EP1279745B1 - Process for batchwise preparation of big sugar crystals - Google Patents
Process for batchwise preparation of big sugar crystals Download PDFInfo
- Publication number
- EP1279745B1 EP1279745B1 EP02015121A EP02015121A EP1279745B1 EP 1279745 B1 EP1279745 B1 EP 1279745B1 EP 02015121 A EP02015121 A EP 02015121A EP 02015121 A EP02015121 A EP 02015121A EP 1279745 B1 EP1279745 B1 EP 1279745B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- crystals
- sugar
- sugar solution
- crystallization
- solution
- 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.)
- Expired - Lifetime
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C13—SUGAR INDUSTRY
- C13B—PRODUCTION OF SUCROSE; APPARATUS SPECIALLY ADAPTED THEREFOR
- C13B30/00—Crystallisation; Crystallising apparatus; Separating crystals from mother liquors ; Evaporating or boiling sugar juice
- C13B30/02—Crystallisation; Crystallising apparatus
-
- C—CHEMISTRY; METALLURGY
- C13—SUGAR INDUSTRY
- C13B—PRODUCTION OF SUCROSE; APPARATUS SPECIALLY ADAPTED THEREFOR
- C13B25/00—Evaporators or boiling pans specially adapted for sugar juices; Evaporating or boiling sugar juices
-
- C—CHEMISTRY; METALLURGY
- C13—SUGAR INDUSTRY
- C13B—PRODUCTION OF SUCROSE; APPARATUS SPECIALLY ADAPTED THEREFOR
- C13B30/00—Crystallisation; Crystallising apparatus; Separating crystals from mother liquors ; Evaporating or boiling sugar juice
- C13B30/02—Crystallisation; Crystallising apparatus
- C13B30/026—Discontinuous processes or apparatus therefor
-
- C—CHEMISTRY; METALLURGY
- C13—SUGAR INDUSTRY
- C13B—PRODUCTION OF SUCROSE; APPARATUS SPECIALLY ADAPTED THEREFOR
- C13B30/00—Crystallisation; Crystallising apparatus; Separating crystals from mother liquors ; Evaporating or boiling sugar juice
- C13B30/04—Separating crystals from mother liquor
- C13B30/12—Recycling mother liquor or wash liquors
-
- C—CHEMISTRY; METALLURGY
- C13—SUGAR INDUSTRY
- C13B—PRODUCTION OF SUCROSE; APPARATUS SPECIALLY ADAPTED THEREFOR
- C13B30/00—Crystallisation; Crystallising apparatus; Separating crystals from mother liquors ; Evaporating or boiling sugar juice
- C13B30/04—Separating crystals from mother liquor
- C13B30/14—Dissolving or refining raw sugar
Definitions
- the present invention is a process for the batch production of large sugar crystals with crystal sizes over 5 mm, preferably over 8 mm by evaporation crystallization in a crystallization vessel, wherein between the growing sugar crystals and the supersaturated sugar solution, a relative movement is produced, which suspended the growing sugar crystals holds using a device as defined in the claims for carrying out this method.
- Large sugar crystals over 5 mm, produced by special crystallization processes from concentrated, pure sugar solutions, are also called candy sugar.
- sugar candy with crystal sizes over 5 mm, preferably even over 8 mm is still used.
- Crystallization of sugar from supersaturated solutions produces, depending on the process conditions, more or less fine-grained products and, under certain other conditions, solid agglomerates of crystals of various sizes, which are mechanically coarsely granular. These products have the irregular shape of regrind and not the regular monklin sphenoidal form of sugar crystals, which is a sign of quality and purity to the consumer.
- a process for the production of stringent candy in which a continuously supersaturated hot sucrose solution circulated outside the crystallization vessel is recirculated is, are added during the crystallization process at constant temperature seed crystals in cocurrent or countercurrent.
- the sucrose crystals growing in the recycled sucrose solution are separated by sieving after reaching the desired crystal size. This method also leads to a relatively strong mechanical stress on the sugar crystals and thus not or only with very low yields to the desired large sugar crystals.
- the object of the invention is therefore to provide a process for producing large sugar crystals having crystal sizes of more than 5 mm, preferably more than 8 mm, in which a relative movement is produced by evaporation crystallization in a crystallization vessel between the growing sugar crystals and the supersaturated sugar solution which keeps the growing sugar crystals in suspension, however, further measures are taken to control the crystallization process so as to minimize nucleation disturbances so that the incorporated sugar crystals surely reach the size otherwise achievable only in poor yields.
- the crystallization vessel according to the invention has an overflow at the upper end into a collecting vessel with a larger diameter than the crystallization vessel, which already leads to a slowing down of the flow velocity. Through installations for flow calming, this leads to a sedimentation of newly formed fine grain, which can collect at the bottom of the collecting vessel and thus can no longer disturb the crystal growth of the large sugar crystals.
- This is preferably used to increase the rate of production by increasing the rate of upward flow of the sugar solution as the size of the growing sugar crystals increases.
- water In order to maintain the supersaturation in the solution as a driving force for the crystallization, water must be removed from the solution. In the process according to the invention, this is preferably done by evaporation under reduced pressure. The amount of heat consumed by the evaporation is supplied by appropriate heat in the sugar solution, with a small part is also available through the released heat of crystallization available.
- the process according to the invention is capable of producing large sugar crystals with high yields, with crystal sizes of up to 25 mm.
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Sustainable Development (AREA)
- Saccharide Compounds (AREA)
- Seasonings (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
Description
Gegenstand der vorliegenden Erfindung ist ein Verfahren zur chargenweisen Herstellung von großen Zuckerkristallen mit Kristallgrößen über 5 mm, vorzugsweise über 8 mm durch Verdampfungskristallisation in einem Kristallisationsbehälter, wobei zwischen den wachsenden Zuckerkristallen und der übersättigten Zuckerlösung eine Relativbewegung hergestellt wird, welche die wachsenden Zuckerkristalle in der Schwebe hält unter Verwendung einer Vorrichtung wie in den Ansprüchen definiert zur Durchführung dieses Verfahrens. Große Zuckerkristalle über 5 mm, durch spezielle Kristallisationsverfahren aus konzentrierten, reinen Zuckerlösungen hergestellt, werden auch Kandiszucker genannt.The present invention is a process for the batch production of large sugar crystals with crystal sizes over 5 mm, preferably over 8 mm by evaporation crystallization in a crystallization vessel, wherein between the growing sugar crystals and the supersaturated sugar solution, a relative movement is produced, which suspended the growing sugar crystals holds using a device as defined in the claims for carrying out this method. Large sugar crystals over 5 mm, produced by special crystallization processes from concentrated, pure sugar solutions, are also called candy sugar.
Bei besonderen Anwendungen des Zuckers kommt es darauf an, dass sich der Zucker langsam auflöst und sich erst langsam eine hohe Konzentration bzw. der süße Geschmack einstellt. Hierfür wird nach wie vor Kandiszucker mit Kristallgrößen über 5 mm, vorzugsweise sogar über 8 mm eingesetzt.In special applications of sugar, it is important that the sugar slowly dissolves and only slowly sets a high concentration or the sweet taste. For this purpose, sugar candy with crystal sizes over 5 mm, preferably even over 8 mm is still used.
Die Herstellungsverfahren für Zuckerkristalle mit Kristallgrößen über 5 mm, vorzugsweise über 8 mm, entwickelten sich aus der Kristallisation an Fäden, welche, in übersättigte Zuckerlösungen eingebracht, ein langsames und gleichmäßiges Wachsen der Zuckerkristalle ermöglichen. Die Fäden verbleiben dabei jedoch in den Zuckerkristallen, was von Verbrauchern als störend empfunden wird. Für Kandis ohne Fäden sind daher seit ca. 100 Jahren verschiedene Herstellungsverfahren entwickelt und eingesetzt worden; vgl.
Bei der Kristallisation von Zucker aus übersättigten Lösungen entstehen je nach Verfahrensbedingungen mehr oder weniger feinkörnige Produkte und unter gewissen anderen Bedingungen feste Agglomerate von Kristallen verschiedener Größe, die mechanisch aufgebrochen grobkörnig anfallen. Dieses Produkte haben die unregelmäßige Form von Mahlgut und nicht die regelmäßige monklin sphenoidale Form von Zuckerkristallen, die für den Verbraucher ein Zeichen von Qualität und Reinheit darstellt.Crystallization of sugar from supersaturated solutions produces, depending on the process conditions, more or less fine-grained products and, under certain other conditions, solid agglomerates of crystals of various sizes, which are mechanically coarsely granular. These products have the irregular shape of regrind and not the regular monklin sphenoidal form of sugar crystals, which is a sign of quality and purity to the consumer.
Aus der Patentliteratur der Jahre 1896 bis 1910 sind eine Reihe von mehr oder weniger aufwendigen und umständlichen Verfahren zur Herstellung von Kandis bekannt, d.h. grobkristallinem Zucker.
Da die spezifische Oberfläche der Kristalle (Fläche/Kristallmasse) mit zunehmendem Kristalldurchmesser abnimmt, nehmen die Schwierigkeiten der Steuerung der Kristallisation mit der Kristallgröße zu. Der Wasserentzug aus der Lösung, durch den die Übersättigung als Triebkraft der Kristallisation erzeugt wird, sollte nicht größer sein als die bei der gegebenen Kristalloberfläche mögliche Kristallisationsrate. Bei den bestehenden Verfahren wird das Gleichgewicht nicht eingehalten. Dadurch entstehen unerwünschte Kristallkeime, die die Ausbeute an großen Kristallen verringern und deren Qualität mindern.As the specific surface area of crystals (area / crystal mass) decreases with increasing crystal diameter, the difficulty of controlling crystallization increases with crystal size. The removal of water from the solution, by which the supersaturation is generated as a driving force of crystallization, should not be greater than the possible crystallization rate at the given crystal surface. The existing procedures do not maintain equilibrium. This results in unwanted crystal nuclei, which reduce the yield of large crystals and reduce their quality.
Weiterhin ist das Verfahren nach Wulf und Bock bekannt, bei dem eine längere, flache Wanne mit Impfkristallen in schaukelnder Bewegung gehalten wird. Die Ausbeute beträgt aber nur 18 bis 20 % der eingebrachten Zuckermenge; vgl.
Aus der
Auch das Verfahren gemäß
Die Erfindung hat sich somit die Aufgabe gestellt, ein Verfahren zur Herstellung von großen Zuckerkristallen mit Kristallgrößen über 5 mm, vorzugsweise über 8 mm zur Verfügung zu stellen, bei dem durch Verdampfungskristallisation in einem Kristallisationsbehälter zwischen den wachsenden Zuckerkristallen und der übersättigten Zuckerlösung eine Relativbewegung hergestellt wird, welche die wachsenden Zuckerkristalle in der Schwebe hält, jedoch durch weitere Maßnahmen dafür gesorgt wird, dass der Kristallisationsprozess so gesteuert wird, dass Störungen durch Keimbildung minimiert werden, damit die eingebrachten Zuckerkristalle sicher die Größe erreichen, die sonst nur in schlechten Ausbeuten erreichbar war.The object of the invention is therefore to provide a process for producing large sugar crystals having crystal sizes of more than 5 mm, preferably more than 8 mm, in which a relative movement is produced by evaporation crystallization in a crystallization vessel between the growing sugar crystals and the supersaturated sugar solution which keeps the growing sugar crystals in suspension, however, further measures are taken to control the crystallization process so as to minimize nucleation disturbances so that the incorporated sugar crystals surely reach the size otherwise achievable only in poor yields.
Die Aufgabe wird jetzt dadurch gelöst, dass die Relativbewegung hergestellt wird ohne mechanisch bewegte Teile im Kristallisationsbehälter durch einen aufwärtsgerichteten Strom der Zuckerlösung, welcher die wachsenden Zuckerkristalle in der Schwebe hält, wobei die durch Verdampfung aus dem System abgeführte Wassermenge gesteuert wird durch die Wärmezufuhr in die Zuckerlösung und die Wärmezufuhr so gesteuert wird, dass die Übersättigung der Zuckerlösung erhalten bleibt unter Verwendung einer Vorrichtung bestehend aus
- a) einem senkrecht stehenden Kristallisationsbehälter mit
- b) einer unteren Zuführung für die übersättigte Zuckerlösung,
- c) einem beheizbaren Siebboden,
- d) einem Überlauf in ein Auffanggefäß mit größerem Durchmesser als der Kristallisationsbehälter, welcher Einbauten zur Strömungsberuhigung aufweist,
- e) einer Rückführleitung mit Pumpe für die Zuckerlösung vom Auffanggefäß zur unteren Zuführung des Kristallisationsbehälters,
- f) einer Abführung im oberen Teil des Auffanggefäßes für Wasserdampf
- g) einer Zuführöffnung im oberen Teil des Auffanggefäßes für Impfkristalle
- h) eine Entleerungsöffnung oberhalb des Siebbodens für die fertigen Zuckerkristalle
- i) Mess- und Steuerungseinrichtungen für Temperatur, Wärmezufuhr und Fließgeschwindigkeit der Zuckerlösung.
- a) a vertical crystallization vessel with
- b) a lower feed for the supersaturated sugar solution,
- c) a heated sieve tray,
- d) an overflow into a collecting vessel with a larger diameter than the crystallization vessel, which has internals for flow calming,
- e) a return line with pump for the sugar solution from the collecting vessel to the lower feed of the crystallization tank,
- f) a discharge in the upper part of the collecting vessel for water vapor
- g) a feed opening in the upper part of the collecting vessel for seed crystals
- h) an emptying opening above the sieve bottom for the finished sugar crystals
- i) measuring and control devices for temperature, heat input and flow rate of the sugar solution.
Der erfindungsgemäße Kristallisationsbehälter weist am oberen Ende einen Überlauf auf in ein Auffanggefäß mit einem größeren Durchmesser als der Kristallisationsbehälter, was bereits zu einer Verlangsamung der Strömungsgeschwindigkeit führt. Durch Einbauten zur Strömungsberuhigung führt dies zu einer Sedimentation von neugebildetem Feinkorn, welches sich am Boden des Auffanggefäßes sammeln kann und somit nicht mehr das Kristallwachstum der großen Zuckerkristalle stören kann.The crystallization vessel according to the invention has an overflow at the upper end into a collecting vessel with a larger diameter than the crystallization vessel, which already leads to a slowing down of the flow velocity. Through installations for flow calming, this leads to a sedimentation of newly formed fine grain, which can collect at the bottom of the collecting vessel and thus can no longer disturb the crystal growth of the large sugar crystals.
Durch Messung der Temperatur, der Wärmezufuhr und der Fließgeschwindigkeit der Zuckerlösung ist es möglich, das gesamte System so zu steuern, dass in möglichst kurzer Zeit ungestört große Zuckerkristalle mit Kristallgrößen über 5 mm und auch deutlich über 8 mm entstehen können, so dass Kristallgrößen zur Verfügung gestellt werden, die sonst nur in schlechten Ausbeuten erzielt werden konnten.By measuring the temperature, the heat input and the flow rate of the sugar solution, it is possible to control the entire system in such a short time undisturbed large sugar crystals with crystal sizes over 5 mm and well over 8 mm may arise, so that crystal sizes available be made, which otherwise could only be achieved in poor yields.
Vorzugsweise wird dabei dafür gesorgt, dass in der Zuckerlösung neugebildetes Feinkorn abgetrennt wird und somit nicht das weitere Wachstum der großen Zuckerkristalle stören kann.Preferably, it is ensured that newly formed fine grain is separated in the sugar solution and thus can not interfere with the further growth of the large sugar crystals.
Da die Oberfläche der wachsenden Zuckerkristalle zunehmend größer wird, wächst auch die Menge des aus der Lösung entfernten Zuckers. Dies wird vorzugsweise dazu ausgenutzt, die Produktionsgeschwindigkeit zu erhöhen, indem die Geschwindigkeit des aufwärtsgerichteten Stromes der Zuckerlösung mit zunehmender Größe der wachsenden Zuckerkristalle erhöht wird.As the surface of the growing sugar crystals becomes increasingly larger, so does the amount of sugar removed from the solution. This is preferably used to increase the rate of production by increasing the rate of upward flow of the sugar solution as the size of the growing sugar crystals increases.
Um die Übersättigung in der Lösung als Triebkraft für die Kristallisation aufrecht zu erhalten, muss Wasser aus der Lösung entfernt werden. Vorzugsweise erfolgt dies beim erfindungsgemäßen Verfahren durch Verdampfung bei Unterdruck. Die durch die Verdampfung verbrauchte Wärmemenge wird durch entsprechende Wärmezufuhr in die Zuckerlösung geliefert, wobei ein geringer Teil auch durch die freiwerdende Kristallisationswärme zur Verfügung steht. Das erfindungsgemäße Verfahren ist in der Lage, mit hoher Ausbeute große Zuckerkristalle zu liefern mit Kristallgrößen bis 25 mm.In order to maintain the supersaturation in the solution as a driving force for the crystallization, water must be removed from the solution. In the process according to the invention, this is preferably done by evaporation under reduced pressure. The amount of heat consumed by the evaporation is supplied by appropriate heat in the sugar solution, with a small part is also available through the released heat of crystallization available. The process according to the invention is capable of producing large sugar crystals with high yields, with crystal sizes of up to 25 mm.
Claims (4)
- A process for the discontinuous preparation of large sugar crystals with crystal sizes of above 5 mm, preferably above 8 mm, by evaporation crystallization in a crystallization tank, wherein a relative motion is created between the growing sugar crystals and the supersaturated sugar solution, keeping the growing sugar crystals floating, characterized in that said relative motion is created without mechanically moving parts in the crystallization tank, by an upward stream of the sugar solution, wherein the amount of water removed from the system by evaporation is controlled by the heat supply into the sugar solution, and the heat supply is controlled to maintain the supersaturation of the sugar solution using a device consisting of:a) a vertically oriented crystallization tank comprisingb) a lower inlet for the supersaturated sugar solution,c) a heatable perforated base,d) a level drain leading into a collector vessel having a larger diameter than that of the crystallization tank and having built-in structures for calming the flow,e) a return line with a pump for the sugar solution leading from the collector vessel to the lower inlet of the crystallization tank;f) an exhaust for water vapor in the upper part of the collector vessel,g) an inlet for seed crystals in the upper part of the collector vessel,h) a discharge opening above the perforated base for the finished sugar crystals,i) measuring and controlling means for temperature, heat supply and flow rate of the sugar solution.
- The process according to claim 1, characterized in that newly formed fine grains are separated from the stream of said supersaturated sugar solution.
- The process according to claim 1 or 2, characterized in that the velocity of the upward stream of the sugar solution is increased as the size of the growing sugar crystals increases.
- The process according to any of claims 1 to 3, characterized in that the evaporation of the water is effected under reduced pressure.
Applications Claiming Priority (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE10135079 | 2001-07-19 | ||
DE2001135079 DE10135079C2 (en) | 2001-07-19 | 2001-07-19 | Process for the batchwise production of sugar crystals without threads and device for carrying them out |
DE10142027 | 2001-08-28 | ||
DE10142027 | 2001-08-28 |
Publications (2)
Publication Number | Publication Date |
---|---|
EP1279745A1 EP1279745A1 (en) | 2003-01-29 |
EP1279745B1 true EP1279745B1 (en) | 2010-06-23 |
Family
ID=26009730
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP02015121A Expired - Lifetime EP1279745B1 (en) | 2001-07-19 | 2002-07-06 | Process for batchwise preparation of big sugar crystals |
Country Status (7)
Country | Link |
---|---|
EP (1) | EP1279745B1 (en) |
AT (1) | ATE471992T1 (en) |
DE (1) | DE50214497D1 (en) |
DK (1) | DK1279745T3 (en) |
ES (1) | ES2347530T3 (en) |
HU (1) | HUP0202375A3 (en) |
PL (1) | PL208331B1 (en) |
Families Citing this family (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE102007020671A1 (en) * | 2007-05-01 | 2008-11-06 | Justus-Liebig-Universität Giessen | Growth of inorganic, organic, bioorganic or biological object e.g. tissue or embryos from saturated/supersaturated nutrient solution, comprises flowing growth object in flow direction of the solution and then regulating the flow direction |
Family Cites Families (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
FR838690A (en) * | 1937-11-25 | 1939-03-13 | Quint & Flamant Reunis Ets | Process for the crystallization of sweet liquors or others |
DE1172200B (en) * | 1963-02-28 | 1964-06-11 | Tintelnot Geb | Process and device for the production of rock candy in the form of crystal conglomerates |
CH447980A (en) * | 1964-06-05 | 1967-11-30 | Soc D Raffineries De Sucre De | Apparatus for the regulation of sucrose crystallization |
US4004886A (en) * | 1969-12-12 | 1977-01-25 | Stamicarbon B.V. | Two stage continuous process and apparatus for crystallization |
DE3420001A1 (en) * | 1984-05-29 | 1985-12-05 | Pfeifer & Langen, 5000 Köln | METHOD FOR REGULATING THE VACUUM COOKING PROCESS FOR PRODUCING CRYSTALLINE SUGAR |
DD294731A5 (en) * | 1990-05-25 | 1991-10-10 | Institut Fuer Forschung Und Rationalisierung Der Zuckerindustrie,De | METHOD FOR PRODUCING THINNESS KANDIS |
FR2669510B1 (en) * | 1990-11-22 | 1993-01-22 | Fcb | DISCONTINUOUS PROCESS FOR CRYSTALIZING A SYRUP AND APPARATUS FOR CARRYING OUT SAID METHOD. |
-
2002
- 2002-07-06 AT AT02015121T patent/ATE471992T1/en active
- 2002-07-06 EP EP02015121A patent/EP1279745B1/en not_active Expired - Lifetime
- 2002-07-06 ES ES02015121T patent/ES2347530T3/en not_active Expired - Lifetime
- 2002-07-06 DE DE50214497T patent/DE50214497D1/en not_active Expired - Lifetime
- 2002-07-06 DK DK02015121.3T patent/DK1279745T3/en active
- 2002-07-11 PL PL355007A patent/PL208331B1/en unknown
- 2002-07-18 HU HU0202375A patent/HUP0202375A3/en not_active Application Discontinuation
Also Published As
Publication number | Publication date |
---|---|
HUP0202375A3 (en) | 2003-09-29 |
PL208331B1 (en) | 2011-04-29 |
DK1279745T3 (en) | 2010-10-18 |
DE50214497D1 (en) | 2010-08-05 |
HUP0202375A2 (en) | 2003-08-28 |
ATE471992T1 (en) | 2010-07-15 |
ES2347530T3 (en) | 2010-11-02 |
EP1279745A1 (en) | 2003-01-29 |
HU0202375D0 (en) | 2002-10-28 |
PL355007A1 (en) | 2003-01-27 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
DE60028806T2 (en) | CRYSTALLIZATION OF MATERIALS FROM WATER SOLUTIONS | |
EP1286737B1 (en) | Device for producing crystals | |
DE10242746B4 (en) | Washing device, a process for cleaning a laundry and the use of the washing device | |
DE2406663B2 (en) | Process for the production of anhydrous fructose crystals | |
EP3408415B1 (en) | Method for obtaining crystals from a mother solution, and crystallization device suitable for this purpose | |
DE102009014668A1 (en) | Crystallization apparatus and method for molten fats | |
DE3001644C2 (en) | Process for the precipitation of Al (OH)? 3? from a supersaturated raw liquor | |
EP1279745B1 (en) | Process for batchwise preparation of big sugar crystals | |
WO2000056416A1 (en) | Method for controlling crystal size during continuous mass crystallisation | |
CH373054A (en) | Process for the optical resolution of racemic mixtures of glutamic acid, glutamic acid hydrohalides or glutamates | |
DE3934341C2 (en) | Process for the crystallization of fructose | |
DE3412752C2 (en) | ||
WO2020114850A1 (en) | Continuous method for obtaining a crystalline monosaccharide and device for continuous crystallization | |
JPH07630B2 (en) | Method and apparatus for producing crystalline multi-tool | |
DE10135079C2 (en) | Process for the batchwise production of sugar crystals without threads and device for carrying them out | |
WO2022219094A1 (en) | Process for producing 1,1-gpm- and/or 1,6-gps-enriched isomalt compositions | |
DE1150397B (en) | Process and device for the continuous crystallization and recovery of calcium nitrate tetrahydrate from solutions of raw phosphates digested with nitric acid | |
Atwood et al. | Continuous sugar crystallization: a chemical engineer’s viewpoint | |
DE60023232T2 (en) | Crystallization of alpha-L-aspartyl-L-phenylalanine methyl ester from supersaturated solutions | |
DE112019001119T5 (en) | Evaporation crystallization device | |
DE69909048T2 (en) | Process for the production of raffinose crystals | |
DE3831305C2 (en) | ||
EP2419187B1 (en) | Process for continuously treating a solution containing a salt | |
EP0436763A1 (en) | Process for continuously producing a crystal magma | |
DE69827141T2 (en) | METHOD FOR REFINING CRYSTALLINE MATERIAL |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PUAI | Public reference made under article 153(3) epc to a published international application that has entered the european phase |
Free format text: ORIGINAL CODE: 0009012 |
|
AK | Designated contracting states |
Designated state(s): AT BE BG CH CY CZ DE DK EE ES FI FR GB GR IE IT LI LU MC NL PT SE SK TR |
|
AX | Request for extension of the european patent |
Extension state: AL LT LV MK RO SI |
|
17P | Request for examination filed |
Effective date: 20030725 |
|
AKX | Designation fees paid |
Designated state(s): AT BE BG CH CY CZ DE DK EE ES FI FR GB GR IE IT LI LU MC NL PT SE SK TR |
|
AXX | Extension fees paid |
Extension state: SI Payment date: 20030725 Extension state: RO Payment date: 20030725 |
|
17Q | First examination report despatched |
Effective date: 20041029 |
|
GRAP | Despatch of communication of intention to grant a patent |
Free format text: ORIGINAL CODE: EPIDOSNIGR1 |
|
RTI1 | Title (correction) |
Free format text: PROCESS FOR BATCHWISE PREPARATION OF BIG SUGAR CRYSTALS |
|
GRAS | Grant fee paid |
Free format text: ORIGINAL CODE: EPIDOSNIGR3 |
|
GRAA | (expected) grant |
Free format text: ORIGINAL CODE: 0009210 |
|
AK | Designated contracting states |
Kind code of ref document: B1 Designated state(s): AT BE BG CH CY CZ DE DK EE ES FI FR GB GR IE IT LI LU MC NL PT SE SK TR |
|
AX | Request for extension of the european patent |
Extension state: RO SI |
|
REG | Reference to a national code |
Ref country code: CH Ref legal event code: EP |
|
REG | Reference to a national code |
Ref country code: IE Ref legal event code: FG4D Free format text: LANGUAGE OF EP DOCUMENT: GERMAN |
|
REG | Reference to a national code |
Ref country code: CH Ref legal event code: NV Representative=s name: SCHMAUDER & PARTNER AG PATENT- UND MARKENANWAELTE |
|
REF | Corresponds to: |
Ref document number: 50214497 Country of ref document: DE Date of ref document: 20100805 Kind code of ref document: P |
|
REG | Reference to a national code |
Ref country code: NL Ref legal event code: T3 |
|
REG | Reference to a national code |
Ref country code: SE Ref legal event code: TRGR |
|
REG | Reference to a national code |
Ref country code: DK Ref legal event code: T3 |
|
REG | Reference to a national code |
Ref country code: ES Ref legal event code: FG2A Ref document number: 2347530 Country of ref document: ES Kind code of ref document: T3 |
|
REG | Reference to a national code |
Ref country code: SK Ref legal event code: T3 Ref document number: E 7670 Country of ref document: SK |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: GR Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20100924 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: EE Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20100623 |
|
REG | Reference to a national code |
Ref country code: IE Ref legal event code: FD4D |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: CY Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20100623 Ref country code: MC Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20100731 Ref country code: PT Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20101025 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: IE Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20100623 |
|
PLBE | No opposition filed within time limit |
Free format text: ORIGINAL CODE: 0009261 |
|
STAA | Information on the status of an ep patent application or granted ep patent |
Free format text: STATUS: NO OPPOSITION FILED WITHIN TIME LIMIT |
|
26N | No opposition filed |
Effective date: 20110324 |
|
REG | Reference to a national code |
Ref country code: DE Ref legal event code: R097 Ref document number: 50214497 Country of ref document: DE Effective date: 20110323 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: LU Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20100706 Ref country code: BG Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20100623 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: BG Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20100923 |
|
PGFP | Annual fee paid to national office [announced via postgrant information from national office to epo] |
Ref country code: SK Payment date: 20140630 Year of fee payment: 13 Ref country code: CZ Payment date: 20140624 Year of fee payment: 13 Ref country code: TR Payment date: 20140626 Year of fee payment: 13 |
|
PGFP | Annual fee paid to national office [announced via postgrant information from national office to epo] |
Ref country code: FI Payment date: 20140721 Year of fee payment: 13 Ref country code: CH Payment date: 20140722 Year of fee payment: 13 |
|
PGFP | Annual fee paid to national office [announced via postgrant information from national office to epo] |
Ref country code: ES Payment date: 20140721 Year of fee payment: 13 |
|
PGFP | Annual fee paid to national office [announced via postgrant information from national office to epo] |
Ref country code: IT Payment date: 20140728 Year of fee payment: 13 |
|
REG | Reference to a national code |
Ref country code: FR Ref legal event code: PLFP Year of fee payment: 14 |
|
REG | Reference to a national code |
Ref country code: CH Ref legal event code: PL |
|
REG | Reference to a national code |
Ref country code: SK Ref legal event code: MM4A Ref document number: E 7670 Country of ref document: SK Effective date: 20150706 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: LI Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20150731 Ref country code: IT Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20150706 Ref country code: CH Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20150731 Ref country code: SK Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20150706 Ref country code: CZ Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20150706 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: FI Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20150706 |
|
REG | Reference to a national code |
Ref country code: FR Ref legal event code: PLFP Year of fee payment: 15 |
|
REG | Reference to a national code |
Ref country code: ES Ref legal event code: FD2A Effective date: 20160826 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: ES Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20150707 |
|
REG | Reference to a national code |
Ref country code: FR Ref legal event code: PLFP Year of fee payment: 16 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: TR Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20150706 |
|
REG | Reference to a national code |
Ref country code: FR Ref legal event code: PLFP Year of fee payment: 17 |
|
PGFP | Annual fee paid to national office [announced via postgrant information from national office to epo] |
Ref country code: NL Payment date: 20200728 Year of fee payment: 19 |
|
PGFP | Annual fee paid to national office [announced via postgrant information from national office to epo] |
Ref country code: DE Payment date: 20200803 Year of fee payment: 19 Ref country code: DK Payment date: 20200723 Year of fee payment: 19 Ref country code: GB Payment date: 20200728 Year of fee payment: 19 Ref country code: FR Payment date: 20200722 Year of fee payment: 19 |
|
PGFP | Annual fee paid to national office [announced via postgrant information from national office to epo] |
Ref country code: AT Payment date: 20200721 Year of fee payment: 19 Ref country code: BE Payment date: 20200722 Year of fee payment: 19 Ref country code: SE Payment date: 20200728 Year of fee payment: 19 |
|
REG | Reference to a national code |
Ref country code: DE Ref legal event code: R119 Ref document number: 50214497 Country of ref document: DE |
|
REG | Reference to a national code |
Ref country code: DK Ref legal event code: EBP Effective date: 20210731 |
|
REG | Reference to a national code |
Ref country code: NL Ref legal event code: MM Effective date: 20210801 |
|
REG | Reference to a national code |
Ref country code: AT Ref legal event code: MM01 Ref document number: 471992 Country of ref document: AT Kind code of ref document: T Effective date: 20210706 |
|
GBPC | Gb: european patent ceased through non-payment of renewal fee |
Effective date: 20210706 |
|
REG | Reference to a national code |
Ref country code: BE Ref legal event code: MM Effective date: 20210731 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: GB Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20210706 Ref country code: DE Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20220201 Ref country code: AT Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20210706 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: SE Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20210707 Ref country code: NL Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20210801 Ref country code: FR Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20210731 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: DK Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20210731 Ref country code: BE Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20210731 |