EP1005888B1 - Rinsing system for removing residues - Google Patents
Rinsing system for removing residues Download PDFInfo
- Publication number
- EP1005888B1 EP1005888B1 EP99123942A EP99123942A EP1005888B1 EP 1005888 B1 EP1005888 B1 EP 1005888B1 EP 99123942 A EP99123942 A EP 99123942A EP 99123942 A EP99123942 A EP 99123942A EP 1005888 B1 EP1005888 B1 EP 1005888B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- outflow
- line
- vessel
- valve
- cleaning
- 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
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B9/00—Cleaning hollow articles by methods or apparatus specially adapted thereto
- B08B9/08—Cleaning containers, e.g. tanks
Definitions
- the invention relates to a flushing device for the removal of residues the sump drain of an evaporator and their use for the Distillative workup of saline solutions.
- Thin-film evaporation is used for continuous distillation, in particular for Evaporation of temperature-sensitive substances from high-boiling Residues, and for the concentration of temperature-labile substances used.
- the liquid is distributed by trickling (falling film evaporator), Influence of centrifugal force (special embodiment of a Rotary evaporator), specially designed wipers (Filmtruder) or others Techniques for thin layers (order of magnitude of the layer thickness usually approx. 0.1 mm) on the (usually) heated surfaces. thin Liquid layers allow rapid evaporation, so that the contained components only briefly the (usually) higher Temperatures are exposed in the evaporator.
- a typical thin-film evaporator has a vertical, from the outside heated tube on the inner surface of the product to be evaporated from a rotor is spread as a thin layer.
- the product occurs above the Heating zone in the evaporator and flows due to the mechanical distribution through the rotor as a liquid film over the heating surface.
- the low-boiling Components evaporate as the residue runs down.
- the Brüdendämpfe flow through a mist eliminator located in the head of the Evaporator is and will be in a separately arranged condenser condensed.
- For the mechanical fluid distribution is a rotor with fitted swinging suspended wiper blades made of metal. During operation the wiper blades are due to the centrifugal force against the evaporator wall pressed, resulting in even product distribution and intensive Fluid mixing of the liquid film causes.
- the dissolved residues for example, dissolved salts
- the dissolved residues include: The cause can be found in the fact that these residues are deposited in the sump. These are residues, which are usually before evaporation as dissolved components in the liquid and after evaporation of solvent as a solid.
- the evaporation salt solutions, with salt, after evaporation of Solvent, as a solid residue in the bottom of the evaporator accrues.
- soluble residues can in principle all Be solids that are removed with a dishwashing liquid - usually in one Solvent can be solved.
- the thin film evaporator described in the introduction is not only the complete Evaporation of vaporizable components from a residue - - Example, to ensure saline - solution, but also the residues as one provide pumpable mass from the sump.
- a Thin-film evaporator which operates on the principle described above, is this is not the case; because residues, such as salts, may be in the range Depositing the sump drain and form incrustations, so that the sump discharge due to blockages can not be easily removed.
- the Swamp drain is usually the tapered part - usually going down to a pipe tapering part - of the swamp, through which the sump product at discharge is passed through the evaporation apparatus.
- the continuous operation of the Thin film evaporation must be adjusted when such blockages occur so that appropriate cleaning work can be initiated. Also at the Use of other evaporation equipment, such as distillation columns, occur often the same problems.
- the object of the present invention was to provide a device with the dissolved residues containing liquids in an evaporator can be separated without the bottom outlet of the evaporation device clogged by the residues. There should be no cleaning necessary be that would interrupt a continuous evaporation. Both the bottoms product as well as the top product of the corresponding evaporation process be preserved in the gentlest possible way.
- the device should be effective and inexpensive work.
- the drainage container is via connecting lines directly with the drain valve, the flushing water valve, the tank drain valve, the purge valve and the vent valve connected.
- the drain tank is usually above the sump and below the Swamp arranged.
- the Spülablauf founded can open into the sump drain line, so that the drain line device a common outlet for detergent and bottom product having.
- the drain conduit means in the form of two lines, a Spülablauf für and a sump drain line, formed so that Sump and detergent separated, discharged through various outputs.
- Injecting gas for example nitrogen
- the ingress of air (and thus also of oxygen) in the apparatus to prevent In this way can be located in the top product or bottom product, oxidation-sensitive Protecting substances.
- the collecting container is preferably connected to a pump. With this can the contents of the collecting container are circulated so that it remains homogeneous and the deposition of residues is avoided.
- the evaporation device is a thin film evaporator.
- the flushing device according to the invention is especially for the distillative Working up saline solutions used. These are usually to solutions, in addition to the dissolved salts still value products (often oxidation-sensitive value products). Most are more Work-up steps necessary to obtain pure value products.
- the bottom outlet of the evaporation apparatus is using the inventive Rinsing device periodically rinsed.
- a rinsing agent is used, in the residues are dissolved.
- the flushing device according to the invention Accordingly, it is preferred to remove soluble residues. It can, however Also, mechanical rinsing effects to be effective because the detergent with a certain Speed can hit the corresponding residues. It is thus Not absolutely necessary that the residues completely soluble in the detergent are.
- the sump discharge of the evaporation apparatus can after rinsing and mixing with the detergent (water) pumped out and stored.
- the detergent water
- the resulting mixture can this burned, for example, in a residue combustion, in a biological wastewater treatment plant disposed of or (if value added products are still included) be further worked up.
- the operation of the device according to the invention is based on a preferred embodiment, the example of a salt-depositing Thin-film evaporator, are described.
- FIG. 1 is a thin film evaporator with an inventive Flushing device shown.
- This flushing device has drainage means (6, 16), in the form of two lines, a Spülablauf für (6) and a sump drain line (16) are formed.
- the bottom product is first in a drain tank 7, which gradually fills up. After reaching a certain Level, the drain valve 10 is closed and the vacuum in the drain tank 7 lifted by opening the container drain valve 12 to the sump 8 (The collection 8 is under normal pressure or slight overpressure). Subsequently the vent valve 14 is opened, and the contents of the drain container. 7 runs into the collecting container 8.
- the content of the collecting container 8 is expediently circulated by means of a pump 9 in order to keep it homogeneous and possible Prevent salt deposition.
- the content becomes temporary storage and more Recycling, for example, combustion, continuously or discontinuously dissipated.
- the drain tank 7 is rinsed. It is expedient to use water, prefers warm water or steam condensate.
- the container drain valve 12 are closed, the purge valve 13 and the Rinse water valve 11 is opened.
- the warm rinse water flowing through the inlet pipe for Rinsing agent 3 is supplied, now flows through the drain tank 7 and removed this way salt deposits.
- the rinsing process can (depending on the ingredients contained) For example, be fed to a biological treatment plant. Rinse duration and water flow are adjusted as needed so that the required amount of water so low as necessary. As a rule (depending on the load of the evaporator and salinity) a rinse time of 1 to 2 minutes is sufficient.
- this line is opened by opening the Container drain valve 12 (instead of Spülablaufventils 13) periodically flushed. Preferably this is done every 10 to 20 flush cycles.
- the Spülablaufventil 13 After expiration of a pre-purging the Spülablaufventil 13 is closed, and in the course of the rinsing phase, the water is flushed through the drain tank 7 and the drain line through the vent line and through the vent valve 14. Subsequently, the rinse water valve 11 is closed and to empty the drain tank, the purge valve 13 is opened. Remaining rinse water is allowed to drain by opening the container drain valve 12. Thereafter, all valves are closed again. By opening the drain valve 10, the drain tank is evacuated again and the drain cycle can begin again.
- the drain lines are to the sump and for flushing with inert gas flushes (usually nitrogen flushing) Mistake.
- inert gas flushes usually nitrogen flushing
- FIG. 1 opens between the run-up tank 7 and the drain valve 10, a first Inlet pipe 5 for introducing inert gas into the conduit 17 for transferring the Bottoms.
- the collecting container 8 is connected to the drain container 7 via a line, which is provided with the container drain valve 12 and into which a second inlet pipe 4 opens for the introduction of inert gas.
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
- Cleaning By Liquid Or Steam (AREA)
- Cleaning In General (AREA)
- Pipeline Systems (AREA)
- Heat Treatment Of Water, Waste Water Or Sewage (AREA)
- Apparatuses And Processes For Manufacturing Resistors (AREA)
- Silver Salt Photography Or Processing Solution Therefor (AREA)
- Cleaning Or Drying Semiconductors (AREA)
Abstract
Description
Die Erfindung betrifft eine Spülvorrichtung zur Entfernung von Rückständen aus dem Sumpfablauf einer Verdampfungsvorrichtung und ihre Verwendung für die destillative Aufarbeitung salzhaltiger Lösungen.The invention relates to a flushing device for the removal of residues the sump drain of an evaporator and their use for the Distillative workup of saline solutions.
Dünnschichtverdampfung wird für kontinuierliche Destillation, insbesondere zur Verdampfung temperaturempfindlicher Substanzen aus hochsiedenden Rückständen, und für die Aufkonzentration von temperaturlabilen Stoffen eingesetzt. Hierbei verteilt man die Flüssigkeit durch Abrieselnlassen (FallfilmVerdampfer), Einwirkung von Zentrifugalkraft (spezielle Ausführungsform eines Rotationsverdampfers), besonders konstruierte Wischer (Filmtruder) oder anderen Techniken zu dünnen Schichten (Größenordnung der Schichtdicke in der Regel ca. 0,1 mm) auf den (in der Regel) beheizten Flächen. Dünne Flüssigkeitsschichten ermöglichen eine schnelle Verdampfung, so daß die enthaltenen Komponenten nur kurzzeitig den (in der Regel) höheren Temperaturen im Verdampfer ausgesetzt sind. Die Verweilzeit, die Temperatur und der Druck (Vakuum) werden entsprechend der jeweiligen Trennaufgabe ausgelegt. Dabei sind zur Schonung der betreffenden Substanzen möglichst niedrige Temperaturen und kurze Verweilzeiten zu bevorzugen. Neben Verdampfungsvorrichtungen, die im allgemeinen technischen Sprachgebrauch bereits als Dünnschichtverdampfer bezeichnet werden, werden erfindungsgemäß auch alle anderen Verdampfungsvorrichtungen als Dünnschichtverdampfer verstanden, die nach dem vorstehend beschriebenen Prinzip arbeiten. Thin-film evaporation is used for continuous distillation, in particular for Evaporation of temperature-sensitive substances from high-boiling Residues, and for the concentration of temperature-labile substances used. In this case, the liquid is distributed by trickling (falling film evaporator), Influence of centrifugal force (special embodiment of a Rotary evaporator), specially designed wipers (Filmtruder) or others Techniques for thin layers (order of magnitude of the layer thickness usually approx. 0.1 mm) on the (usually) heated surfaces. thin Liquid layers allow rapid evaporation, so that the contained components only briefly the (usually) higher Temperatures are exposed in the evaporator. The residence time, the temperature and the pressure (vacuum) corresponding to the respective separation task designed. It is as possible to protect the substances concerned to favor low temperatures and short residence times. Next Evaporation devices, in general technical usage already be referred to as thin-film evaporator, according to the invention also all other evaporation devices as a thin-film evaporator understood that operate on the principle described above.
Ein typischer Dünnschichtverdampfer weist ein senkrecht stehendes, von außen beheiztes Rohr auf, auf dessen Innenfläche das zu verdampfende Produkt von einem Rotor als dünne Schicht ausgebreitet wird. Das Produkt tritt oberhalb der Heizzone in den Verdampfer ein und fließt infolge der mechanischen Verteilung durch den Rotor als Flüssigkeitsfilm über die Heizfläche. Die leichtsiedenden Komponenten verdampfen, während der Rückstand nach unten abläuft. Die Brüdendämpfe strömen durch einen Tropfenabscheider, der sich im Kopf des Verdampfers befindet und werden in einem separat angeordneten Kondensator kondensiert. Für die mechanische Flüssigkeitsverteilung ist ein Rotor mit pendelnd aufgehängten Wischerblättern aus Metall eingebaut. Beim Betrieb werden die Wischerblätter infolge der Fliehkraft gegen die Verdampferwand gedrückt, was eine gleichmäßige Produktverteilung und eine intensive Flüssigkeitsdurchmischung des Flüssigkeitsfilmes bewirkt.A typical thin-film evaporator has a vertical, from the outside heated tube on the inner surface of the product to be evaporated from a rotor is spread as a thin layer. The product occurs above the Heating zone in the evaporator and flows due to the mechanical distribution through the rotor as a liquid film over the heating surface. The low-boiling Components evaporate as the residue runs down. The Brüdendämpfe flow through a mist eliminator located in the head of the Evaporator is and will be in a separately arranged condenser condensed. For the mechanical fluid distribution is a rotor with fitted swinging suspended wiper blades made of metal. During operation the wiper blades are due to the centrifugal force against the evaporator wall pressed, resulting in even product distribution and intensive Fluid mixing of the liquid film causes.
Ein besonderes Problem tritt jedoch häufig dann auf, wenn Flüssigkeiten verdampft werden, die gelöste Rückstände, zum Beispiel gelöste Salze, enthalten: Die Ursache ist darin zu finden, daß sich diese Rückstände im Sumpf abscheiden. Dabei handelt es sich um Rückstände, die in der Regel vor der Verdampfung als gelöste Komponenten in der Flüssigkeit vorlagen und sich nach der Verdampfung von Lösungsmittel als Feststoff abscheiden. Als Beispiel kann die Verdampfung von Salzlösungen angeführt werden, wobei Salz, nach der Verdampfung von Lösungsmittel, als fester Rückstand im Sumpf des Verdampfungsapparates anfällt. Neben solchen Salzen können lösliche Rückstände prinzipiell alle Feststoffe sein, die mit einem Spülmittel entfernt - in der Regel in einem Lösungsmittel gelöst - werden können.However, a particular problem often occurs when liquids evaporated, the dissolved residues, for example, dissolved salts, include: The cause can be found in the fact that these residues are deposited in the sump. These are residues, which are usually before evaporation as dissolved components in the liquid and after evaporation of solvent as a solid. As an example, the evaporation salt solutions, with salt, after evaporation of Solvent, as a solid residue in the bottom of the evaporator accrues. In addition to such salts, soluble residues can in principle all Be solids that are removed with a dishwashing liquid - usually in one Solvent can be solved.
Der einleitend beschriebene Dünnschichtverdampfer soll nicht nur die vollständige Verdampfung verdampfbarer Komponenten aus einer rückstandshaltigen - zum Beispiel salzhaltigen - Lösung gewährleisten, sondern auch die Rückstände als eine aus dem Sumpf abführbare, pumpfähige Masse bereitstellen. Bei einem Dünnschichtverdampfer, der nach dem vorstehend beschriebenen Prinzip arbeitet, ist dies jedoch nicht der Fall; denn Rückstände, beispielsweise Salze, können sich im Bereich des Sumpfablaufs abscheiden und Verkrustungen ausbilden, so daß der Sumpfaustrag aufgrund von Verstopfungen nicht mehr problemlos abgeführt werden kann. Der Sumpfablauf ist in der Regel der sich verjüngende Teil - meist der sich zu einem Rohr verjüngende Teil - des Sumpfes, durch den das Sumpfprodukt bei der Abführung aus dem Verdampfungsapparat hindurchgeführt wird. Der kontinuierliche Betrieb der Dünnschichtverdampfung muß beim Auftreten solcher Verstopfungen eingestellt werden, damit entsprechende Reinigungsarbeiten eingeleitet werden können. Auch bei der Verwendung anderer Verdampfungsapparate, zum Beispiel Destillationskolonnen, treten häufig die gleichen Probleme auf.The thin film evaporator described in the introduction is not only the complete Evaporation of vaporizable components from a residue - - Example, to ensure saline - solution, but also the residues as one provide pumpable mass from the sump. At a Thin-film evaporator, which operates on the principle described above, is this is not the case; because residues, such as salts, may be in the range Depositing the sump drain and form incrustations, so that the sump discharge due to blockages can not be easily removed. Of the Swamp drain is usually the tapered part - usually going down to a pipe tapering part - of the swamp, through which the sump product at discharge is passed through the evaporation apparatus. The continuous operation of the Thin film evaporation must be adjusted when such blockages occur so that appropriate cleaning work can be initiated. Also at the Use of other evaporation equipment, such as distillation columns, occur often the same problems.
Der vorliegenden Erfindung lag die Aufgabe zugrunde, eine Vorrichtung bereitzustellen, mit der gelöste Rückstände enthaltende Flüssigkeiten in einer Verdampfungsvorrichtung getrennt werden können, ohne daß der Sumpfablauf der Verdampfungsvorrichtung durch die Rückstände verstopft. Dabei sollen keine Reinigungsarbeiten notwendig sein, die eine kontinuierliche Verdampfung unterbrechen würden. Sowohl das Sumpfprodukt als auch das Kopfprodukt des entsprechenden Verdampfungsverfahrens sollen in möglichst schonender Weise erhalten werden. Die Vorrichtung soll effektiv und kostengünstig arbeiten.The object of the present invention was to provide a device with the dissolved residues containing liquids in an evaporator can be separated without the bottom outlet of the evaporation device clogged by the residues. There should be no cleaning necessary be that would interrupt a continuous evaporation. Both the bottoms product as well as the top product of the corresponding evaporation process be preserved in the gentlest possible way. The device should be effective and inexpensive work.
Lösung dieser Aufgabe ist dann eine Spülvorrichtung zur Entfernung von Rückständen aus dem Sumpfablauf einer Kopfprodukt und Sumpfprodukt erzeugenden, mit einem Sumpfablauf ausgestatteten Verdampfungsvorrichtung, enthaltend die Merkmale von Anspruch 1. The solution to this problem is then a flushing device for the removal of residues from the bottom effluent of a top product and bottom product producing, with a A sump drain equipped evaporation device, comprising the features of claim 1.
In einer bevorzugten Ausführungsform ist der Ablaufbehälter über Verbindungsleitungen unmittelbar mit dem Ablaufventil, dem Spülwasserventil, dem Behälterablaufventil, dem Spülablaufventil und dem Entlüftungsventil verbunden.In a preferred embodiment, the drainage container is via connecting lines directly with the drain valve, the flushing water valve, the tank drain valve, the purge valve and the vent valve connected.
Der Ablaufbehälter ist in der Regel oberhalb des Sammelbehälters und unterhalb des Sumpfes angeordnet.The drain tank is usually above the sump and below the Swamp arranged.
Die Spülablaufleitung kann in die Sumpfablaufleitung münden, so daß die Ablauf-Leitungseinrichtung einen für Spülmittel und Sumpfprodukt gemeinsamen Ausgang aufweist. Bevorzugt ist jedoch die Ablauf-Leitungseinrichtung in Form von zwei Leitungen, einer Spülablaufleitung und einer Sumpfablaufleitung, ausgebildet, so daß Sumpf und Spülmittel getrennt, durch verschiedene Ausgänge abgeführt werden. The Spülablaufleitung can open into the sump drain line, so that the drain line device a common outlet for detergent and bottom product having. Preferably, however, the drain conduit means in the form of two lines, a Spülablaufleitung and a sump drain line, formed so that Sump and detergent separated, discharged through various outputs.
Meist ist die Verdampfungseinrichtung evakuiert, da in der Regel nur unter vermindertem Druck eine schonende Verdampfung (dann unter niedrigeren Temperaturen stattfindend) möglich ist. Während der Abführung von Sumpfprodukt aus dem Verdampfungsapparat könnte deshalb Luft durch den Sumpfablauf in den Verdampfungsapparat eindringen. Erfindungsgemäß kann jedoch das Eindringen von Luft in den Verdampfungsapparat verhindert werden.Most of the evaporation device is evacuated, as usually only below reduced pressure gentle evaporation (then lower Temperatures taking place) is possible. During the discharge of Bottom product from the evaporator could therefore air through the Enter sump drain into the evaporator. According to the invention However, the penetration of air into the evaporator can be prevented.
In einer bevorzugten Ausführungsform der Erfindung münden ein oder mehrere Einleitungsrohre für Inertgas in den Ablaufbehälter und/oder in den Sammelbehälter und/oder in Verbindungsleitungen zwischen den Einrichtungen a) bis j). Diese Vorkehrungen sind insbesondere deshalb sinnvoll, um durch Einleiten von Schutzgas, zum Beispiel Stickstoff, das Eindringen von Luft (und damit auch von Sauerstoff) in die Apparatur zu verhindern. Auf diese Weise können im Kopfprodukt oder Sumpfprodukt befindliche, oxidationsempfindliche Stoffe geschont werden.In a preferred embodiment of the invention, one or more ends Introductory tubes for inert gas in the drain and / or in the Collecting container and / or in connecting lines between the facilities a) to j). These arrangements are therefore particularly useful to by Injecting gas, for example nitrogen, the ingress of air (and thus also of oxygen) in the apparatus to prevent. In this way can be located in the top product or bottom product, oxidation-sensitive Protecting substances.
Der Sammelbehälter ist bevorzugt mit einer Pumpe verbunden. Mit dieser kann der Inhalt des Sammelbehälters zirkuliert werden, so daß dieser homogen bleibt und die Absetzung von Rückständen vermieden wird.The collecting container is preferably connected to a pump. With this can the contents of the collecting container are circulated so that it remains homogeneous and the deposition of residues is avoided.
Es können prinzipiell alle Arten von Verdampfungsvorrichtungen eingesetzt werden, die Kopfprodukt und Sumpfprodukt erzeugen. Sowohl Kopfprodukt als auch Sumpfprodukt sind in der Regel Gemische. Jedoch kann insbesondere das Kopfprodukt auch aus einem einzigen Stoff bestehen. In einer bevorzugten Ausführungsform ist die Verdampfungsvorrichtung ein Dünnschichtverdampfer.In principle, all types of evaporation devices can be used which produce top product and bottoms product. Both top product also bottoms are usually mixtures. However, especially the Top product also consist of a single substance. In a preferred Embodiment, the evaporation device is a thin film evaporator.
Die erfindungsgemäße Spülvorrichtung wird insbesondere für die destillative Aufarbeitung salzhaltiger Lösungen verwendet. Es handelt sich dabei in der Regel um Lösungen, die neben den gelösten Salzen noch Wertprodukte (häufig oxidationsempfindliche Wertprodukte) enthalten. Meist sind noch weitere Aufarbeitungsschritte notwendig, um reine Wertprodukte zu erhalten.The flushing device according to the invention is especially for the distillative Working up saline solutions used. These are usually to solutions, in addition to the dissolved salts still value products (often oxidation-sensitive value products). Most are more Work-up steps necessary to obtain pure value products.
Der Sumpfablauf des Verdampfungsapparates wird mit Hilfe der erfindungsgemäßen Spülvorrichtung periodisch gespült. In der Regel wird ein Spülmittel eingesetzt, in dem enthaltende Rückstände gelöst werden. Die erfindungsgemäße Spülvorrichtung dient demgemäß bevorzugt der Entfernung löslicher Rückstände. Es können jedoch auch mechanische Spüleffekte wirksam sein, da das Spülmittel mit einer gewissen Geschwindigkeit auf die entsprechenden Rückstände auftreffen kann. Es ist somit nicht unbedingt notwendig, daß die Rückstände vollständig in dem Spülmittel löslich sind.The bottom outlet of the evaporation apparatus is using the inventive Rinsing device periodically rinsed. As a rule, a rinsing agent is used, in the residues are dissolved. The flushing device according to the invention Accordingly, it is preferred to remove soluble residues. It can, however Also, mechanical rinsing effects to be effective because the detergent with a certain Speed can hit the corresponding residues. It is thus Not absolutely necessary that the residues completely soluble in the detergent are.
Insbesondere dann, wenn Salze den Sumpfablauf verstopfen, empfiehlt es sich, Wasser als Spülmittel zu verwenden. Da in einigen Fällen in der Praxis Spülmittel in das Kopfprodukt des Verdampfungsapparates gelangen kann, empfiehlt es sich in diesen Fällen, ein Spülmittel zu verwenden, das die Qualität des Kopfproduktes und/oder die weitere Aufarbeitung des Kopfproduktes nicht nachhaltig negativ beeinträchtigt.In particular, when salts clog the sump drain, it is recommended that To use water as a detergent. As in some cases in practice rinse aid in the head product of the evaporation apparatus can get, it is recommended in In these cases, use a dishwashing detergent that improves the quality of the top product and / or the further workup of the overhead product not sustainably negative impaired.
Bei Verstopfung mit Salzen kann der Sumpfaustrag des Verdampfungsapparates nach dem Spülen und dem Vermischen mit dem Spülmittel (Wasser) abgepumpt und gelagert werden. Je nach der Beschaffenheit des erhaltenden Gemischs kann dieses beispielsweise in einer Rückstandsverbrennung verbrannt, in einer biologischen Kläranlage entsorgt, oder (falls noch Wertprodukte enthalten sind) weiter aufgearbeitet werden.In the case of blockage with salts, the sump discharge of the evaporation apparatus can after rinsing and mixing with the detergent (water) pumped out and stored. Depending on the nature of the resulting mixture can this burned, for example, in a residue combustion, in a biological wastewater treatment plant disposed of or (if value added products are still included) be further worked up.
Im folgenden soll die Funktionsweise der erfindungsgemäßen Vorrichtung anhand einer bevorzugten Ausführungsform, am Beispiel eines Salze abscheidenden Dünnschichtverdampfers, beschrieben werden. In the following, the operation of the device according to the invention is based on a preferred embodiment, the example of a salt-depositing Thin-film evaporator, are described.
In der anliegenden Zeichnung ist in Fig. 1 ein Dünnschichtverdampfer mit einer erfindungsgemäßen Spülvorrichtung dargestellt. Diese Spülvorrichtung weist eine Ablaufleitungs-Einrichtungen (6, 16) auf, die in Form von zwei Leitungen, einer Spülablaufleitung (6) und einer Sumpfablaufleitung (16), ausgebildet sind.In the accompanying drawing, in Fig. 1 is a thin film evaporator with an inventive Flushing device shown. This flushing device has drainage means (6, 16), in the form of two lines, a Spülablaufleitung (6) and a sump drain line (16) are formed.
Um zu vermeiden, daß der Sumpfablauf durch auskristallisierende Salze verstopft, wird
dieser periodisch gespült. Dazu wird das Sumpfprodukt zunächst in einem Ablaufbehälter
7 aufgefangen, welcher sich dabei allmählich auffüllt. Nach Erreichen eines bestimmten
Füllstandes wird das Ablaufventil 10 geschlossen und das Vakuum im Ablaufbehälter
7 durch Öffnen des Behälterablaufventils 12 zum Sammelbehälter 8 aufgehoben
(der Sammelbehälter 8 steht unter Normaldruck oder leichtem Überdruck). Anschließend
wird das Entlüftungsventil 14 geöffnet, und der Inhalt des Ablaufbehälters 7
läuft in den Sammelbehälter 8 ab. Der Inhalt des Sammelbehälters 8 wird zweckmäßigerweise
mittels einer Pumpe 9 zirkuliert, um diesen homogen zu halten und um mögliche
Salzabsetzung zu verhindern. Der Inhalt wird zur Zwischenlagerung und weiteren
Verwertung, zum Beispiel der Verbrennung, kontinuierlich oder diskontinuierlich abgeführt.In order to avoid that the sump drain is blocked by crystallizing salts, is
this periodically rinsed. For this, the bottom product is first in a
Nun wird der Ablaufbehälter 7 gespült. Zweckmäßigerweise verwendet man dazu Wasser,
bevorzugt warmes Wasser oder Dampfkondensat. Zum Einleiten des Spülvorganges
werden das Behälterablaufventil 12 geschlossen, das Spülablaufventil 13 und das
Spülwasserventil 11 geöffnet. Das warme Spülwasser, das durch das Einleitungsrohr für
Spülmittel 3 zugeführt wird, durchströmt nun den Ablaufbehälter 7 und entfernt auf
diese Weise Salzabsetzungen. Der Spülablauf kann (je nach enthaltenden Bestandteilen)
beispielsweise einer biologischen Kläranlage zugeführt werden. Spüldauer und Wasserdurchfluß
werden nach Bedarf so eingestellt, daß die benötigte Wassermenge so gering
wie nötig ist. In der Regel ist (je nach Belastung des Verdampfungsapparates und Salzgehalt)
eine Spülzeit von 1 bis 2 Minuten ausreichend. Um Verstopfungen in der Ablaufleitung
zum Sammelbehälter 8 zu vermeiden, wird diese Leitung durch Öffnen des
Behälterablaufventils 12 (anstelle des Spülablaufventils 13) periodisch gespült. Vorzugsweise
erfolgt dies alle 10 bis 20 Spüldurchgänge. Now the
Nach Ablauf einer Vorspülzeit wird das Spülablaufventil 13 geschlossen, und im weiteren
Verlauf der Spülphase wird das Wasser über den Ablaufbehälter 7 und die Ablaufleitung
durch die Entlüftungsleitung und durch das Entlüftungsventil 14 gespült. Anschließend
wird das Spülwasserventil 11 geschlossen und um den Ablaufbehälter zu
entleeren, das Spülablaufventil 13 geöffnet. Restliches Spülwasser läßt man durch Öffnen
des Behälterablaufventils 12 ablaufen. Danach werden alle Ventile wieder geschlossen.
Durch Öffnen des Ablaufventils 10 wird der Ablaufbehälter wieder evakuiert, und der
Ablaufzyclus kann erneut beginnen.After expiration of a pre-purging the
By opening the
Um das Eindringen von Luft zu vermeiden, sind die Ablaufleitungen zum Sammelbehälter und zum Spülmittelablauf mit Inertgasspülungen (in der Regel Stickstoffspülung) versehen. Die Zufuhr von Inertgas erfolgt über die Einleitungsrohre (4; 5).To prevent the ingress of air, the drain lines are to the sump and for flushing with inert gas flushes (usually nitrogen flushing) Mistake. The supply of inert gas via the inlet pipes (4; 5).
Vorteilhaft ist eine automatisierte Ablaufsteuerung dieser Ablauf- und Spülvorgänge.An automatic sequence control of these draining and rinsing operations is advantageous.
In Fig. 1 mündet zwischen dem Anlaufbehälter 7 und dem Ablaufventil 10 ein erstes
Einleitungsrohr 5 zum Einleiten von Inertgas in die Leitung 17 zur Überführung des
Sumpfprodukts.In Fig. 1 opens between the run-
Weiterhin ist der Sammelbehälter 8 mit dem Ablaufbehälter 7 über eine Leitung verbunden,
die mit dem Behälterablaufventil 12 versehen ist und in die ein zweites Einleitungsrohr
4 zum Einleiten von Inertgas mündet. Furthermore, the collecting
- 1.1.
- Zulauf in den VerdampfungsapparatFeed into the evaporation apparatus
- 2.Second
- Dampfstrom zur Beheizung des Mantels des VerdampfungsapparatesSteam flow for heating the jacket of the evaporator
- 3.Third
- Einleitungsrohr für SpülmittelInlet pipe for detergent
- 4.4th
- Einleitungsrohr für InertgasInlet pipe for inert gas
- 5.5th
- Einleitungsrohr für InertgasInlet pipe for inert gas
- 6.6th
- SpülablaufleitungSpülablaufleitung
- 7.7th
- Ablaufbehälterdrain tank
- 8.8th.
- SammelbehälterClippings
- 9.9th
- Pumpepump
- 10.10th
- Ablaufventildrain valve
- 11.11th
- SpülwasserventilFlush Water
- 12.12th
- BehälterablaufventilTank drain valve
- 13.13th
- Spülablaufventilcleaning outflow valve
- 14.14th
- Entlüftungsventilvent valve
- 15.15th
- Kopfstrom des VerdampfungsapparatesTop stream of the evaporator
- 16.16th
- SumpfablaufleitungSump drain line
- 17.17th
- aus dem Sumpf zum Ablaufventil führende Leitungfrom the sump to the drain valve leading line
Claims (11)
- A cleaning apparatus for removing residues from the bottoms outflow of an evaporation apparatus which generates a tops product and bottoms product and is equipped with a bottoms outflow, comprising:an outflow vessel (7) which has a line (17) provided with an outflow valve (10) for transferring the bottoms product of the evaporation apparatus, a further line (5) provided with an outflow valve (14) for aeration and deaeration, also an inlet tube (3) provided with a cleaning water valve (11) for introducing cleaning agent and also a first outflow line device (6) provided with a cleaning outflow valve (13) for draining off the cleaning agent; anda collection vessel (8) for receiving the outflow vessel contents, which collection vessel is connected via a further line provided with a vessel outflow valve (12) to the outflow vessel (7) and is further connected to a second outflow line device (16).
- A cleaning apparatus according to claim 1, wherein the line (5) for aeration and deaeration opens between the outflow vessel (7) and the outflow valve (10) into the line (17) for transferring the bottoms product.
- A cleaning apparatus according to claim 1 or 2, wherein an introduction tube (4) for introducing inert gas opens between the vessel outflow valve (12) and the collection vessel (8) into the line via which the collection vessel (8) is connected to the outflow vessel (7).
- A cleaning apparatus according to one of claims 1 to 3, wherein the outflow line devices (6, 16) are constructed in the form of two lines, a cleaning outflow line (6), which comprises the cleaning outflow valve (13) and a bottoms outflow line (16), which is connected to the collection vessel (8), in such a way that the two lines have a common exit or two separate exits.
- A cleaning apparatus according to one of claims 1 to 4, wherein introduction tubes for introducing inert gas open into the outflow vessel (7) and/or into the collection vessel (8).
- A cleaning apparatus according to one of claims 4 or 5, wherein the bottoms outflow line (16) has a pump (9).
- A cleaning apparatus according to one of claims 1 to 6 additionally comprising an evaporation apparatus for the workup of salt-containing solutions by distillation, which evaporation apparatus produces tops product and bottoms product and has a bottoms outflow which is connected to the line (17) for transferring the bottoms product.
- A cleaning apparatus according to claim 7, wherein the outflow vessel (7) is disposed above the collection vessel (8) and below the bottoms outflow of the evaporation apparatus.
- A cleaning apparatus according to claim 7 or 8, wherein the evaporation apparatus is a thin-film evaporator.
- A cleaning apparatus according to one of claims 7 to 9, wherein the evaporation apparatus may be evacuated.
- The use of a cleaning apparatus according to one of claims 1 to 10 for the workup of salt-containing solutions by distillation.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE19855910 | 1998-12-03 | ||
| DE19855910A DE19855910A1 (en) | 1998-12-03 | 1998-12-03 | Rinsing device for removing residues |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| EP1005888A1 EP1005888A1 (en) | 2000-06-07 |
| EP1005888B1 true EP1005888B1 (en) | 2005-09-14 |
Family
ID=7889920
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP99123942A Expired - Lifetime EP1005888B1 (en) | 1998-12-03 | 1999-12-03 | Rinsing system for removing residues |
Country Status (6)
| Country | Link |
|---|---|
| US (1) | US6443170B1 (en) |
| EP (1) | EP1005888B1 (en) |
| JP (1) | JP2000197862A (en) |
| CN (1) | CN1216697C (en) |
| AT (1) | ATE304395T1 (en) |
| DE (2) | DE19855910A1 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2013164308A1 (en) | 2012-05-04 | 2013-11-07 | Bayer Materialscience Ag | Method for treating a substance mixture comprising an aromatic amine, in particular a substance mixture of raw aniline |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE10361003B3 (en) | 2003-12-23 | 2005-07-28 | Hte Ag The High Throughput Experimentation Company | Apparatus and method for pressure and flow control in parallel reactors |
| DE102011109454A1 (en) * | 2011-08-04 | 2013-02-07 | Hte Aktiengesellschaft | Process for treating product fluid streams |
| CN104411681B (en) | 2012-07-11 | 2017-03-29 | 科思创德国股份有限公司 | Method of the post processing by the bottoms for preparing isocyanates generation |
| JP6010457B2 (en) * | 2012-12-28 | 2016-10-19 | 東京エレクトロン株式会社 | Liquid processing apparatus and chemical recovery method |
| US10345058B1 (en) | 2015-11-18 | 2019-07-09 | Gradiant Corporation | Scale removal in humidification-dehumidification systems |
| US10513445B2 (en) | 2016-05-20 | 2019-12-24 | Gradiant Corporation | Control system and method for multiple parallel desalination systems |
| CN115229187B (en) * | 2021-10-29 | 2023-07-28 | 南京尚吉增材制造研究院有限公司 | Device and method for removing inorganic salt pore-forming agent in porous metal preparation process |
| CN114769245A (en) * | 2022-04-25 | 2022-07-22 | 河南开祥精细化工有限公司 | Float valve tower cleaning system and cleaning method |
Family Cites Families (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3046163A (en) * | 1960-04-06 | 1962-07-24 | Detrex Chem Ind | Method and apparatus for interiorly cleaning tanks and the like |
| US3185661A (en) * | 1963-06-03 | 1965-05-25 | Phillips Petroleum Co | Particle agitation system |
| US4770196A (en) * | 1986-02-13 | 1988-09-13 | Osswald Hannes E | Chemical cleaning system |
| US5061348A (en) | 1988-08-12 | 1991-10-29 | Alameda Instruments | Sulfuric acid reprocessor with continuous purge of second distillation vessel |
| US5330624A (en) | 1991-12-27 | 1994-07-19 | Phillips Petroleum Company | Fractionator-reboiler sludge removal system and method |
| US5603826A (en) * | 1996-02-15 | 1997-02-18 | V Q Corporation | Return pump system for use with clean-in-place system for use with vessels |
| US5690151A (en) * | 1996-04-02 | 1997-11-25 | Packaging Systems, Inc. | Dual channel bag filling machine with a clean-in-place system that cleans one channel while the other continues to fill bags |
-
1998
- 1998-12-03 DE DE19855910A patent/DE19855910A1/en not_active Withdrawn
-
1999
- 1999-12-01 US US09/451,858 patent/US6443170B1/en not_active Expired - Lifetime
- 1999-12-02 JP JP11376206A patent/JP2000197862A/en active Pending
- 1999-12-03 DE DE59912551T patent/DE59912551D1/en not_active Expired - Lifetime
- 1999-12-03 EP EP99123942A patent/EP1005888B1/en not_active Expired - Lifetime
- 1999-12-03 AT AT99123942T patent/ATE304395T1/en not_active IP Right Cessation
- 1999-12-03 CN CN991159950A patent/CN1216697C/en not_active Expired - Lifetime
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2013164308A1 (en) | 2012-05-04 | 2013-11-07 | Bayer Materialscience Ag | Method for treating a substance mixture comprising an aromatic amine, in particular a substance mixture of raw aniline |
Also Published As
| Publication number | Publication date |
|---|---|
| ATE304395T1 (en) | 2005-09-15 |
| DE19855910A1 (en) | 2000-06-08 |
| CN1216697C (en) | 2005-08-31 |
| EP1005888A1 (en) | 2000-06-07 |
| CN1260248A (en) | 2000-07-19 |
| DE59912551D1 (en) | 2005-10-20 |
| JP2000197862A (en) | 2000-07-18 |
| US6443170B1 (en) | 2002-09-03 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| EP0451721B1 (en) | Process for cleaning objects and apparatus therefor | |
| DE2136686A1 (en) | Apparatus and method for vaporizing liquids | |
| EP1005888B1 (en) | Rinsing system for removing residues | |
| WO2007107260A1 (en) | Process for removing volatile components from a substance mixture and apparatus for performing this process | |
| DE2850104A1 (en) | METHOD FOR DIRECTLY WARMING A LIQUID MEDIUM USING THE CONDENSATION HEAT, AND DEVICE FOR CARRYING OUT THE METHOD | |
| DE10237281A1 (en) | Device for the continuous extraction of extract substances from plants | |
| DE2342064C2 (en) | Method and device for degreasing wool | |
| DE3935892A1 (en) | METHOD AND DEVICE FOR CONCENTRATING A SULFURIC ACID AND WATER CONTAINING WATER | |
| EP0508986B1 (en) | Process for purifying organically polluted waste water | |
| DE2428604A1 (en) | CLEANING SYSTEM FOR REMOVING SOLID AND SOLUBLE MATERIALS FROM SOLUTIONS | |
| DE1771810A1 (en) | Method and device for cleaning metal parts | |
| DE3226344C2 (en) | ||
| DE2115589C3 (en) | Process for separating emulsions and using a thin-film evaporator for this purpose | |
| EP0057228A1 (en) | Method and device for purifying waste water | |
| DE60013484T2 (en) | METHOD FOR CLEANING OBJECTS THROUGH A WARMED LIQUID, AND APPARATUS FOR CARRYING OUT THIS METHOD | |
| DE2034372B2 (en) | Method and apparatus for treating separation vapor from the fractionation of tall oil | |
| DE2162838C3 (en) | Liquid evaporator and method of filling or emptying the same | |
| DE19830046C1 (en) | Removal of water from metalworking coolant-lubricating emulsions | |
| DE2713266A1 (en) | Flash evaporation for treatment bath recovery - using vapour recompression and recycle to balance evaporator load | |
| DE2416457C3 (en) | Process and device for working up phthalic anhydride distillation bottoms | |
| DE906691C (en) | Process for evaporation of liquids | |
| DE9203968U1 (en) | Oil separator with integrated microfiltration device | |
| DE1093160B (en) | Method and device for electrolytic treatment, in particular for electroplating metal objects | |
| DE2360491C2 (en) | Processes for wastewater treatment and systems set up for this purpose | |
| DE3022679A1 (en) | Industrial wastes treatment - by adding heavy metal complex decomposing agents before ultrafiltration |
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 |
Kind code of ref document: A1 Designated state(s): AT BE CH CY DE DK ES FI FR GB GR IE IT LI LU MC NL PT SE |
|
| AX | Request for extension of the european patent |
Free format text: AL;LT;LV;MK;RO;SI |
|
| 17P | Request for examination filed |
Effective date: 20000825 |
|
| AKX | Designation fees paid |
Free format text: AT BE CH CY DE DK ES FI FR GB GR IE IT LI LU MC NL PT SE |
|
| 17Q | First examination report despatched |
Effective date: 20020515 |
|
| GRAP | Despatch of communication of intention to grant a patent |
Free format text: ORIGINAL CODE: EPIDOSNIGR1 |
|
| 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 CH CY DE DK ES FI FR GB GR IE IT LI LU MC NL PT SE |
|
| 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: 20050914 Ref country code: FI 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: 20050914 |
|
| REG | Reference to a national code |
Ref country code: GB Ref legal event code: FG4D Free format text: NOT ENGLISH |
|
| 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 |
|
| REF | Corresponds to: |
Ref document number: 59912551 Country of ref document: DE Date of ref document: 20051020 Kind code of ref document: P |
|
| 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: 20051203 Ref country code: AT Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20051203 |
|
| GBT | Gb: translation of ep patent filed (gb section 77(6)(a)/1977) | ||
| 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: 20051214 Ref country code: DK 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: 20051214 |
|
| 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 FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20051225 |
|
| PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: MC Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20051231 Ref country code: LU Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20051231 |
|
| REG | Reference to a national code |
Ref country code: SE Ref legal event code: TRGR |
|
| PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
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: 20060214 |
|
| REG | Reference to a national code |
Ref country code: IE Ref legal event code: FD4D |
|
| ET | Fr: translation filed | ||
| 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: 20060615 |
|
| REG | Reference to a national code |
Ref country code: FR Ref legal event code: PLFP Year of fee payment: 17 |
|
| REG | Reference to a national code |
Ref country code: FR Ref legal event code: PLFP Year of fee payment: 18 |
|
| REG | Reference to a national code |
Ref country code: FR Ref legal event code: PLFP Year of fee payment: 19 |
|
| PGFP | Annual fee paid to national office [announced via postgrant information from national office to epo] |
Ref country code: BE Payment date: 20181221 Year of fee payment: 20 Ref country code: CH Payment date: 20181227 Year of fee payment: 20 Ref country code: FR Payment date: 20181231 Year of fee payment: 20 Ref country code: GB Payment date: 20181221 Year of fee payment: 20 |
|
| PGFP | Annual fee paid to national office [announced via postgrant information from national office to epo] |
Ref country code: DE Payment date: 20190228 Year of fee payment: 20 Ref country code: NL Payment date: 20181221 Year of fee payment: 20 Ref country code: IT Payment date: 20181220 Year of fee payment: 20 |
|
| PGFP | Annual fee paid to national office [announced via postgrant information from national office to epo] |
Ref country code: SE Payment date: 20181228 Year of fee payment: 20 |
|
| REG | Reference to a national code |
Ref country code: DE Ref legal event code: R071 Ref document number: 59912551 Country of ref document: DE |
|
| REG | Reference to a national code |
Ref country code: NL Ref legal event code: MK Effective date: 20191202 |
|
| REG | Reference to a national code |
Ref country code: CH Ref legal event code: PL |
|
| REG | Reference to a national code |
Ref country code: BE Ref legal event code: MK Effective date: 20191203 |
|
| REG | Reference to a national code |
Ref country code: GB Ref legal event code: PE20 Expiry date: 20191202 |
|
| REG | Reference to a national code |
Ref country code: SE Ref legal event code: EUG |
|
| 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 EXPIRATION OF PROTECTION Effective date: 20191202 |