substantially maintenance-free..
The condition that the liquid to be frozen must be viscous only means that drops having a defined size can be produced from the liquid. Liquids with a very broad viscosity range are, therefore, suitable for the device of the invention; only very low viscosity liquids are not 4, -4suitable. It is important that the drops, while falling into the cooling medium bath, have sufficient time to assume the spherical shape. But the drops also may not enter the bath, for example, consisting of liquid nitrogen at too high a speed since the spherical shape of the drops might then be impaired. In addition to the size of the drops, their falling path into the liquid nitrogen bath, in other words, their drop height is decisive for an optimum freezing of the liquid. The appropriate optimum drop height can be easily determined for each liquid by simple tests.
Another important criterion for an optimally controlled freezing process is the dwell time in the bath consisting of liquid cooling medium. The dwell time can be simply regulated by means of a conveyor belt running through 15 the bath and known per se, which has baffles to transport the liquid drops frozen to pellets.
The Drawings FIG. 1 shows a complete deep freezing installation and subsequent vacuum drying; 20^ FIG. 2 shows the freezing and drop formation device of FIG. 1 on an enlarged scale; FIG. 3 shows a section of FIG. 2; and FIG. 4 shows a detail of the drop formation device.
Detailed Description t 25 The essential parts of the installation shown in 25 FIG. 1 consists of the drop formation device 1, the freezing io unit 2, the catching device 3, a freezer 4 and a vacuum drier 5. The liquid to be frozen in present in the drop formation device 1 and drips into a liquid nitrogen bath 6 30 present in the freezing unit 2. A conveyor belt 7 runs r« through the bath 6 at an adjustable rotational speed.
Liquid nitrogen arrives through line 8 in the freezing unit 2 to replace the evaporated nitrogen. The evaporated nitrogen is withdrawn from the freezing unit 2 through the i pipe 9 by means of the fan 10 and serves to keep the freezer i 4 used as intermediate storage at a suitable temperature, for example, -60 0 C. The flow and travel directions are indicated by arrows without reference numbers.
BA 4 ‘y The liquid dripping from the drop formation device 1, according to the. invention, into the liquid nitrogen bath 6 freezes there to pellets and, after a predetermined dwell time, is carried away from the bath 6 by the conveyor belt 7. The pellets drop through the funnels 11 and 12 into the catching device 3 where they are caught in basins. The basins filled with pellets are placed in the freezer 4 for intermediate storage. They are then placed in the vacuum drier 5 from’ which the finished product can be removed.
The pellets falling from the funnel 12 can of course also be directly caught in bags and stored in a freezer, for example, at -40 0
C.
FIG. 2 shows the freezing unit 2 somewhat enlarged.
The whole freezing unit 2 is surrounded by an insulation 13 S 15 to diminish the cold losses. The drop formation device 1 also has an insulation 14 to keep the liquid to be deep S tsb. frozen at an as constant as possible temperature. The detail characterized by the dash-dot circle 15 is shown in FIG. 3 in an enlarged perspective drawing.
t 20 FIG. 3 shows a part of the trough 16 which contains the liquid nitrogen bath 6. The conveyor belt 17 slides through the bath 6 and is provided with baffles 18. The surface 19 of the liquid nitrogen is higher than the baffles 18. The pellets 20 to be deep frozen are present between t the baffles 18 and are deep frozen to a core temperature of 25 0
C.
The drop formation device 1 is found above the liquid nitrogen bath 6. This device essentially consists of a container 21 which holds the liquid 22 to be frozen. The 30 bottom of the container 21 consists of the drip plates 23 Sand 24. The drip plates 23, 24 are provided with bores and have more or less open area by moving one drip plate, preferably, the bottom drip plate 23 so that variable thLottling positions are produced which control the flow rate of the liquid 22 to be frozen in such a way that the drop sequence is determined. The drip plates 23, 24 are, preferably, exchangeable so that drip plates with different size bores 25 can be used depending on the viscosity of the j- liquid 22 to be frozen and on the desired drop size.
-6- FIG. 4, on an enlarged scale, shows a perspective drawing of parts of the drip plates 23 and 24 with a bore Depending on the viscosity of the liquid to be frozen, the annular surface is either larger or smaller.
3 also shows other devices which make sure that the drops 26 have a constant size. The proximity switch 28, for example, keeps the level of the liquid 22 constant and controls the appropriate liquid delivery through the line 29 so that the pressure of the liquid 22 in front of the bores 25 is constant. Instead of the proximity switch 28, also other means used for this purpose may be employed. The container 21 is, moreover, surrounded by a heating tape 30 which keeps the temperature of the liquid 22 constant.
15 This is important since the viscosity of the liquid t is highly dependent on the temperature, the viscosity in turn is codecisive for the viscosity of the drops 26 and a freezing up of the bores 25 is prevented at the same time.
The device according to the invention can, therefore, be used to produce drops having a constant and reproducible size from a given liquid. A controlled deep freezing then only still requires that the drops penetrate the nitrogen bath in spherical shape and that the dwell time r in the nitrogen bath is exactly fined. The dwell time is exclusively determined by the rotational speed of the conveyor belt 17. The baffles 18 make sure that all drops 26 immediately after they dip into the liquid nitrogen are n moved through the bath 6 for a predetermined time whereby they are frozen to pellets having the desired core temperature. In order to attain the desired spherical shape ?which makes an extremely uniform deep freezing possible, the fall height of the drops 26 must be adapted to the appropriate liquid. Very viscous liquids require longer falling paths since they are slower to assume the spherical shape. The best fall height can be quickly found by means of a few tests since the shape of the pellet immediately demonstrates whether the fall height is optimum.
L
-7- The device according to the invention is suitable for all liquids having a viscosity which allows for a controlled and reproducible drop formation. Bacteria suspensions with solids fractions ranging from 8 to 16 wt.% were successfully frozen, for example. These bacteria suspensions had viscosities ranging from 0.001 to 12.5 Ns/M 2 and surface tensions from 0.05 to 0.08 Ns/m. Depending on the viscosity of the bacteria suspensions to be frozen, drop plates with different dimension bores were used. The smallest bore diameter was 0.7 mm, the largest bore diameter was 2 mm. The thickness of the drip plate facing the *nitrogen bath also influences the size of the produced drops to some extent. But the height of the drop, in other words, the distance of the bottom drip plate from the level of the to 15 nitrogen bath has a much greater influence. In individual 15 cases, for example, optimum drop heights ranging from 50 to 120 mm were determined. The diameter of the spherical pellet obtained in this way was between 2 and 5 mm. A certain bore diameter, a certain drop height and a certain sphere diameter must always be associated with a certain bacteria suspension.
Summary Viscous liquids, for example, bacteria suspensions S or vaccines can be deep frozen in low-boiling liquified gases by producing drops from the liquid, which are frozen to pellets. For the production of pellets having X»f substantially equal diameters, a container 21 is used which is arranged above the bath 6 consisting of liquified gas which is filled with the liquid 22 to be frozen. The bottom of the container consists of two drip plates 23, 24 provided i ;with bores 25 which can have more or less open area so that a variable throttling position is produced which determines the flow rate of the liquid and, therefore, the sequence of r t the drops. Viscosity of the liquid and the diameter of the I bore determine the drop size. The discharge edges of the bores are designed as release edges to make the size of the drops as uniform as possible (FIG. 3).
JVT C (c*AI T zi;. j

Claims (7)

1. In a device for the controlled deep freezing of viscous liquids by means of a low-boiling liquified gas, which device is used for the production of drops from the liquid, which are frozen to pellets in a liquid nitrogen bath, the improvement bei’ig in that said device includes a liquid nitrogen )th, a container arranged above said bath to hold the liquid to be frozen, viscous liquid supply means communicating with said container, the bottom of said container consisting of two drip plates which can be moved .v in relation to each other, and said drip plates being provided with alignable bores.

2. Device according to claim 1, charcterized in that the edges of said bores of said bottom drip plate facing the surface of said bath are designed as release edges.

3. Device according to claim 2, characterized by means for maintaining a constant liquid level in said container.

4. Device according to claim 3, characterized by a heating tape surrounding said container to maintain a constant temperature of said liquid. 4 4

5. Device according to claim 2, characterized by a heating tape surrounding said container to maintain a i constant temperature of said liquid.

6. Device according to claim 1, characterized by a heating tape surrounding said container to maintain a i constant temperature of said liquid. O T i 1 i i. .1 ‘4 t i 2~1 -9-

7. Device according to claim 1, characterized by means for maintaining a constant liquid level in said container. DATED this 9th day of August, 1989. MESSER GRIESHEIM GMBH WATERMARK t 4 4*44 4 4 4~4 I III *444 I 4 PATENT ATTORNEYS, 50 QUEEN STREET MELBOURNE VIC. 3000 44 4 4 4 4 1 44 II 4 4 4* 4 84 1.55/129/OK

AU14047/88A
1987-04-02
1988-03-31
Device for the controlled freezing of viscous liquids

Ceased

AU593499B2
(en)

Applications Claiming Priority (2)

Application Number
Priority Date
Filing Date
Title

DE19873711169

DE3711169A1
(en)

1987-04-02
1987-04-02

DEVICE FOR CONTROLLED FREEZING OF TOW FLOWING LIQUIDS

DE3711169

1987-04-02

Publications (2)

Publication Number
Publication Date

AU1404788A

AU1404788A
(en)

1988-10-06

AU593499B2
true

AU593499B2
(en)

1990-02-08

Family
ID=6324745
Family Applications (1)

Application Number
Title
Priority Date
Filing Date

AU14047/88A
Ceased

AU593499B2
(en)

1987-04-02
1988-03-31
Device for the controlled freezing of viscous liquids

Country Status (15)

Country
Link

US
(1)

US4829783A
(en)

EP
(1)

EP0284837B1
(en)

JP
(1)

JPH0740915B2
(en)

CN
(1)

CN1017969B
(en)

AT
(1)

ATE84137T1
(en)

AU
(1)

AU593499B2
(en)

CA
(1)

CA1307402C
(en)

DE
(1)

DE3711169A1
(en)

ES
(1)

ES2038226T3
(en)

FI
(1)

FI881276A
(en)

GR
(1)

GR3007485T3
(en)

NO
(1)

NO168285C
(en)

NZ
(1)

NZ224021A
(en)

TR
(1)

TR25208A
(en)

ZA
(1)

ZA882329B
(en)

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Method and equipment for manufacturing frozen particle by using confinement band of atomized cryogenic droplet

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1993-08-30
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Buse Gase Gmbh & Co
Process and apparatus for pellet freezing of pelletisable liquids

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1994-06-16
1995-07-20
Buse Gase Gmbh & Co
Method of pelletising material

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1995-02-24
2003-10-02
Air Liquide Gmbh

Device for freezing liquid substances using a refrigerant

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1999-06-01
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Hiran Asoka Malinga Ratwatte
A method of tableting

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1999-08-27
2001-03-01
Lohmann Therapie Syst Lts

Rapidly disintegrating pellets based on chitosan

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1999-11-23
2001-06-13
Messer Griesheim Gmbh

Method and device for pelleting a liquid or pasty mass

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1999-11-23
2001-06-13
Messer Griesheim Gmbh

Method and device for pelleting a liquid or pasty mass

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2001-12-10
2003-06-26
Hte Ag The High Throughput Exp
Production of shaped body used as e.g. ion exchanger, by dividing settable and flowable composition into droplets, freezing droplets using coolant, and drying and/or calcining frozen droplets

CA2789993C
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2003-04-11
2016-02-16
Cargill, Incorporated
Pellet systems for preparing beverages

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2003-10-29
2008-08-19
The University Of Mississippi
Process and apparatus for producing spherical pellets using molten solid matrices

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2004-07-23
2011-12-07
バイエル・テクノロジー・サービシーズ・ゲゼルシャフト・ミット・ベシュレンクテル・ハフツング

Aseptic freezing, drying, storage, analysis and filling method (SFD-SAF method) (pellet lyophilization method for parenteral biopharmaceuticals)

DE102005053695B4
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2005-11-10
2008-04-30
Airbus Deutschland Gmbh

Method for handling a liquid

EP2550873A1
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2011-07-29
2013-01-30
AMBIENTE E NUTRIZIONE S.r.l.
Process for the deep-freezing of a fluid food preparation

JP6596250B2
(en)

2015-07-22
2019-10-23
大陽日酸株式会社

Droplet production equipment

CN114311390B
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2022-03-17
2022-10-11
山东海科创新研究院有限公司
High-viscosity liquid phase granulation equipment

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Process and apparatus for freezing liquid or semiliquid foods in the form of essentially uniform pellets

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patent/DE3711169A1/en
active
Granted

1988

1988-03-08
EP
EP88103595A
patent/EP0284837B1/en
not_active
Expired – Lifetime

1988-03-08
AT
AT88103595T
patent/ATE84137T1/en
not_active
IP Right Cessation

1988-03-08
ES
ES198888103595T
patent/ES2038226T3/en
not_active
Expired – Lifetime

1988-03-08
NO
NO881025A
patent/NO168285C/en
unknown

1988-03-17
FI
FI881276A
patent/FI881276A/en
not_active
Application Discontinuation

1988-03-25
NZ
NZ224021A
patent/NZ224021A/en
unknown

1988-03-29
CA
CA000562772A
patent/CA1307402C/en
not_active
Expired – Fee Related

1988-03-31
AU
AU14047/88A
patent/AU593499B2/en
not_active
Ceased

1988-03-31
ZA
ZA882329A
patent/ZA882329B/en
unknown

1988-04-01
TR
TR88/0244A
patent/TR25208A/en
unknown

1988-04-01
CN
CN88101711A
patent/CN1017969B/en
not_active
Expired

1988-04-01
JP
JP63078281A
patent/JPH0740915B2/en
not_active
Expired – Lifetime

1988-04-04
US
US07/176,928
patent/US4829783A/en
not_active
Expired – Lifetime

1993

1993-03-26
GR
GR930400670T
patent/GR3007485T3/el
unknown

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Publication number
Priority date
Publication date
Assignee
Title

AU7426387A
(en)

1986-06-16
1987-12-17
Frigoscandia Contracting A.B.
Process and apparatus for freezing liquid or semiliquid foods in the form of essentially uniform pellets

Also Published As

Publication number
Publication date

ES2038226T3
(en)

1993-07-16

JPH0740915B2
(en)

1995-05-10

EP0284837A3
(en)

1990-05-16

CA1307402C
(en)

1992-09-15

AU1404788A
(en)

1988-10-06

EP0284837B1
(en)

1992-12-30

CN1017969B
(en)

1992-08-26

CN88101711A
(en)

1988-11-02

FI881276A0
(en)

1988-03-17

JPS63263078A
(en)

1988-10-31

NO881025D0
(en)

1988-03-08

ATE84137T1
(en)

1993-01-15

NO168285B
(en)

1991-10-28

NZ224021A
(en)

1989-07-27

GR3007485T3
(en)

1993-07-30

NO881025L
(en)

1988-10-03

ZA882329B
(en)

1988-09-23

DE3711169C2
(en)

1989-11-16

TR25208A
(en)

1992-11-26

US4829783A
(en)

1989-05-16

DE3711169A1
(en)

1988-10-20

FI881276A
(en)

1988-10-03

EP0284837A2
(en)

1988-10-05

NO168285C
(en)

1992-02-05

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