EP1844126B1 - Method for increasing selectivity of physically active solvents during absorption of gas components from technical gases - Google Patents

Method for increasing selectivity of physically active solvents during absorption of gas components from technical gases Download PDF

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EP1844126B1
EP1844126B1 EP06700913.4A EP06700913A EP1844126B1 EP 1844126 B1 EP1844126 B1 EP 1844126B1 EP 06700913 A EP06700913 A EP 06700913A EP 1844126 B1 EP1844126 B1 EP 1844126B1
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absorption
gas
stripping column
medium
hydrocarbons
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German (de)
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EP1844126A1 (en
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Johannes Menzel
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ThyssenKrupp Industrial Solutions AG
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ThyssenKrupp Industrial Solutions AG
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    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10K—PURIFYING OR MODIFYING THE CHEMICAL COMPOSITION OF COMBUSTIBLE GASES CONTAINING CARBON MONOXIDE
    • C10K1/00—Purifying combustible gases containing carbon monoxide
    • C10K1/08—Purifying combustible gases containing carbon monoxide by washing with liquids; Reviving the used wash liquors
    • C10K1/16—Purifying combustible gases containing carbon monoxide by washing with liquids; Reviving the used wash liquors with non-aqueous liquids
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10J—PRODUCTION OF PRODUCER GAS, WATER-GAS, SYNTHESIS GAS FROM SOLID CARBONACEOUS MATERIAL, OR MIXTURES CONTAINING THESE GASES; CARBURETTING AIR OR OTHER GASES
    • C10J3/00—Production of combustible gases containing carbon monoxide from solid carbonaceous fuels
    • C10J3/72—Other features
    • C10J3/82—Gas withdrawal means

Definitions

  • the physically acting solvent also triggers value components out of the technical gas.
  • the conditions must often be set so that the amount of mitabsorb vigilant value components are hardly negligible, which is an unavoidable disadvantage of all physically acting solvent.
  • the recovery processes are used in conjunction with a corresponding absorption device.
  • Corresponding absorption devices are used for raw natural gases or synthesis gases which contain, in addition to valuable components such as methane, higher hydrocarbons, hydrogen, carbon dioxide, if desired, and carbon monoxide, impurities such as hydrogen sulphide, organic sulfur components, e.g. Mercaptan and carbon dioxide sulfide, and also carbon dioxide - where undesirable - and contained small amounts of water vapor in different proportions used.
  • the recovered compounds can either be re-added to the respective, purified technical gas or marketed as a separate product.
  • the e.g. sulfur components contained in the raw natural gas for further technical use up to ppm levels from the gas to remove.
  • the removal of hydrogen sulphide, mercaptans, carbon dioxide and other sour gas constituents from industrial gases is generally accomplished by means of chemically acting absorbents, such as e.g. Amine solutions, alkali salt solutions, etc., or physically acting absorbents, e.g. Selexol, propylene carbonate, N-methyl-pyrrolidone, Morphysorb, methanol and the like, in circulatory systems, wherein physically acting absorbents, in contrast to chemically acting detergents are able to remove organic sulfur components.
  • the carbon dioxide contained in the gas is either completely, partially or as little as possible removed.
  • the temperature of the laden absorbent coming from the absorption device is changed before being discharged into the stripping column.
  • both a temperature increase and a temperature drop is considered.
  • a device for the indirect heat exchange is selected for this purpose, which can be operated both with cooling medium and with heating medium.
  • a cooling of the loaded absorbent takes place during operation when a sharper separation efficiency of the stripping column is desired. This will be the case when it is desired to reduce the sour gas levels in the recycle gas or to reduce the hydrocarbon levels in the bottoms feed or both.
  • the cooling capacity therefore corresponds to that of a reflux condenser for the stripping columns, which can therefore be dispensed with. However, this increases the required heat output of the reboiler of the stripping column.
  • a heating of the loaded absorbent takes place during operation, when the physical absorbent has also mitabsorbed large amounts of lower hydrocarbons, so especially methane, which can easily desorb and be flashed in the head of the stripping column.
  • the increase in pressure when heated is best effected by a pump.
  • the required in the stripping column increased pressure level can also be caused by static pressure due to different installation altitude by the absorption device is higher than the stripping column and adjusts a liquid column in the liquid supply lines, which corresponds to the pressure difference, which for promoting the Recyclegases in the absorption device is sufficient.
  • Fig. 1 shows the inventive method consisting of a stripping column and the associated pumps and heat exchangers, and their interaction with an absorption column and a two-stage sour gas desorption.
  • the feed gas 1 is introduced into the bottom of the absorption column 2 and flows through it from bottom to top, being washed by regenerated, physical absorbent 3, which is abandoned from above, and freed from acid gases.
  • the clean gas 4 leaves the absorption column 2 overhead.
  • the loaded with acid gases absorbent 5, in which hydrocarbons are mitabsorbiert is withdrawn at the bottom of the absorption column 2 and brought by the booster pump 6 to an elevated pressure and, depending on the operating conditions, heated or cooled in the heat exchanger 7.
  • the changed in pressure and temperature loaded absorbent 8 is abandoned in the head of the stripping column 9. It passes through the output column equipped with packing or tray 9 from top to bottom, while the desorbed gases flow in countercurrent from bottom to top.
  • the essentially loaded only with sour gas absorbent is withdrawn at the bottom of the stripping column 9 and heated in part in the reboiler 10, which partially desorb acid gases that support the stripping in the lower part of the stripping column 9.
  • the reboiler 10 which partially desorb acid gases that support the stripping in the lower part of the stripping column 9.
  • the rich in hydrocarbons, but sour gas constituents poor recycle gas 14 is withdrawn overhead of the stripping column 9, cooled in the condenser 15 and returned to the absorption column 2.
  • the operating pressure is adjusted so that the pressure gradient between the head of the stripping column 9 and the feed point 16 of the absorption column 2 for conveying the Recycle gas 14 sufficient sufficient.
  • the choice of the feed point 16 depends on the concentration of sour gas constituents, which should be about the same at the selected task both in the absorption column 2 and in the recycle gas 14.
  • the withdrawn from the stripping column 9, loaded with sour gas absorbent 17 is further heated in the heater 18 and fed into the medium-pressure flash tank 19, where a significant pressure release takes place.
  • a first part of the desorbed sour gas 24 is released.
  • the partially desorbed absorbent 20 is then passed into the low pressure stripper 21 where further pressure release takes place and almost complete expulsion of the still absorbed acid gases 27 from the absorbent is effected by a gaseous stripping medium 22, such as CO 2 or N 2 .
  • the desorbed acid gases 23 and 24 are cooled in the sour gas coolers 25 and 26, combined as sour gas 27 and fed to a further use.
  • the complete regeneration could also take place in a desorption column without the external supply of stripping gas, the regeneration then being effected by a sump cooker which generates the necessary stripping steam.
  • the regenerated absorbent 28 is first conveyed by the feed pump 29 to the side cooker 13, where it serves for heating, and then to the cooler 30, where it is brought to the desired absorption temperature and then fed as regenerated absorbent 3 to the top of the absorption column 2. If further heat consumers can be served, even more heat utilization is possible, for example, the bottom reboiler 10 and the heat exchanger 7 can be supplied with waste heat.
  • the absorption medium was a mixture of n-formylmorpholine and n-acetylmorpholine selected according to the use of the Morphysorb method.
  • Table 1 electricity temperature print methane H 2 S sour gas Hydrocarbons C2 + Other (CO 2 , N 2 , etc.) absorbents [° C] [bar] [Kmol / h] [Kmol / h] [Kmol / h] [Kmol / h] [Kmol / h] [Kmol / h] 1 50 67.5 5470 1944 2004 580 - 4 16 67 5470 0.02 1987 543 - 5 60 67 300 2321 623 238 4719 8th 85 70 300 2321 623 238 4719 14 92 68 300 376 608 189 - 17 184 68 - 1944 15.7 49 4718 22 100 10 - - - 300 - 27 50 5 - 1944 15.7 338 - 28 174 5 - 0,003 - - 4718
  • the hydrocarbon losses are reduced by a factor of 10 with the process according to the invention, which is an advantage of the process according to the invention.
  • the process according to the invention results in a gain of about 100 MW of thermal power, which would otherwise be lost with the sour gas after the conventional procedure (recycle flash).
  • a recycle compressor of about 3.5 MW of electrical power is required for the conventional procedure, which is completely eliminated by the novel procedure.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Combustion & Propulsion (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Gas Separation By Absorption (AREA)

Description

Die Erfindung betrifft ein Verfahren zur Erhöhung der Selektivität von physikalisch wirkenden Lösungsmitteln bei einer Absorption von Gaskomponenten aus technischen Gasen. Beispiele für derartige Absorptionen sind:

  • die Absorption von Sauergasen aus rohem Erdgas,
  • die Absorption von Sauergasen aus rohem Synthesegas,
  • die Absorption von Kohlendioxid aus Erdgas,
  • die Absorption von Kohlendioxid aus Synthesegas,
  • die Absorption von Ammoniak.
The invention relates to a method for increasing the selectivity of physically acting solvents in an absorption of gas components from industrial gases. Examples of such absorptions are:
  • the absorption of acid gases from crude natural gas,
  • the absorption of acid gases from crude synthesis gas,
  • the absorption of carbon dioxide from natural gas,
  • the absorption of carbon dioxide from synthesis gas,
  • the absorption of ammonia.

In den meisten Fällen löst das physikalisch wirkende Lösungsmittel jedoch auch Wertkomponenten aus dem technischen Gas heraus. Insbesondere bei hohen Anforderungen an die Endreinheit des gewünschten technischen Gases hinsichtlich der auszusondernden Komponenten müssen die Bedingungen oft derart eingestellt werden, dass die Menge der mitabsorbierten Wertkomponenten kaum mehr vernachlässigbar sind, was ein unvermeidbarer Nachteil aller physikalisch wirkenden Lösungsmittel ist.In most cases, however, the physically acting solvent also triggers value components out of the technical gas. Especially with high demands on the final purity of the desired technical gas in terms of auszusondernden components, the conditions must often be set so that the amount of mitabsorbierten value components are hardly negligible, which is an unavoidable disadvantage of all physically acting solvent.

Diese Wertkomponenten werden daher üblicherweise noch vor der Regeneration des physikalisch wirkenden Lösungsmittels in aufwändiger Weise zurückgewonnen. Beispiele für derartige Rückgewinnungsmaßnahmen nach dem Stand der Technik sind:

  • Rückgewinnung von Kohlendioxid,
  • Rückgewinnung von Kohlenwasserstoffverbindungen und Wasserstoff.
These value components are therefore usually recovered before the regeneration of the physically acting solvent in a complex manner. Examples of such prior art recovery measures are:
  • Recovery of carbon dioxide,
  • Recovery of hydrocarbon compounds and hydrogen.

Die Verfahren zur Rückgewinnung werden im Verbund mit einer entsprechenden Absorptionsvorrichtung eingesetzt. Entsprechende Absorptionsvorrichtungen werden für rohe Erdgase oder Synthesegase, die neben Wertstoffkomponenten wie Methan, höheren Kohlenwasserstoffen, Wasserstoff, Kohlendioxid - soweit erwünscht - und Kohlenmonoxid Verunreinigungen wie Schwefelwasserstoff, organische Schwefelkomponenten, wie z.B. Merkaptane und Kohlenoxidsulfid, ferner auch Kohlendioxid - soweit unerwünscht - und geringe Mengen an Wasserdampf in unterschiedlichen Anteilen enthalten, genutzt. Die zurückgewonnenen Verbindungen können entweder dem jeweiligen, gereinigten technischen Gas wieder zugesetzt oder als eigenes Produkt weitervermarktet werden.The recovery processes are used in conjunction with a corresponding absorption device. Corresponding absorption devices are used for raw natural gases or synthesis gases which contain, in addition to valuable components such as methane, higher hydrocarbons, hydrogen, carbon dioxide, if desired, and carbon monoxide, impurities such as hydrogen sulphide, organic sulfur components, e.g. Mercaptan and carbon dioxide sulfide, and also carbon dioxide - where undesirable - and contained small amounts of water vapor in different proportions used. The recovered compounds can either be re-added to the respective, purified technical gas or marketed as a separate product.

Zum Beispiel offenbart US2813126 ein Verfahren zur Rückgewinnung von Kohlenwasserstoffverbindungen, die bei der Absorption von Sauergasen aus Erdgas mittels physikalisch wirkender Absorptionsmittel mitabsorbiert werden.For example, disclosed US2813126 a process for the recovery of hydrocarbon compounds, which are absorbed in the absorption of acid gases from natural gas by means of physically acting absorbents.

In der Regel ist es notwendig, die z.B. im rohen Erdgas enthaltenen Schwefelkomponenten für die weitere technische Nutzung bis auf ppm-Gehalte aus dem Gas zu entfernen. Die Entfernung von Schwefelwasserstoff, Merkaptanen, Kohlendioxid und sonstigen Sauergasbestandteilen aus technischen Gasen erfolgt im allgemeinen mittels chemisch wirkender Absorptionsmittel, wie z.B. Aminlösungen, Alkalisalzlösungen etc. oder physikalisch wirkender Absorptionsmittel wie z.B. Selexol, Propylencarbonat, N-Methyl-Pyrrolidon, Morphysorb, Methanol u.a., in Kreislaufsystemen, wobei physikalisch wirkende Absorptionsmittel im Gegensatz zu chemisch wirkenden Waschmitteln in der Lage sind, auch organische Schwefelkomponenten zu entfernen. Das im Gas enthaltene Kohlendioxid wird dabei je nach Zielsetzung und Aufgabenstellung entweder ganz, zum Teil oder auch so wenig wie möglich entfernt.In general, it is necessary to use the e.g. sulfur components contained in the raw natural gas for further technical use up to ppm levels from the gas to remove. The removal of hydrogen sulphide, mercaptans, carbon dioxide and other sour gas constituents from industrial gases is generally accomplished by means of chemically acting absorbents, such as e.g. Amine solutions, alkali salt solutions, etc., or physically acting absorbents, e.g. Selexol, propylene carbonate, N-methyl-pyrrolidone, Morphysorb, methanol and the like, in circulatory systems, wherein physically acting absorbents, in contrast to chemically acting detergents are able to remove organic sulfur components. Depending on the objectives and the task, the carbon dioxide contained in the gas is either completely, partially or as little as possible removed.

Da physikalisch wirkende Absorptionsmittel bei der Entfernung von Sauergaskomponenten aus technischen Gasen in der Regel auch einen Anteil an Kohlenwasserstoffen mit absorbieren, wird in der Regel die den Absorber verlassende Lösung vor der Desorption der Sauergase in einem Recycleflashbehälter auf einen gegenüber der Absorption niedrigeren Druck entspannt, wobei das dort frei werdende Flashgas mittels eines Recyclekompressors rückverdichtet und als Recyclegas zur erneuten Reinigung dem Einsatzgas vor der Absorptionsstufe beigemischt wird. Problematisch ist hierbei aber eine Eigenschaft aller höheren Kohlenwasserstoffe bei physikalischen Absorptionsmitteln: Deren Löslichkeit im Absorptionsmittel steigt mit der Anzahl der Kohlenstoffatome.Since physically acting absorbents in the removal of sour gas components from technical gases usually also absorb a proportion of hydrocarbons, the solution leaving the absorber is usually relieved before the desorption of the acid gases in a Recycleflashbehälter to a lower pressure compared to the absorption, the flash gas released there is recompressed by means of a recycle compressor and admixed as recycle gas for re-purification of the feed gas before the absorption stage. However, the problem here is a property of all higher hydrocarbons in physical absorbents: their solubility in the absorbent increases with the number of carbon atoms.

Dies bedeutet, dass bei einer einfachen Flashstufe leichte Kohlenwasserstoffe tendenziell leicht und höhere Kohlenwasserstoffe tendenziell schwierig aus dem Absorptionsmittel durch Flashen entfernt werden können. Sollen also auch die höheren Kohlenwasserstoffe vor der eigentlichen Regeneration des Absorptionsmittels zurückgewonnen werden, müssen eventuell mehrere Flashstufen und sehr große Druckabsenkungen vorgenommen werden, wobei dann aber auch größere Mengen der Sauergase vorzeitig desorbieren und ebenfalls rückverdichtet werden müssen. Die Problematik stellt sich besonders, wenn, etwa bei der Reinigung von rohem Erdgas, das geförderte Gas neben einem hohen Sauergasanteil auch einen besonders hohen Anteil an Ethan, Propan sowie weiteren höheren Kohlenwasserstoffen aufweist.This means that in a simple flash stage, light hydrocarbons tend to be light and higher hydrocarbons tend to be difficult to remove from the absorbent by flashing. Thus, if the higher hydrocarbons are to be recovered before the actual regeneration of the absorbent, several flash stages and very large pressure drops may need to be made, but then also larger amounts of acid gases must desorb prematurely and must also be recompressed. The problem arises especially when, for example, in the purification of raw natural gas, the extracted gas in addition to a high proportion of sour gas also has a particularly high proportion of ethane, propane and other higher hydrocarbons.

Nachteilig ist daher für die Auslegung in einem solchen Fall, dass

  • ein aufwändiges Flashstufensystem mit großen Druckabsenkungen vor der eigentlichen Regeneration des Absorptionsmittels vorgesehen werden muss,
  • ein teuerer Recyclegaskompressor installiert und wegen der größeren Gasmengen und der größeren Druckdifferenz mit erheblichem Energieaufwand betrieben werden muss, und
  • die Absorptionsvorrichtung wegen des rückverdichteten Recyclegases sowohl hinsichtlich der zwangsläufig mitgeflashten Sauergase als auch hinsichtlich des Gasvolumens um den Betrag des zurückgeführten Volumens vergrößert ausgelegt werden muss.
A disadvantage, therefore, for the interpretation in such a case that
  • a complex flash stage system with large pressure drops must be provided before the actual regeneration of the absorbent,
  • a costly Recyclegaskompressor installed and must be operated because of the larger gas volumes and the larger pressure difference with considerable energy expenditure, and
  • because of the recompressed recycle gas, the absorption device has to be designed to be enlarged by the amount of recirculated volume, both with regard to the inevitably flickered acid gases and with respect to the gas volume.

Der Erfindung liegt daher die Aufgabe zugrunde, ein Verfahren zur Rückgewinnung von Kohlenwasserstoffverbindungen, die bei der Absorption von Sauergasen aus technischen Gasen, wie z.B. Erdgas, mittels physikalisch wirkender Absorptionsmittel mitabsorbiert werden, zur Verfügung zu stellen, welches

  • starke Druckabsenkungen unter den Absorptionsdruck vermeidet,
  • nach Möglichkeit ohne Recyclegaskompressor auskommt, und
  • nur so wenig wie möglich verunreinigtes Recyclegas zur Absorption zurückleitet, so dass keine Vergrößerung der Absorptionsvorrichtung notwendig wird.
The invention is therefore based on the object, a process for the recovery of hydrocarbon compounds, which are mitabsorbiert in the absorption of acid gases from industrial gases, such as natural gas, by means of physically acting absorbent available, which
  • avoids high pressure drops below the absorption pressure,
  • if possible manages without Recyclegaskompressor, and
  • recycled as little as possible contaminated recycle gas for absorption, so that no enlargement of the absorption device is necessary.

Die Erfindung löst die Aufgabe dadurch, dass

  • zuerst der Druck des aus der Absorptionseinrichtung abgezogenen, beladenen Absorptionsmittels erhöht wird,
  • dann das beladene Absorptionsmittel auf den Kopf einer Abtriebskolonne gegeben wird, welche einen Sumpfaufkocher aufweist und einen oder mehrere Seitenaufkocher aufweisen kann, sowie unter einem geringfügig höheren Druck als die Absorptionskolonne betrieben wird,
  • in dieser Abtriebskolonne mittels des Zusammenspiels von Sumpfkocher und Aufgabetemperatur ein Gleichgewicht derart eingestellt wird, dass die Sauergaskonzentration im Absorptionsmittel zum Sumpf hin zunimmt und die Konzentration der Kohlenwasserstoffe zum Sumpf hin abnimmt,
  • ein erhitztes, an Kohlenwasserstoffen armes und an Sauergaskomponenten reiches Absorptionsmittel am Sumpf abgezogen und einer Sauergasdesorptionseinrichtung zugeführt wird,
  • ein an Kohlenwasserstoffen reiches und an Sauergaskomponenten armes Recyclegas am Kopf der Abtriebskolonne abgezogen wird, und
  • das Recyclegas in einem Recyclegas-Kühler auf etwa die Temperatur des Einsatzgases, welches in die Absorptionseinrichtung geleitet wird, abgekühlt und entweder direkt in die Absorptionsvorrichtung gegeben oder dem Einsatzgas beigemischt wird.
Als arm an Sauergaskomponenten im Sinne der Erfindung ist das Recyclegas, welches am Kopf der Abtriebskolonne abgezogen wird, dann anzusehen, wenn der Sauergasgehalt weniger als 50 % beträgt.The invention solves the problem in that
  • first the pressure of the loaded absorbent withdrawn from the absorber is increased,
  • then loading the loaded absorbent on the top of a stripping column having a bottom reboiler and having one or more side reboilers, and operating at a slightly higher pressure than the absorption column,
  • in this stripping column by means of the interaction of sump cooker and application temperature, an equilibrium is set such that the sour gas concentration in the absorbent increases toward the sump and the concentration of the hydrocarbons decreases towards the sump,
  • withdrawn a heated absorbent poor in hydrocarbons and rich in acid gas components at the bottom and fed to an acid gas desorption device,
  • a rich in hydrocarbons and sour gas components poor recycle gas is withdrawn at the top of the stripping column, and
  • the recycle gas in a recycle gas cooler is cooled to about the temperature of the feed gas passed into the absorber, and either added directly to the absorber or admixed with the feed gas.
As low acid components in the sense of the invention is the recycle gas, which is withdrawn at the top of the stripping column, to be considered when the sour gas content is less than 50%.

Gegenüber einer Lösung nach dem herkömmlichen Stand der Technik mit Flashstufen und Recyclegaskompressor ergibt sich darüber hinaus der Vorteil, dass wesentlich mehr Kohlenwasserstoffe zurückgewonnen werden können als bisher überhaupt möglich ist.Compared to a solution according to the conventional state of the art with flash stages and Recyclegaskompressor also results in the advantage that significantly more hydrocarbons can be recovered than previously possible.

In einer Ausgestaltung des erfindungsgemäßen Verfahrens wird die Temperatur des aus der Absorptionsvorrichtung kommenden, beladenen Absorptionsmittels vor Aufgabe in die Abtriebskolonne geändert. Hierbei kommt sowohl eine Temperaturerhöhung als auch eine Temperaturabsenkung in Betracht. Zweckmäßigerweise wird hierfür eine Vorrichtung für den indirekten Wärmetausch gewählt, die sowohl mit Kühlmedium als auch mit Heizmedium betrieben werden kann.In one embodiment of the method according to the invention, the temperature of the laden absorbent coming from the absorption device is changed before being discharged into the stripping column. In this case, both a temperature increase and a temperature drop is considered. Conveniently, a device for the indirect heat exchange is selected for this purpose, which can be operated both with cooling medium and with heating medium.

Eine Kühlung des beladenen Absorptionsmittels erfolgt während des Betriebs dann, wenn eine schärfere Trennleistung der Abtriebskolonne gewünscht wird. Dies wird dann der Fall sein, wenn eine Verringerung der Sauergasanteile im Recyclegas oder eine Verringerung der Kohlenwasserstoffanteile im Sumpfabzug oder beides gewünscht wird. Die Kühlleistung entspricht daher der eines Rückflusskühlers für die Abtriebskolonnen, auf den daher verzichtet werden kann. Allerdings erhöht sich auf diese Weise auch die erforderliche Wärmeleistung der Aufkocher der Abtriebskolonne.A cooling of the loaded absorbent takes place during operation when a sharper separation efficiency of the stripping column is desired. This will be the case when it is desired to reduce the sour gas levels in the recycle gas or to reduce the hydrocarbon levels in the bottoms feed or both. The cooling capacity therefore corresponds to that of a reflux condenser for the stripping columns, which can therefore be dispensed with. However, this increases the required heat output of the reboiler of the stripping column.

Eine Erwärmung des beladenen Absorptionsmittels erfolgt während des Betriebs dann, wenn das physikalische Absorptionsmittel auch große Mengen von niedrigeren Kohlenwasserstoffen, also vor allem Methan, mitabsorbiert hat, welche leicht desorbieren und im Kopf der Abtriebskolonne geflasht werden können.A heating of the loaded absorbent takes place during operation, when the physical absorbent has also mitabsorbed large amounts of lower hydrocarbons, so especially methane, which can easily desorb and be flashed in the head of the stripping column.

Die Druckerhöhung bei Erwärmung wird am besten durch eine Pumpe bewirkt. Für den Betrieb ohne Erwärmung kann das in der Abtriebskolonne erforderliche erhöhte Druckniveau auch durch statischen Druck aufgrund von unterschiedlicher Aufstellungshöhe bewirkt werden, indem die Absorptionsvorrichtung höher steht als die Abtriebskolonne und sich in den Flüssigkeitszuleitungen eine Flüssigkeitssäule einstellt, die dem Druckunterschied entspricht, welcher zur Förderung des Recyclegases in die Absorptionsvorrichtung ausreicht.The increase in pressure when heated is best effected by a pump. For operation without heating, the required in the stripping column increased pressure level can also be caused by static pressure due to different installation altitude by the absorption device is higher than the stripping column and adjusts a liquid column in the liquid supply lines, which corresponds to the pressure difference, which for promoting the Recyclegases in the absorption device is sufficient.

Sofern man mit dem erfindungsgemäßen Verfahren solche Kohlenwasserstoffe, die aus rohem Erdgas absorbiert wurden, zurückgewinnen will, erhält man auf diese Weise auch eine Möglichkeit und einen Freiheitsgrad, um bei zeitlich wechselnden, absorbierten Gasanteilen das jeweilige wirtschaftliche Optimum an Rückgewinnung einzustellen, was ein weiterer Vorteil des Verfahrens ist.If you want to recover with the inventive method, such hydrocarbons that were absorbed from crude natural gas, you get in this way also a way and a degree of freedom to adjust the respective economic optimum at recovery with time-varying, absorbed gas shares, which is another advantage of the method.

Die Erfindung wird nachfolgend anhand eines Verfahrensschemas in Fig. 1 näher erläutert: Fig. 1 zeigt das erfindungsgemäße Verfahren, bestehend aus einer Abtriebskolonne und den zugehörigen Pumpen und Wärmetauschern, sowie ihr Zusammenwirken mit einer Absorptionskolonne und einer zweistufigen Sauergas-Desorptionsvorrichtung.The invention is described below with reference to a process scheme in Fig. 1 explained in more detail: Fig. 1 shows the inventive method consisting of a stripping column and the associated pumps and heat exchangers, and their interaction with an absorption column and a two-stage sour gas desorption.

Das Einsatzgas 1 wird unten in die Absorptionskolonne 2 eingeleitet und durchströmt diese von unten nach oben, wobei es von regeneriertem, physikalischen Absorptionsmittel 3, welches von oben aufgeben wird, gewaschen und von Sauergasen befreit wird. Das Reingas 4 verlässt die Absorptionskolonne 2 über Kopf.The feed gas 1 is introduced into the bottom of the absorption column 2 and flows through it from bottom to top, being washed by regenerated, physical absorbent 3, which is abandoned from above, and freed from acid gases. The clean gas 4 leaves the absorption column 2 overhead.

Das mit Sauergasen beladene Absorptionsmittel 5, in welchem auch Kohlenwasserstoffe mitabsorbiert sind, wird am Sumpf der Absorptionskolonne 2 abgezogen und mittels der Druckerhöhungspumpe 6 auf einen erhöhten Druck gebracht und, je nach Betriebsfall, im Wärmetauscher 7 erwärmt bzw. gekühlt. Das in Druck und Temperatur geänderte beladene Absorptionsmittel 8 wird im Kopf der Abtriebskolonne 9 aufgegeben. Es durchläuft die mit Packungen oder Böden ausgestattete Abtriebskolonne 9 von oben nach unten, während die desorbierten Gase im Gegenstrom von unten nach oben strömen.The loaded with acid gases absorbent 5, in which hydrocarbons are mitabsorbiert is withdrawn at the bottom of the absorption column 2 and brought by the booster pump 6 to an elevated pressure and, depending on the operating conditions, heated or cooled in the heat exchanger 7. The changed in pressure and temperature loaded absorbent 8 is abandoned in the head of the stripping column 9. It passes through the output column equipped with packing or tray 9 from top to bottom, while the desorbed gases flow in countercurrent from bottom to top.

Das im wesentlichen nur noch mit Sauergas beladene Absorptionsmittel wird am Sumpf der Abtriebskolonne 9 abgezogen und zum Teil im Aufkocher 10 erwärmt, wobei zum Teil Sauergase desorbieren, die die Strippwirkung im unteren Bereich der Abtriebskolonne 9 unterstützen. Um diese Desorption der Sauergase energetisch günstig zu gestalten, ist es zweckmäßig, nicht die ganze benötigte Wärme im Sumpfaufkocher zuzuführen, sondern über einen oder mehrere Seitenkocher, die ihre Energie über den Wärmetausch mit der vom Desorber kommenden heißen, regenerierten Lösung beziehen. Daher wird im mittleren Bereich der Abtriebskolonne ein Seitenabzug 11 vorgesehen, der das beladene Absorptionsmittel mittels der Seitenabzugspumpe 12 in den Seitenkocher 13 und wieder zurück in die Abtriebskolonne 9 fördert.The essentially loaded only with sour gas absorbent is withdrawn at the bottom of the stripping column 9 and heated in part in the reboiler 10, which partially desorb acid gases that support the stripping in the lower part of the stripping column 9. In order to make this desorption of acid gases energetically favorable, it is expedient not to supply all the heat needed in Sumpfaufkocher, but via one or more side cookers that relate their energy through the heat exchange with the hot, regenerated solution coming from the desorber. Therefore, a side take-off 11 is provided in the central region of the stripping column, which conveys the laden absorbent by means of the Seitenabzugspumpe 12 in the side cooker 13 and back into the stripping column 9.

Das an Kohlenwasserstoffen reiche, aber an Sauergasbestandteilen arme Recyclegas 14 wird über Kopf der Abtriebskolonne 9 abgezogen, im Kühler 15 gekühlt und in die Absorptionskolonne 2 zurückgeführt. Hierbei wird in der Abtriebskolonne 9 der Betriebsdruck so eingestellt, dass das Druckgefälle zwischen dem Kopf der Abtriebskolonne 9 und der Aufgabestelle 16 der Absorptionskolonne 2 zur Förderung des Recyclegases 14 sicher ausreicht. Die Wahl der Aufgabestelle 16 richtet sich dabei nach der Konzentration der Sauergasbestandteile, die am gewählten Aufgabeort sowohl in der Absorptionskolonne 2 als auch im Recyclegas 14 etwa die gleiche sein sollte.The rich in hydrocarbons, but sour gas constituents poor recycle gas 14 is withdrawn overhead of the stripping column 9, cooled in the condenser 15 and returned to the absorption column 2. Here, in the stripping column 9, the operating pressure is adjusted so that the pressure gradient between the head of the stripping column 9 and the feed point 16 of the absorption column 2 for conveying the Recycle gas 14 sufficient sufficient. The choice of the feed point 16 depends on the concentration of sour gas constituents, which should be about the same at the selected task both in the absorption column 2 and in the recycle gas 14.

Das aus der Abtriebskolonne 9 abgezogene, mit Sauergas beladene Absorptionsmittel 17 wird im Erhitzer 18 weiter erwärmt und in den Mitteldruck-Flashbehälter 19 geführt, wo eine erhebliche Druckentspannung stattfindet. Hierbei wird ein erster Teil des desorbierten Sauergases 24 frei. Das teildesorbierte Absorptionsmittel 20 wird hiernach in den Niederdruck-Stripper 21 geleitet, wo eine weitere Druckentspannung stattfindet und das nahezu vollständige Austreiben der noch absorbierten Sauergase 27 aus dem Absorptionsmittel durch ein gasförmiges Strippmedium 22, etwa CO2 oder N2, bewirkt wird. Die desorbierten Sauergase 23 und 24 werden in den Sauergaskühlern 25 und 26 gekühlt, als Sauergas 27 zusammengefasst und einer weiteren Verwendung zugeführt. Alternativ könnte die vollständige Regeneration auch in einer Desorptionskolonne ohne die externe Zufuhr von Strippgas erfolgen, wobei die Regeneration dann durch einen Sumpfkocher erfolgen würde, der den notwendigen Strippdampf erzeugt.The withdrawn from the stripping column 9, loaded with sour gas absorbent 17 is further heated in the heater 18 and fed into the medium-pressure flash tank 19, where a significant pressure release takes place. In this case, a first part of the desorbed sour gas 24 is released. The partially desorbed absorbent 20 is then passed into the low pressure stripper 21 where further pressure release takes place and almost complete expulsion of the still absorbed acid gases 27 from the absorbent is effected by a gaseous stripping medium 22, such as CO 2 or N 2 . The desorbed acid gases 23 and 24 are cooled in the sour gas coolers 25 and 26, combined as sour gas 27 and fed to a further use. Alternatively, the complete regeneration could also take place in a desorption column without the external supply of stripping gas, the regeneration then being effected by a sump cooker which generates the necessary stripping steam.

Das regenerierte Absorptionsmittel 28 wird von der Förderpumpe 29 zunächst zum Seitenkocher 13 gefördert, wo es der Beheizung dient, und anschließend zum Kühler 30, wo es auf die gewünschte Absorptionstemperatur gebracht wird und dann als regeneriertes Absorptionsmittel 3 auf den Kopf der Absorptionskolonne 2 aufgegeben wird. Sofern weitere Wärmeverbraucher bedient werden können, sind auch weitergehende Wärmenutzungen möglich, beispielsweise können auch der Sumpfaufkocher 10 und der Wärmetauscher 7 mit Abwärme versorgt werden.The regenerated absorbent 28 is first conveyed by the feed pump 29 to the side cooker 13, where it serves for heating, and then to the cooler 30, where it is brought to the desired absorption temperature and then fed as regenerated absorbent 3 to the top of the absorption column 2. If further heat consumers can be served, even more heat utilization is possible, for example, the bottom reboiler 10 and the heat exchanger 7 can be supplied with waste heat.

Zur besseren Verdeutlichung der Vorteile dient folgendes Auslegungs-Rechenbeispiel, welches in Tabelle 1 tabellarisch dargestellt ist, wobei die Ziffern denen in Fig. 1 entsprechen. Als Absorptionsmedium wurde eine Mischung aus n-Formylmorpholin und n-Acetylmorpholin entsprechend der Verwendung nach dem Morphysorb-Verfahren gewählt. Tabelle 1: Strom Temperatur Druck Methan H2S Sauer gas Kohlenwasserstoffe C2+ Sonstige (CO2, N2, etc.) Absorptionsmittel [°C] [bar] [kmol/h] [kmol/h] [kmol/h] [kmol/h] [kmol/h] 1 50 67,5 5470 1944 2004 580 - 4 16 67 5470 0,02 1987 543 - 5 60 67 300 2321 623 238 4719 8 85 70 300 2321 623 238 4719 14 92 68 300 376 608 189 - 17 184 68 - 1944 15,7 49 4718 22 100 10 - - - 300 - 27 50 5 - 1944 15,7 338 - 28 174 5 - 0,003 - - 4718 To better illustrate the advantages of the following design calculation example, which is tabulated in Table 1, where the numbers in those in Fig. 1 correspond. The absorption medium was a mixture of n-formylmorpholine and n-acetylmorpholine selected according to the use of the Morphysorb method. Table 1: electricity temperature print methane H 2 S sour gas Hydrocarbons C2 + Other (CO 2 , N 2 , etc.) absorbents [° C] [bar] [Kmol / h] [Kmol / h] [Kmol / h] [Kmol / h] [Kmol / h] 1 50 67.5 5470 1944 2004 580 - 4 16 67 5470 0.02 1987 543 - 5 60 67 300 2321 623 238 4719 8th 85 70 300 2321 623 238 4719 14 92 68 300 376 608 189 - 17 184 68 - 1944 15.7 49 4718 22 100 10 - - - 300 - 27 50 5 - 1944 15.7 338 - 28 174 5 - 0,003 - - 4718

In einem Vergleichsbeispiel wurde auch eine Anlage herkömmlicher Art berechnet. In der folgenden Tabelle 2 werden die Ströme 14 und 27 des oben beschriebenen Rechenbeispiels mit denen des Vergleichsbeispiels (in Tabelle 2 mit V bezeichnet) gegenübergestellt. Tabelle 2: Strom Temperatur Druck Methan H2S Sauer gas Kohlenwasserstoffe C2+ Sonstige (CO2, N2, etc.) Absorptionsmittel [°C] [bar] [kmol/h] [kmol/h] [kmol/h] [kmol/h] [kmol/h] 14 92 68 300 376 608 189 - 14 V 45 9 317 900 458 196 - 27 50 5 - 1944 15,7 338 - 27 V 50 5 10 1944 167 361 - In a comparative example, a plant of conventional type was also calculated. In the following Table 2, the currents 14 and 27 of the above-described calculation example are compared with those of the comparative example (denoted by V in Table 2). Table 2: electricity temperature print methane H 2 S sour gas Hydrocarbons C2 + Other (CO 2 , N 2 , etc.) absorbents [° C] [bar] [Kmol / h] [Kmol / h] [Kmol / h] [Kmol / h] [Kmol / h] 14 92 68 300 376 608 189 - 14 v 45 9 317 900 458 196 - 27 50 5 - 1944 15.7 338 - 27 v 50 5 10 1944 167 361 -

Wie man sieht, verringern sich mit dem erfindungsgemäßen Verfahren die Kohlenwasserstoffverluste um den Faktor 10, was ein Vorteil des erfindungsgemäßen Verfahrens ist. Für das hier angeführte Beispiel ergibt sich ein Gewinn von ca. 100 MW an thermischer Leistung, der nach der konventionellen Verfahrensweise (Recycleflash) ansonsten mit dem Sauergas verloren gehen würde. Des weiteren wird für die konventionelle Verfahrensweise ein Recyclekompressor von ca. 3,5 MW elektrischer Leistung benötigt, der nach der erfindungsgemäßen Verfahrensweise ganz entfällt.As can be seen, the hydrocarbon losses are reduced by a factor of 10 with the process according to the invention, which is an advantage of the process according to the invention. For the example given here results in a gain of about 100 MW of thermal power, which would otherwise be lost with the sour gas after the conventional procedure (recycle flash). Furthermore, a recycle compressor of about 3.5 MW of electrical power is required for the conventional procedure, which is completely eliminated by the novel procedure.

BezugszeichenlisteLIST OF REFERENCE NUMBERS

11
Einsatzgasfeed gas
22
Absorptionskolonneabsorption column
33
regeneriertes Absorptionsmittelregenerated absorbent
44
Reingasclean gas
55
beladenes Absorptionsmittelloaded absorbent
66
DruckerhöhungspumpeBooster pump
77
Wärmetauscherheat exchangers
88th
beladenes Absorptionsmittelloaded absorbent
99
Abtriebskolonnestripping column
1010
Aufkocherreboiler
1111
Seitenabzugside draw
1212
SeitenabzugspumpeSide draw pump
1313
Seitenkocherside Burner
1414
Recyclegasrecycle
1515
Kühlercooler
1616
Aufgabestelleapplication site
1717
beladenes Absorptionsmittelloaded absorbent
1818
Erhitzerheaters
1919
Mitteldruck-FlashbehälterMedium pressure flash vessel
2020
teildesorbiertes Absorptionsmittelpartially absorbed absorbent
2121
Niederdruck-StripperLow pressure stripper
2222
Strippmediumstripping
2323
desorbiertes Sauergasdesorbed sour gas
2424
desorbiertes Sauergasdesorbed sour gas
2525
SauergaskühlerSour gas cooler
2626
SauergaskühlerSour gas cooler
2727
Sauergassour gas
2828
regeneriertes Absorptionsmittelregenerated absorbent
2929
Förderpumpefeed pump
3030
Kühlercooler

Claims (3)

  1. Process for recovering hydrocarbon compounds co-absorbed in the absorption of acid gases from industrial gases, for example natural gas, by physical absorption media,
    characterized in that
    • first the pressure of the laden absorption medium withdrawn from the absorption device is increased,
    • then the laden absorption medium is applied to the top of a stripping column which comprises a bottom boiler and may comprise one or more side boilers and is operated at a slightly higher pressure than the absorption column,
    • in this stripping column an equilibrium is established such that the acid gas concentration in the absorption medium increases towards the bottom and the concentration of the hydrocarbons decreases towards the bottom,
    • a heated absorption medium poor in hydrocarbons and rich in acid gas components is withdrawn at the bottom and supplied to an acid gas desorption apparatus,
    • a recycle gas rich in hydrocarbons and poor in acid gas components is withdrawn at the top of the stripping column and
    • the recycle gas is cooled in a recycle gas cooler to approximately the temperature of the input gas passed into the absorption device and either conducted directly into the absorption apparatus or admixed with the input gas.
  2. Process according to Claim 1, characterized in that the temperature of the laden absorption medium arriving from the absorption apparatus is changed before application into the stripping column.
  3. Use according to Claim 2, characterized in that an apparatus for indirect heat exchange is provided which may be operated either with cooling medium or with heating medium.
EP06700913.4A 2005-02-02 2006-01-12 Method for increasing selectivity of physically active solvents during absorption of gas components from technical gases Active EP1844126B1 (en)

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DE102005004948A DE102005004948B3 (en) 2005-02-02 2005-02-02 Hydrocarbon recovery, using absorbents, comprises increasing pressure of absorbents, loading absorbents into a drift column, heating hydrocarbon poor and acid gas rich component, drawing-off hydrocarbon rich and acid gas poor component
PCT/EP2006/000208 WO2006081921A1 (en) 2005-02-02 2006-01-12 Method for increasing physically active solvents while absorbing gas components from technical gases

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JP4803470B2 (en) * 2009-10-05 2011-10-26 独立行政法人産業技術総合研究所 Heat exchange type distillation equipment
US8673135B2 (en) * 2010-05-28 2014-03-18 Axens Coal liquefaction complex with minimal carbon dioxide emissions
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DE102011108308A1 (en) 2011-07-25 2013-01-31 Thyssenkrupp Uhde Gmbh Heat recovery in absorption and desorption processes with reduced heat exchange surface
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JP5956772B2 (en) * 2012-02-20 2016-07-27 東洋エンジニアリング株式会社 Heat exchange type distillation equipment
JP5923335B2 (en) * 2012-02-24 2016-05-24 東洋エンジニアリング株式会社 Heat exchange type distillation equipment
JP5923367B2 (en) * 2012-03-30 2016-05-24 東洋エンジニアリング株式会社 Heat exchange type distillation equipment
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