EP1005888A1 - Rinsing system for removing residues - Google Patents

Rinsing system for removing residues Download PDF

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Publication number
EP1005888A1
EP1005888A1 EP99123942A EP99123942A EP1005888A1 EP 1005888 A1 EP1005888 A1 EP 1005888A1 EP 99123942 A EP99123942 A EP 99123942A EP 99123942 A EP99123942 A EP 99123942A EP 1005888 A1 EP1005888 A1 EP 1005888A1
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EP
European Patent Office
Prior art keywords
drain
container
valve
flushing
evaporator
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Granted
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EP99123942A
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German (de)
French (fr)
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EP1005888B1 (en
Inventor
Frans Dr. Vansant
Jozef De Hert
Dieter Dr. Köffer
Gerhard Dr. Theis
Winfried Terjung
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BASF SE
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BASF SE
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    • 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 removing residues the bottom drain of an evaporator and its use for Working up saline solutions by distillation.
  • Thin film evaporation is used for continuous distillation, especially for Evaporation of temperature-sensitive substances from high-boiling Residues, and for the concentration of temperature-sensitive substances used.
  • you distribute the liquid by trickling it down (falling film evaporator), Action of centrifugal force (special embodiment of a Rotary evaporator), specially designed wipers (film trudder) or others Techniques for thin layers (magnitude of the layer thickness usually 0.1 mm) on the (usually) heated surfaces.
  • Thin Liquid layers allow rapid evaporation, so that the contained components only briefly the (usually) higher Are exposed to temperatures in the evaporator.
  • the dwell time, the temperature and the pressure (vacuum) are according to the respective separation task designed.
  • Evaporation devices which are in common technical usage are already referred to as thin film evaporators, according to the invention also all other evaporation devices as thin film evaporators understood that work on the principle described above.
  • a typical thin film evaporator has a vertical one from the outside heated pipe, on the inner surface of which the product to be evaporated by a rotor is spread out 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 film of liquid over the heating surface.
  • the low-boiling Components evaporate as the residue drains down.
  • the Vapor vapors flow through a droplet separator, which is in the head of the Evaporator is located in a separately arranged condenser condensed.
  • a rotor is included for the mechanical liquid distribution swinging metal wiper blades installed. During operation are the wiper blades due to the centrifugal force against the evaporator wall pressed, which is an even product distribution and an intense Liquid mixing of the liquid film causes.
  • the thin film evaporator described in the introduction is not only intended to be the complete one Evaporation of evaporable components from a residue - for Example saline - ensure solution, but also the residues as one Provide pumpable mass that can be removed from the sump.
  • a Thin film evaporator which works according to the principle described above however, this is not the case; because residues, for example salts, can accumulate in the Separate the area of the sump drain and form incrustations so that the Swamp discharge no longer easily removed due to blockages can be.
  • the swamp drain is usually the tapered part - usually that part tapering to a tube - the sump through which the sump product is led away from the evaporator during discharge.
  • the continuous operation of thin film evaporation must occur when such Blockages are set so that appropriate cleaning work can be initiated. Even when using others Evaporation devices, for example distillation columns, often occur same problems
  • the object of the present invention was a device Provide with the liquid containing dissolved residues in one Evaporator can be separated without the sump drain the evaporation device is blocked by the residues. None should Cleaning work may be necessary which requires continuous evaporation would interrupt. Both the bottom product and the top product of the corresponding evaporation process should be as gentle as possible be preserved. The device should work effectively and inexpensively.
  • the drain container is over Connecting lines directly to the drain valve, the flushing water valve, the tank drain valve, the flush drain valve and the vent valve connected.
  • the drain container is usually above and below the collection container of the swamp.
  • the flushing drain pipe can open into the sump drain, so that the Drain line device a common for detergent and sump product Has output.
  • the drain line device is preferably in the form of two lines, a rinsing drain line and a sump drain line, trained so that sump and detergent separated, through different exits be dissipated.
  • the evaporation device is mostly evacuated, since it is usually only under reduced evaporation gentle evaporation (then under lower Temperatures taking place) is possible. During the removal of Bottom product from the evaporator could therefore air through the Penetrate sump drain into the evaporator. According to the invention However, air can be prevented from entering the evaporator:
  • These precautions are particularly useful to get through Introducing protective gas, for example nitrogen, the penetration of air (and to prevent oxygen from entering the apparatus. In this way can be in the top product or bottom product, sensitive to oxidation Protect fabrics.
  • 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 removal of residues is avoided.
  • the evaporation device is a thin-film evaporator.
  • the rinsing device according to the invention is particularly for the distillative Processing saline solutions used. This is usually the case for solutions that, in addition to the dissolved salts, also valuable products (often contain oxidation sensitive products). There are usually more Refurbishment steps necessary to obtain pure value products.
  • the bottom outlet of the evaporator is with the help of the invention Flushing device rinsed periodically.
  • a detergent is used in the residues contained are solved.
  • the flushing device according to the invention is therefore preferably used to remove soluble residues.
  • it can mechanical washing effects can also be effective, as the detergent has a certain Speed can hit the corresponding residues. So it is it is not absolutely necessary for the residues to be completely soluble in the detergent are.
  • detergent in the top product of the evaporator can reach, it is recommended in In these cases, use a detergent that matches the quality of the head product and / or the further processing of the top product is not sustainable negative impaired.
  • the bottom of the evaporator can be discharged pumped out after rinsing and mixing with the detergent (water) and stored.
  • the detergent water
  • this burned for example, in a residue incinerator, in a biological wastewater treatment plant, or (if valuable products are still contained) to be worked up further.
  • This flushing device has one Drain line device (6, 16) on, in the form of two lines, one Flush drain line (6) and a sump drain line (16) is formed.
  • the bottom product is first in one Drainage container 7 collected, which fills up gradually.
  • the drain valve 10 is closed and the vacuum in the drain container 7 by opening the container drain valve 12 for Collection container 8 lifted (the collection container 8 is under normal pressure or slight overpressure).
  • the vent valve 14 is opened, and the content of the drain container 7 runs into the collecting container 8.
  • the content the collecting container 8 is expediently circulated by means of a pump 9, to keep it homogeneous and to prevent possible salt settling.
  • the Content is used for intermediate storage and further use, for example the Combustion, continuously or discontinuously removed.
  • the drain container 7 is rinsed. It is expedient to use this Water, preferably warm water or steam condensate.
  • the container drain valve 12 are closed Flush drain valve 13 and the flush water valve 11 opened.
  • the warm Rinse water which is supplied through the detergent feed pipe 13, now flows through the drain container 7 and is removed in this way Salt deposits.
  • the rinsing process can (depending on the components it contains) for example, a biological sewage treatment plant. Rinsing time and Water flow are adjusted as required so that the required The amount of water is as small as necessary. As a rule, (depending on the load on the Evaporator and salinity) a rinsing time of 1 to 2 minutes sufficient.
  • To blockages in the drain line to the collecting tank 8 avoid this line by opening the container drain valve 12 (instead of the flushing drain valve 13) flushed periodically. This is preferably done every 10 to 20 rinses.
  • the rinse drain valve 13 is closed, and in further course of the rinsing phase, the water is via the drain tank 7 and the drain line through the vent line and through the vent valve 14 rinsed. Then the flushing water valve 11 is closed and around the To empty the drain container, the flushing drain valve 13 opened. The rest Flushing water is allowed to run off by opening the container drain valve 12. After that all valves are closed again.
  • the drain container is evacuated again, and the cycle can begin again.
  • the drain lines are to Collection container and for flushing detergent with inert gas flushing (usually Nitrogen purging). Inert gas is supplied via the Inlet pipes (4; 5).

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  • 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)
  • Apparatuses And Processes For Manufacturing Resistors (AREA)
  • Silver Salt Photography Or Processing Solution Therefor (AREA)
  • Cleaning Or Drying Semiconductors (AREA)
  • Pipeline Systems (AREA)
  • Heat Treatment Of Water, Waste Water Or Sewage (AREA)

Abstract

The rinsing apparatus for removing residue from the sump run-off of an evaporator comprises (a) a run-off container (7), (b) a collector container (8), (c) a run-off valve (10), (d) a rinsing water valve (11), (e) run-off container valve (12), (f) rinsing run-off valve (13), (g) vent valve (14), (h) a delivery pipe (17) from the sump to the run-off valve (10), (i) a inlet pipe (3) for the rinsing agent, (j) a run-off pipe device (6,16) and a connector to the devices (a) to (j). An Independent claim is included for the use of a rinsing apparatus.

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 removing residues the bottom drain of an evaporator and its use for Working up saline solutions by distillation.

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 (Fallfilm-Verdampfer), 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, especially for Evaporation of temperature-sensitive substances from high-boiling Residues, and for the concentration of temperature-sensitive substances used. Here you distribute the liquid by trickling it down (falling film evaporator), Action of centrifugal force (special embodiment of a Rotary evaporator), specially designed wipers (film trudder) or others Techniques for thin layers (magnitude of the layer thickness usually 0.1 mm) on the (usually) heated surfaces. Thin Liquid layers allow rapid evaporation, so that the contained components only briefly the (usually) higher Are exposed to temperatures in the evaporator. The dwell time, the temperature and the pressure (vacuum) are according to the respective separation task designed. Thereby to protect the substances concerned are possible prefer low temperatures and short dwell times. Next Evaporation devices, which are in common technical usage are already referred to as thin film evaporators, according to the invention also all other evaporation devices as thin film evaporators understood that work 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 one from the outside heated pipe, on the inner surface of which the product to be evaporated by a rotor is spread out 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 film of liquid over the heating surface. The low-boiling Components evaporate as the residue drains down. The Vapor vapors flow through a droplet separator, which is in the head of the Evaporator is located in a separately arranged condenser condensed. A rotor is included for the mechanical liquid distribution swinging metal wiper blades installed. During operation are the wiper blades due to the centrifugal force against the evaporator wall pressed, which is an even product distribution and an intense Liquid 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 arises when evaporating liquids that contain dissolved residues, for example dissolved salts:
  • The reason is that these residues are deposited in the swamp. These are residues that were usually present as dissolved components in the liquid before the evaporation and separate out as a solid after the evaporation of the solvent. The evaporation of salt solutions can be cited as an example, salt being obtained as a solid residue in the bottom of the evaporator after the evaporation of solvent. In addition to such salts, soluble residues can in principle be any solids that can be removed with a detergent - usually dissolved in a solvent.

    • 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 aufThe thin film evaporator described in the introduction is not only intended to be the complete one Evaporation of evaporable components from a residue - for Example saline - ensure solution, but also the residues as one Provide pumpable mass that can be removed from the sump. At a Thin film evaporator, which works according to the principle described above however, this is not the case; because residues, for example salts, can accumulate in the Separate the area of the sump drain and form incrustations so that the Swamp discharge no longer easily removed due to blockages can be. The swamp drain is usually the tapered part - usually that part tapering to a tube - the sump through which the sump product is led away from the evaporator during discharge. The continuous operation of thin film evaporation must occur when such Blockages are set so that appropriate cleaning work can be initiated. Even when using others Evaporation devices, for example distillation columns, often occur 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 a device Provide with the liquid containing dissolved residues in one Evaporator can be separated without the sump drain the evaporation device is blocked by the residues. None should Cleaning work may be necessary which requires continuous evaporation would interrupt. Both the bottom product and the top product of the corresponding evaporation process should be as gentle as possible be preserved. The device should work effectively and inexpensively.

    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:

  • a) einen Ablaufbehälter,
  • b) einen Sammelbehälter,
  • c) ein Ablaufventil,
  • d) ein Spülwasserventil,
  • e) ein Behälterablaufventil,
  • f) ein Spülablaufventil,
  • g) ein Entlüftungsventil,
  • h) eine aus dem Sumpf zum Ablaufventil führende Leitung,
  • i) ein Einleitungsrohr für Spülmittel,
  • j) eine Ablaufleitungs-Einrichtung und
    • Verbindungsleitungen zwischen den Einrichtungen a) bis j).The solution to this problem is then a rinsing device for removing residues from the bottom drain of an overhead product and bottom product-producing evaporation device equipped with a bottom outlet, comprising:
  • a) a drain container,
  • b) a collecting container,
  • c) a drain valve,
  • d) a flushing water valve,
  • e) a container drain valve,
  • f) a flushing drain valve,
  • g) a vent valve,
  • h) a line leading from the sump to the drain valve,
  • i) an inlet pipe for detergent,
  • j) a drain line facility and
    • Connection lines between the devices a) to j).

    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 drain container is over Connecting lines directly to the drain valve, the flushing water valve, the tank drain valve, the flush drain valve and the vent valve connected.

    Der Ablaufbehälter ist in der Regel oberhalb des Sammelbehälters und unterhalb des Sumpfes angeordnet.The drain container is usually above and below the collection container of the swamp.

    Die Spülablaufleitung kann in die Sumpfabtaufleitung 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 flushing drain pipe can open into the sump drain, so that the Drain line device a common for detergent and sump product Has output. However, the drain line device is preferably in the form of two lines, a rinsing drain line and a sump drain line, trained so that sump and detergent separated, through different exits be dissipated.

    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:The evaporation device is mostly evacuated, since it is usually only under reduced evaporation gentle evaporation (then under lower Temperatures taking place) is possible. During the removal of Bottom product from the evaporator could therefore air through the Penetrate sump drain into the evaporator. According to the invention However, air can be prevented from entering the evaporator:

    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 open Inlet pipes for inert gas in the drain container and / or in the Collection containers and / or in connecting lines between the facilities a) to j). These precautions are particularly useful to get through Introducing protective gas, for example nitrogen, the penetration of air (and to prevent oxygen from entering the apparatus. In this way can be in the top product or bottom product, sensitive to oxidation Protect fabrics.

    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 removal 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 that produce top product and bottom product. Both head product and mixtures are also usually the bottom product. However, especially that Head product also consist of a single substance. In a preferred one In one 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 rinsing device according to the invention is particularly for the distillative Processing saline solutions used. This is usually the case for solutions that, in addition to the dissolved salts, also valuable products (often contain oxidation sensitive products). There are usually more Refurbishment steps necessary to obtain pure value products.

    Der Sumpfablauf des Verdampfungsapparates wird mit Hilfe der erfindungsgemaßen 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 evaporator is with the help of the invention Flushing device rinsed periodically. As a rule, a detergent is used in the residues contained are solved. The flushing device according to the invention is therefore preferably used to remove soluble residues. However, it can mechanical washing effects can also be effective, as the detergent has a certain Speed can hit the corresponding residues. So it is it is not absolutely necessary for the residues to be 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 Kopfprodukts nicht nachhaltig negativ beeinträchtigt.Especially when salts clog the sump drain, it is advisable to Use water as a detergent. In some cases, in practice, detergent in the top product of the evaporator can reach, it is recommended in In these cases, use a detergent that matches the quality of the head product and / or the further processing of the top product is not sustainable 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 event of constipation with salts, the bottom of the evaporator can be discharged pumped out after rinsing and mixing with the detergent (water) and stored. Depending on the nature of the mixture obtained this burned, for example, in a residue incinerator, in a biological wastewater treatment plant, or (if valuable products are still contained) to be worked up further.

    Im folgenden soll die Funktionsweise der erfindungsgemäßen Vorrichtung anhand einer bevorzugten Ausführungsform, am Beispiel eines Salze abscheidenden Dünnschichtverdampfers, beschrieben werden. In the following, the mode of operation of the device according to the invention will be described a preferred embodiment, using the example of a salt separating 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-Einrichtung (6, 16) auf, die in Form von zwei Leitungen, einer Spülablaufleitung (6) und einer Sumpfablaufleitung (16), ausgebildet ist.In the accompanying drawing, a thin-film evaporator with a shown flushing device according to the invention. This flushing device has one Drain line device (6, 16) on, in the form of two lines, one Flush drain line (6) and a sump drain line (16) is 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 bottom drain is blocked by crystallizing salts, it is flushed periodically. For this purpose, the bottom product is first in one Drainage container 7 collected, which fills up gradually. To When a certain fill level is reached, the drain valve 10 is closed and the vacuum in the drain container 7 by opening the container drain valve 12 for Collection container 8 lifted (the collection container 8 is under normal pressure or slight overpressure). Then the vent valve 14 is opened, and the content of the drain container 7 runs into the collecting container 8. The content the collecting container 8 is expediently circulated by means of a pump 9, to keep it homogeneous and to prevent possible salt settling. The Content is used for intermediate storage and further use, for example the Combustion, continuously or discontinuously removed.

    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 13 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 drain container 7 is rinsed. It is expedient to use this Water, preferably warm water or steam condensate. To initiate the Flushing the container drain valve 12 are closed Flush drain valve 13 and the flush water valve 11 opened. The warm Rinse water which is supplied through the detergent feed pipe 13, now flows through the drain container 7 and is removed in this way Salt deposits. The rinsing process can (depending on the components it contains) for example, a biological sewage treatment plant. Rinsing time and Water flow are adjusted as required so that the required The amount of water is as small as necessary. As a rule, (depending on the load on the Evaporator and salinity) a rinsing time of 1 to 2 minutes sufficient. To blockages in the drain line to the collecting tank 8 avoid this line by opening the container drain valve 12 (instead of the flushing drain valve 13) flushed periodically. This is preferably done every 10 to 20 rinses.

    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.After a pre-rinse time, the rinse drain valve 13 is closed, and in further course of the rinsing phase, the water is via the drain tank 7 and the drain line through the vent line and through the vent valve 14 rinsed. Then the flushing water valve 11 is closed and around the To empty the drain container, the flushing drain valve 13 opened. The rest Flushing water is allowed to run off by opening the container drain valve 12. After that all valves are closed again.

    Durch Öffnen des Ablaufventils 10 wird der Ablaufbehälter wieder evakuiert, und der Ablaufzyclus kann erneut beginnen.By opening the drain valve 10, the drain container is evacuated again, and the cycle can begin again.

    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).In order to avoid the ingress of air, the drain lines are to Collection container and for flushing detergent with inert gas flushing (usually Nitrogen purging). Inert gas is supplied via the Inlet pipes (4; 5).

    Vorteilhaft ist eine automatisierte Ablaufsteuerung dieser Ablauf- und Spülvorgänge. An automated sequence control of this sequence and Flushing.

    Bezugszeichenliste:Reference symbol list:

    1.1.
    Zulauf in den VerdampfungsapparatInlet into the evaporator
    2.2nd
    Dampfstrom zur Beheizung des Mantels des VerdampfungsapparatesSteam flow for heating the jacket of the evaporator
    3.3rd
    Einleitungsrohr für SpülmittelInlet pipe for detergent
    4.4th
    Einleitungsrohr für InertgasInlet gas inlet pipe
    5.5.
    Einleitungsrohr für InertgasInlet gas inlet pipe
    6.6.
    SpülablaufleitungFlushing drain line
    7.7.
    AblaufbehälterDrain container
    8.8th.
    SammelbehälterCollection container
    9.9.
    Pumpepump
    10.10th
    AblaufventilDrain valve
    11.11.
    SpülwasserventilFlushing water valve
    12.12th
    BehälterablaufventilContainer drain valve
    13.13.
    SpülablaufventilFlush valve
    14.14.
    EntlüftungsventilVent valve
    15.15.
    Kopfstrom des VerdampfungsapparatesTop stream of the evaporator
    16.16.
    SumpfablaufleitungSwamp drain line
    17.17th
    aus dem Sumpf zum Ablaufventil führende Leitungline leading from the sump to the drain valve

    Claims (9)

    Spülvorrichtung zur Entfernung von Rückständen aus dem Sumpfablauf einer Kopfprodukt und Sumpfprodukt erzeugenden, mit einem Sumpfablauf ausgestatteten Verdampfungsvorrichtung, enthaltend: a) einen Ablaufbehälter (7), b) einen Sammelbehälter (8), c) ein Ablaufventil (10), d) ein Spülwasserventil (11), e) ein Behälterablaufventil (12), f) ein Spülablaufventil (13), g) ein Entlüftungsventil (14), h) eine aus dem Sumpf zum Ablaufventil (10) führende Leitung (17), i) ein Einleitungsrohr (3) für Spülmittel, j) eine Ablaufleitungs-Einrichtung (6, 16) und Verbindungsleitungen zwischen den Einrichtungen a) bis j).Flushing device for removing residues from the bottom drain of a top product and bottom product-producing evaporation device equipped with a bottom drain, comprising: a) a drain container (7), b) a collecting container (8), c) a drain valve (10), d) a flushing water valve (11), e) a container drain valve (12), f) a flushing drain valve (13), g) a vent valve (14), h) a line (17) leading from the sump to the drain valve (10), i) an inlet pipe (3) for detergent, j) a drain line device (6, 16) and connecting lines between the devices a) to j). Spülvorrichtung nach Anspruch 1, dadurch gekennzeichnet, daß der Ablaufbehälter (7) über Verbindungsleitungen unmittelbar mit dem Ablaufventil (10), dem Spülwasserventil (11), dem Behälterablaufventil (12), dem Spülablaufventil (13) und dem Entlüftungsventil (14), verbunden ist. Flushing device according to claim 1, characterized in that the Drain container (7) via connecting lines directly with the Drain valve (10), the flushing water valve (11), the container drain valve (12), the flushing drain valve (13) and the vent valve (14) is connected. Spülvorrichtung nach Anspruch 1 oder 2, dadurch gekennzeichnet, daß der Ablaufbehälter (7) oberhalb des Sammelbehälters (8) und unterhalb des Sumpfes angeordnet ist.Flushing device according to claim 1 or 2, characterized in that the Drain container (7) above the collecting container (8) and below the Swamp is arranged. Spülvorrichtung nach einem der Ansprüche 1 bis 3 dadurch gekennzeichnet, daß die Ablaufleitungs-Einrichtung (6, 16) in Form von zwei Leitungen, einer Spülablaufleitung (6) und einer Sumpfablaufleitung (16), ausgebildet ist.Flushing device according to one of claims 1 to 3, characterized in that the drain line device (6, 16) in the form of two lines, one Flush drain line (6) and a sump drain line (16) is formed. Spülvorrichtung nach einem der Ansprüche 1 bis 4, dadurch gekennzeichnet, daß ein oder mehrere Einleitungsrohre für Inertgas (4; 5) in den Ablaufbehälter (7) und/oder in den Sammelbehälter (8) und/oder in Verbindungsleitungen zwischen den Einrichtungen a) bis j ) münden.Flushing device according to one of claims 1 to 4, characterized in that that one or more inlet pipes for inert gas (4; 5) in the Drain container (7) and / or in the collecting container (8) and / or in Connection lines between the devices a) to j) open. Spülvorrichtung nach einem der Ansprüche 1 bis 5, dadurch gekennzeichnet, daß der Sammelbehälter (8) mit einer Pumpe (9) verbunden ist.Flushing device according to one of claims 1 to 5, characterized in that that the collecting container (8) is connected to a pump (9). Spülvorrichtung nach einem der Ansprüche 1 bis 6, dadurch gekennzeichnet, daß der Verdampfungsapparat ein Dünnschichtverdampfer ist.Flushing device according to one of claims 1 to 6, characterized in that that the evaporator is a thin film evaporator. Spülvorrichtung nach einem der Ansprüche 1 bis 7, dadurch gekennzeichnet, daß der Verdampfungsapparat evakuiert ist.Flushing device according to one of claims 1 to 7, characterized in that that the evaporator is evacuated. Verwendung einer Spülvorrichtung nach einem der Ansprüche 1 bis 8 für die destillative Aufarbeitung salzhaltiger Lösungen.Use of a flushing device according to one of claims 1 to 8 for the Working up saline solutions by distillation.
    EP99123942A 1998-12-03 1999-12-03 Rinsing system for removing residues Expired - Lifetime EP1005888B1 (en)

    Applications Claiming Priority (2)

    Application Number Priority Date Filing Date Title
    DE19855910A DE19855910A1 (en) 1998-12-03 1998-12-03 Rinsing device for removing residues
    DE19855910 1998-12-03

    Publications (2)

    Publication Number Publication Date
    EP1005888A1 true EP1005888A1 (en) 2000-06-07
    EP1005888B1 EP1005888B1 (en) 2005-09-14

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    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)

    * Cited by examiner, † Cited by third party
    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 (7)

    * Cited by examiner, † Cited by third party
    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
    WO2014009342A1 (en) 2012-07-11 2014-01-16 Bayer Materialscience Ag Method for working up distillation residues from isocyanate production
    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

    Citations (2)

    * Cited by examiner, † Cited by third party
    Publication number Priority date Publication date Assignee Title
    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

    Family Cites Families (5)

    * Cited by examiner, † Cited by third party
    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
    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

    Patent Citations (2)

    * Cited by examiner, † Cited by third party
    Publication number Priority date Publication date Assignee Title
    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

    Cited By (1)

    * Cited by examiner, † Cited by third party
    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

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    US6443170B1 (en) 2002-09-03
    CN1260248A (en) 2000-07-19
    ATE304395T1 (en) 2005-09-15
    CN1216697C (en) 2005-08-31
    DE19855910A1 (en) 2000-06-08
    DE59912551D1 (en) 2005-10-20
    JP2000197862A (en) 2000-07-18
    EP1005888B1 (en) 2005-09-14

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