EP0783031A1 - Verfahren zur Entfernung von Wasser, Saüren und Benzin aus Erdgas, unter Verwendung eines Lösungsmittelgemisches - Google Patents

Verfahren zur Entfernung von Wasser, Saüren und Benzin aus Erdgas, unter Verwendung eines Lösungsmittelgemisches Download PDF

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Publication number
EP0783031A1
EP0783031A1 EP96402909A EP96402909A EP0783031A1 EP 0783031 A1 EP0783031 A1 EP 0783031A1 EP 96402909 A EP96402909 A EP 96402909A EP 96402909 A EP96402909 A EP 96402909A EP 0783031 A1 EP0783031 A1 EP 0783031A1
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European Patent Office
Prior art keywords
mixture
gas
methanol
solvents
column
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EP96402909A
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English (en)
French (fr)
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EP0783031B1 (de
Inventor
Alexandre Rojey
Etienne Lebas
Joseph Larue
Ari Minkkinen
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IFP Energies Nouvelles IFPEN
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IFP Energies Nouvelles IFPEN
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    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G OR C10K; LIQUIFIED PETROLEUM GAS; USE OF ADDITIVES TO FUELS OR FIRES; FIRE-LIGHTERS
    • C10L3/00—Gaseous fuels; Natural gas; Synthetic natural gas obtained by processes not covered by subclass C10G, C10K; Liquefied petroleum gas
    • C10L3/06—Natural gas; Synthetic natural gas obtained by processes not covered by C10G, C10K3/02 or C10K3/04
    • C10L3/10—Working-up natural gas or synthetic natural gas
    • C10L3/101—Removal of contaminants
    • C10L3/102—Removal of contaminants of acid contaminants
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G OR C10K; LIQUIFIED PETROLEUM GAS; USE OF ADDITIVES TO FUELS OR FIRES; FIRE-LIGHTERS
    • C10L3/00—Gaseous fuels; Natural gas; Synthetic natural gas obtained by processes not covered by subclass C10G, C10K; Liquefied petroleum gas
    • C10L3/06—Natural gas; Synthetic natural gas obtained by processes not covered by C10G, C10K3/02 or C10K3/04
    • C10L3/10—Working-up natural gas or synthetic natural gas

Definitions

  • the invention relates to a method for dehydrating and / or degassing natural gas, using a mixture of solvents.
  • the treatment of natural gas requires dehydration, degassing, when natural gas contains condensable hydrocarbons and deacidification of this gas when the proportion of acid gases it contains is too high.
  • the present invention also makes it possible to recover the methanol contained in the gas by a simple and economical means.
  • the heavy solvent can for example be a polar solvent such as dimethylformamide (DMF), N-methylpyrrolidone (NMP) or dimethylsulfoxide (DMSO).
  • the heavy solvent can also be a chemical solvent such as for example a secondary or tertiary amine, for example hydroxylated.
  • methanol makes it possible in particular to very significantly reduce the level of solvent for relatively large contents of acid gases in the gas to be treated.
  • the presence of methanol also makes it possible to absorb and separate impurities such as mercaptans, carbonyl sulfide (COS) and carbon disulfide (CS 2 ) from the gas to be treated.
  • impurities such as mercaptans, carbonyl sulfide (COS) and carbon disulfide (CS 2 ) from the gas to be treated.
  • the gas to be treated arrives via line 1. It contains for example methane, ethane, propane, butane, as well as heavier hydrocarbons, water and acid gases such as for example H 2 S and CO 2 .
  • a fraction of this gas is sent via line 2 into the contact column C1, in which it is brought into counter-current contact with a solution of methanol in water arriving via line 3.
  • a solution of methanol in water arriving via line 3 At the bottom of column C1 , an aqueous phase substantially free of methanol is eliminated via line 40.
  • a gas loaded with methanol is recovered via line 4 which is mixed with the gas which has not passed through column C1. The gas thus obtained constitutes the gas loaded with methanol from step (a).
  • This gas is then sent via line 6 to column C2, in which it is brought into contact with a mixture of solvents, comprising methanol, water and a solvent heavier than methanol, which arrives via line 7
  • a mixture of solvents comprising methanol, water and a solvent heavier than methanol
  • This mixture of solvents emerges through the conduit 8 charged with acid gases, while the gas evacuated at the head of the column by the conduit 9 is at least partially freed from the acid gases which it contains at the entry into the column C2 (step (b)).
  • the solvent mixture from this step (b) is first expanded to an intermediate pressure through the expansion valve V1, releasing a gas phase which contains at least part of the hydrocarbons which may have been coabsorbed in the solvent mixture .
  • the gas phase and the liquid phase thus obtained are separated in the flask B1.
  • the additional flow rate of aqueous phase thus provided can be controlled, for example, at a level of solvent mixture in a recipe or storage tank situated, for example, at the outlet of column D1.
  • the gas phase is evacuated at the head of the balloon B1.
  • the residual solvent mixture is discharged through line 10 and passes into the exchanger E1, in which it is heated. It is then expanded through the valve V2 and regenerated in the distillation column D1.
  • This column is cooled at the head, which makes it possible to evacuate via the conduit 11 acid gases relatively little loaded with solvent and heated at the bottom, which allows to evacuate by the conduit 12 a mixture of solvents substantially free of acid gases.
  • the acid gases discharged through line 11 undergo additional refrigeration in the exchanger E5, to recover at least partially the residual methanol.
  • the liquid phase thus obtained is collected in the separator flask B20, which also receives the addition of aqueous phase arriving through the conduit 42 and passing through the expansion valve V40.
  • the liquid phase thus collected in the separator flask 820 is recycled by the pump P12 through the conduit 43 at the head of the column C2.
  • the mixture of solvents evacuated via line 12 is taken up by pump P1 and sent through the exchanger El, in which it is cooled by reheating the mixture of solvents which arrives via line 10. It is then cooled in the exchanger E2 by exchange with water or cooling air and recycled to column C2.
  • the gas leaving column C2 via line 9 causes a greater quantity of water than that which arrives via line 6.
  • a certain amount of water can be evacuated with the acid gases via line 11.
  • This additional aqueous phase can be obtained for example by cooling the gas at the outlet of column C2 and by returning the condensed fraction to the circuit of the solvent mixture. It is also possible, as shown in FIG. 1, to take a fraction of the aqueous phase collected in the separator flask B2 and to recycle it through the conduit 42 and through the expansion valve V40 to the mixing circuit of solvents.
  • the gas coming from stage (b) which is evacuated via line 9 receives an additional methanol arriving via line 13. It is then cooled, first by internal exchange in the exchanger E3, then by exchange with a external refrigeration fluid coming from a refrigeration circuit, in the exchanger E4. This refrigeration condenses a methanol solution and a liquid hydrocarbon phase.
  • the gas phase thus obtained constitutes the treated gas which is substantially free of the water, acid gases and heavy hydrocarbons it contains at the start.
  • the three-phase mixture obtained is separated in the flask B2.
  • the treated gas passes through the exchanger E3, in which it is heated by cooling the gas which arrives from the column C2 and it is evacuated through the pipe 14.
  • the liquid hydrocarbon phase obtained is discharged through line 15 and the fraction of the aqueous phase containing methanol obtained which is not discharged through line 42 is recycled by the pump P2 through line 41 to column C1.
  • the mixture of solvents sent via line 7 comprises methanol, water and a solvent heavier than methanol.
  • the methanol content of the gas discharged through line 9 must be high enough to prevent the formation of ice and / or hydrates during the refrigeration step, the addition of methanol arriving through line 13 being reduced and intended to compensate for losses. This means that this methanol content is higher the lower the refrigeration temperature at the outlet of the exchanger E4. The methanol content in the mixture of solvents arriving via line 7 is also higher the lower the temperature at which the gas is refrigerated.
  • the methanol content can be easily regulated by means of the addition of methanol arriving via line 13.
  • the amount of makeup is for example controlled by the content of methanol in the aqueous phase collected in the separator B2 so as to reach the content required to avoid the formation of hydrates.
  • the methanol content in the mixture of solvents can be in this case for example between 5 and 50% in molar fraction.
  • the heavy solvent which enters into the composition of the mixture of solvents can be a polar solvent such as for example DMF, NMP, DMSO, as described above; it can also be, sulfolane, propylene carbonate, an alcohol heavier than methanol, an ether or a ketone.
  • a polar solvent such as for example DMF, NMP, DMSO, as described above; it can also be, sulfolane, propylene carbonate, an alcohol heavier than methanol, an ether or a ketone.
  • the main condition to respect is that its boiling temperature is higher than the temperature of boiling methanol and preferably higher than the boiling temperature of water. It is also necessary that this solvent is at least partially miscible with water and methanol.
  • the content of heavy solvent in the mixture of solvents can be in this case for example between 10 and 60% in molar fraction.
  • the water content forms the complement but it is preferably at least equal to 10% in molar fraction.
  • the heavy solvent which enters into the composition of the mixture of solvents can also be a solvent of chemical type such as for example a secondary or tertiary amine, in general hydroxylated, chosen for example from monoethanolamine, diethanolamine, diglycolamine, diisopropanolamine, methyldiethanolamine.
  • a solvent of chemical type such as for example a secondary or tertiary amine, in general hydroxylated, chosen for example from monoethanolamine, diethanolamine, diglycolamine, diisopropanolamine, methyldiethanolamine.
  • the content of amine in the mixture of solvents can be for example between 1 and 10% in molar fraction.
  • the heavy solvent is selected according to the specifications required for the treated gas. If selective deacidification is sought, consisting in eliminating H 2 S much more selectively than CO 2 , a selective amine such as for example methyldiethanolamine will be used.
  • additives known to a person skilled in the art, such as for example additives making it possible to activate the absorption of CO 2 , or additives acting as corrosion inhibitors, or else additives acting as anti-foaming agents. It may also be advantageous to filter the mixture of solvents which is sent to column C2, in order to stop the solid particles which can promote foaming.
  • step (d) makes it possible to evacuate at the bottom of said column an aqueous phase substantially stripped of methanol. This makes it possible to easily recover and recycle the methanol and to avoid any pollution linked to the presence of methanol in the discharged aqueous phase.
  • the contact column used can be of different types known to those skilled in the art: trays or packed. In the case of a packed column, it may be advantageous to use structured packing.
  • the other columns used in the process can be of different types known to those skilled in the art: with trays or with packing and in particular with structured filling.
  • composition of natural gas is for example the following (in kg / h):
  • the gas thus obtained is sent via line 6 to column C2.
  • a solution containing 20% by mass of methanol and 20% by mass of diethanolamine in water is injected against the current into column C2 via line 7 at the temperature of 40 ° C. with a flow rate of 117 409 kg / h.
  • the mixture of solvents loaded with carbon dioxide is recovered via line 8 at a temperature of 46 ° C.
  • the gas evacuated at the head of column D1 through line 11 is cooled to -26 ° C after it has passed through exchanger E5.
  • the flask B20 makes it possible to separate a liquid phase containing essentially methanol and water and a gaseous phase containing essentially carbon dioxide.
  • the aqueous phase is recycled to column C2 via line 43.
  • the gaseous phase is removed through line 23.
  • step (b) it can be advantageous, to optimize the performance of the process, to carry out step (b) by bringing the gas successively into contact with fractions of mixtures of solvents of different compositions. If one fraction of the mixture is sent at the top and another at an intermediate point, it is advantageous to send at the top a fraction of the mixture of solvents relatively low in methanol and to send at a intermediate point a fraction of the mixture of solvents relatively rich in methanol.
  • the gas loaded with methanol arrives via line 6 in column C2. It is first of all brought into contact in a first zone (lower part) of column C2 with a fraction of mixture of solvents relatively rich in methanol introduced by line 16.
  • the methanol content in this first fraction of solvent mixture can be for example between 20 and 70% by mole fraction.
  • the mixture of solvents charged with acid gases leaving via the pipe 8 is first expanded to an intermediate pressure level through the valve V1, by releasing a gaseous phase which contains at least part of the hydrocarbons which could be coabsorbed in the solvent mixture.
  • This gas phase can be washed with a fraction of a mixture of solvents relatively poor in methanol, the flow rate of which is controlled by the distribution valve V30 and which is sent via line 17 at the head of a countercurrent contact section located in column element C10.
  • the gas which leaves the head of the column element C10 is thus substantially freed from the acid gases which it contained and can for example serve as fuel-gas or even be recompressed and mixed with the treated gas.
  • step (b) it is possible to subject the mixture of solvents coming from step (b) to a first step of expansion to an intermediate pressure to release at least part of the coabsorbed hydrocarbons.
  • the solvent mixture is expanded again to a low pressure, for example a pressure close to atmospheric pressure, through the expansion valve V20.
  • the liquid-vapor mixture thus obtained is separated in the separator flask B10.
  • the vapor phase formed essentially of acid gases and methane is evacuated through line 18.
  • the liquid phase thus obtained is split into two fractions.
  • a first fraction preferably the largest in flow rate, is taken up by the pump P11 through the conduit 20 and forms the major part of the fraction of solvent mixture relatively rich in methanol which is sent by the conduit 16 at an intermediate point. from column C2.
  • a second fraction of the mixture of solvents obtained at the outlet of the separator flask B10 is reheated in the exchanger El, by heat exchange with the mixture of solvents coming from the bottom of the column D1, then sent to the distillation column D1.
  • a steam reflux is generated at the bottom of the column D1 by means of the reboiler R1 and a liquid reflux is generated at the head of the column D1 by means of the condenser E6.
  • the gaseous phase resulting from the partial condensation in E6 and which is evacuated at the head via line 19 is formed essentially of acid gases and methanol.
  • the liquid phase which is discharged at the bottom of column D1 is depleted in methanol.
  • column D1 stripping at the bottom of the column is ensured by a vapor rich in methanol, which makes it possible to reboil column D1 at a lower temperature and by providing less heat than in the absence of methanol. .
  • the liquid phase discharged at the bottom of column D1 is taken up by pump P10. It is cooled in the exchanger El, from which it emerges through the conduit 21. It is then divided into two fractions by means of the distribution valve V30. A first fraction, the largest in terms of flow rate, is cooled in the exchanger E2 by water or cooling air and sent to the head of the column C2 by the conduit 7. A second fraction is sent by the conduit 17 at the top of column element C10.
  • the gas to be treated contains a large proportion of CO 2 and of H 2 S, it may be desirable to obtain separate fractions of acid gases, respectively rich in CO 2 and in H 2 S.
  • the acid gases containing methanol obtained by mixing the gaseous fractions arriving via the conduits 18 and 19 are sent to the column element C20.
  • the gas fraction at the head of the column element C20 is refrigerated in the exchanger E5.
  • the liquid-vapor mixture thus obtained is separated in the reflux flask BR.
  • the gaseous phase rich in acid gases is discharged through line 23.
  • the liquid phase is sent as reflux to the top of the column element C20.
  • a liquid phase rich in methanol is obtained which is taken up by the pump P12 and sent through the conduit 22.
  • a first fraction is expanded through valve V42 and sent to the head of column D1.
  • This embodiment of the method is therefore characterized in that the fraction of the mixture of solvents relatively rich in methanol which is sent to an intermediate point of the contact column used during step (b) is taken at an intermediate point of the regeneration column used during step (c).
  • each of these fractions can be sent to several different levels. Similarly, it is possible to use more than two fractions of different compositions, said fractions being taken from different points of the regeneration column D1 used during step (c) and sent to different points of the column d absorption C2 used during step (b).
  • the solvent mixture fraction (s) from the regeneration column D1 are cooled to a temperature close to the temperature at which step (b) is carried out by heat exchange with one or more fractions of the solvent mixture from step (b) and optionally by additional heat exchange, with a cooling fluid such as water or air.
  • the absorption step (b) is carried out in column C2 at a temperature for example between +10 and +40 ° C, but it is also possible to reduce the solvent level to carry out this step at higher temperatures. low, with a mixture of solvents selected so as not to become too viscous at these temperature levels.
  • the pressure at which the absorption step is carried out in column C2 can be between a few bars and more than a hundred bars. It can for example be close to 70 bars.
  • the natural gas can be refrigerated to a temperature of, for example, between 0 and -100 ° C., the methanol content in the fraction of solvent mixture sent to the top of the column of contact used during step (b) being adjusted so as to obtain in the gas resulting from step (b) a methanol content making it possible to avoid the formation of hydrates at the lowest temperature obtained during from step (c).
  • step (c) When the gas contains condensable hydrocarbons, the refrigeration carried out during step (c) makes it possible to degasoline this gas and to adjust the hydrocarbon dew point to the value required for the transport of the gas.
  • This refrigeration can also allow this gas to be fractionated, for example by separating the LPG present in the gas. It is possible in this case to use all the devices known to those skilled in the art, such as for example distillation columns or heat exchangers operating with liquid reflux.
  • the regeneration of the mixture of solvents from step (b) can be carried out after expansion at least in part in a device operating in fractionation and in simultaneous heat exchange.
  • the device EC1 can for example be a heat exchanger placed vertically and operating against the current.
  • the mixture of solvents arriving from the separator flask B10 is sent to the head of this exchanger. It is gradually heated downwards in the exchanger, which causes the formation of a gaseous phase containing essentially acid gases and methanol which is evacuated at the head by the conduit 19, by circulating in the exchanger EC1 against the current. of the liquid phase constituted by the mixture of solvents.
  • the solvent mixture thus leaves purified at the bottom of the exchanger EC1. It is taken up by the pump P13, heated in the exchanger E10 and cooled by passing through the exchanger EC1 in which it heats the mixture which descends. At the outlet of the exchanger EC1, the purified solvent mixture is sent via line 21 at the head of the absorption column C2 used during step (b).
  • the EC1 exchanger can be, for example, with tubes and calender or with plates, either in brazed aluminum or in stainless steel.
  • the regeneration step can be carried out in two or more columns operating under different pressure and temperature conditions. It is thus possible, for example, to obtain fractions of acid gases of different compositions, for example a fraction concentrated in CO 2 and a fraction concentrated in H 2 S.
  • Each of these regeneration operations can be carried out in one or more distillation sections, some of which can be carried out with simultaneous heat exchange.
  • the regeneration step (c) thus comprises at least two successive regeneration operations, a gaseous fraction rich in CO 2 being obtained at the end of the first operation and a gaseous fraction rich in H 2 S being obtained at the end of the second operation.
  • the process also makes it possible to separate impurities such as mercaptans, COS and CS 2 which can, for example, be eliminated with the gaseous fraction rich in H 2 S.

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  • Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Gas Separation By Absorption (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Drying Of Gases (AREA)
EP96402909A 1995-12-28 1996-12-27 Verfahren zur Entfernung von Wasser, Saüren und Benzin aus Erdgas, unter Verwendung eines Lösungsmittelgemisches Expired - Lifetime EP0783031B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR9515626 1995-12-28
FR9515626A FR2743083B1 (fr) 1995-12-28 1995-12-28 Procede de deshydratation, de desacidification et de degazolinage d'un gaz naturel, utilisant un melange de solvants

Publications (2)

Publication Number Publication Date
EP0783031A1 true EP0783031A1 (de) 1997-07-09
EP0783031B1 EP0783031B1 (de) 2001-09-26

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EP96402909A Expired - Lifetime EP0783031B1 (de) 1995-12-28 1996-12-27 Verfahren zur Entfernung von Wasser, Saüren und Benzin aus Erdgas, unter Verwendung eines Lösungsmittelgemisches

Country Status (8)

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US (1) US5782958A (de)
EP (1) EP0783031B1 (de)
JP (1) JP4264594B2 (de)
CA (1) CA2194083C (de)
DE (1) DE69615522T2 (de)
DK (1) DK0783031T3 (de)
FR (1) FR2743083B1 (de)
NO (1) NO314901B1 (de)

Cited By (2)

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FR2820430A1 (fr) * 2001-02-02 2002-08-09 Inst Francais Du Petrole Procede de desacidification d'un gaz avec lavage des hydrocarbures desorbes lors de la regeneration du solvant
CN104812876A (zh) * 2012-11-26 2015-07-29 挪威国家石油公司 自井流的结合的气体脱水和液体抑制

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EP0783031B1 (de) 2001-09-26
DE69615522T2 (de) 2002-04-25
CA2194083A1 (fr) 1997-06-29
DK0783031T3 (da) 2001-11-26
FR2743083B1 (fr) 1998-01-30
US5782958A (en) 1998-07-21
FR2743083A1 (fr) 1997-07-04
JP4264594B2 (ja) 2009-05-20
NO965609D0 (no) 1996-12-27
NO965609L (no) 1997-06-30
DE69615522D1 (de) 2001-10-31
CA2194083C (fr) 2006-06-06
JPH09194851A (ja) 1997-07-29
NO314901B1 (no) 2003-06-10

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