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    • 专利摘要:
    A method of treating a gaseous stream (1) containing at least one acid gas, ethane and a light gas selected from methane, carbon monoxide, hydrogen and nitrogen comprising the steps of: Step a ): feeding with said gaseous stream (1) a cryogenic separation unit (A) comprising at least one distillation column (14) for treating said gaseous stream (1), the treatment comprising the partial elimination of the acid gas of said a gaseous stream and producing a gaseous stream depleted in acid gas and said at least one distillation column (14) comprising a main supply means (33) for a liquid stream; Step b): removal of the cryogenic separation unit (A) from at least a portion (23) of the gaseous treated stream depleted in acid gas; Step c): feeding with at least a portion of the gaseous acid-treated gas stream (23) of a physical separation unit (29) separating the acid gas from ethane, wherein said stream is separated to form a residue enriched with light gas and ethane (31) and a stream (30), permeate, enriched with acid gas; Step d): return of the stream (30) enriched in acid gas in the cryogenic separation unit (A) by introducing it separately from the feed defined in step a) of the cryogenic separation unit (A) and below the main feed means (33) of the column (14), for extracting ethane from one of at least one distillation column (14).
    公开号:FR3034509A1
    申请号:FR1552845
    申请日:2015-04-02
    公开日:2016-10-07
    发明作者:Oumar Khan；Mathieu Leclerc；Paul Terrien
    申请人:Air Liquide SA；LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude；
    IPC主号:
    专利说明:

    [0001] The present invention relates to a method for minimizing ethane loss during the treatment of CO2-rich natural gas. Natural gas is desirable for use as a fuel for use in heating buildings, to provide heat for industrial processes for the generation of electricity, for use as a feedstock for various synthesis processes for produce olefins, polymers and the like. Natural gas is a resource still abundant. On the other hand, the amount of conventional natural gas represents a smaller and smaller share of production. Several types of unconventional gas exist. A prime example is shale gas, which accounts for a growing share of production. Another example: the fields of acid gas, hitherto unexploited because of their high CO2 content as well as H2S represent a significant part of the potentially exploitable gas.
    [0002] The use of an efficient and economical process for purifying natural gas into acid compounds (typically H2S and CO2) is therefore of great importance. The efficiency of such a process can be measured in particular in terms of losses of hydrocarbons in the waste stream. This yield can be quantitatively written as an energy efficiency or HHV yield (defined as the ratio of the calorific value of the natural gas treated by said process by the calorific value of the natural gas to be purified). A method of separating CO2 from natural gas by cryogenic means is known and described in patent application FR 2 959 512. This process makes it possible to purify a stream of natural gas in CO2 by means of a first column producing a current. liquid foot containing predominantly CO2 and a gaseous head containing predominantly CH4. This column is equipped with a reboiler and a condenser. A portion of the liquid foot stream of this first column is then used to produce the cold necessary for the process, by means of three detents at three different pressures followed by the vaporization of these same three expanded streams. The successive sprays being partial, residual liquids (rich in CO2 but still containing a significant amount of hydrocarbons 3034509 2 having at least two carbon atoms such as ethane, propane and butane) are harvested, pumped at a rate of some pressure and sent to a second column, this time only provided with a reboiler. This column makes it possible to recover at its head a gaseous stream rich in purified CO2 and at the bottom a liquid stream rich in hydrocarbons having at least three carbon atoms such as propane and butane. The overhead gas stream is then compressed, condensed and mixed with the liquid stream from the first column, before the mixture of these two streams is pumped to the required pressure. The main disadvantage of the process which is the subject of the invention described in FR 2 959 512 relates to the fact that only the non-vaporized liquid during the three successive sprays is treated in the second column: the hydrocarbons having at least two carbon atoms such that Ethane, propane and butane contained in the gaseous phases are therefore sent to the CO2 and thus not recovered in the natural gas. In particular, such a process necessarily has a very high loss of ethane (typically at least 50%). Indeed ethane and carbon dioxide are very difficult to separate as shown in the curve of Figure 1 (binary ethane C2-0O2 at 30 bar). The curve in FIG. 1 illustrates that the separation between ethane and carbon dioxide is difficult: the two curves are very close to each other, especially when the CO2 content is high. - The curve has an azeotrope, which shows that it is impossible without a particular device to make a total distillation in a simple distillation column with condenser and reboiler. Moreover, it is known to separate CO2 and ethane relatively efficiently by membrane separation. On the other hand, membrane separation alone does not make it possible to separate CO2 from methane in a very efficient manner (there are many losses of methane in CO2).
    [0003] The inventors of the present invention have then bridged a solution to solve the problems raised above. An object of the present invention is to effectively separate any mixture containing both at least CO2, ethane and a light compound such as methane, nitrogen, CO or hydrogen. while avoiding the disadvantages mentioned above. The invention can more broadly be applied to the separation of a mixture of at least three gases: an acid gas, a light gas and a low permeability gas. The acid gas may be carbon dioxide or hydrogen sulfide, the light gas of methane and the low permeability gas of ethane. The process according to the invention is particularly advantageous when the cryogenic separation of the low permeability gas and the acid gas are difficult. The present invention relates to a process for treating a gaseous stream containing at least one acid gas, ethane and a light gas selected from methane, carbon monoxide, hydrogen and nitrogen comprising the following: following steps: a) supplying with said gas stream a cryogenic separation unit comprising at least one distillation column for treating said gas stream, the treatment comprising the partial removal of the acid gas from said gas stream and the production of a a gaseous stream depleted in acid gas and said at least one distillation column comprising a main supply means of a liquid stream; b) withdrawing the cryogenic separation unit from at least a portion of the treated gaseous stream depleted in acid gas; c) feeding with at least a portion of the acid gas-treated treated gaseous stream of a physical separation unit separating the acid gas from ethane, wherein said stream is separated to form a residue enriched with light gas and ethane and a permeate stream enriched with acid gas; d) Return of the stream enriched with acid gas in the cryogenic separation unit in order to extract ethane from one of the at least one distillation column by introducing it separately from the feed defined in step a) of the cryogenic separation unit and below the main feed means of the column. Cryogenic separation means separation effected at a temperature below -30 ° C and above -100 ° C, when the pressure is between 5 bara (absolute bar) and 100 bara. Preferably, the temperature of the cryogenic separation is between -40 ° C and -60 ° C for a pressure of between 10 bara and 70 bara. By physical separation is meant separation by one of the following means: Membrane separation; or 5 -Absorption separation (for example by pressure modulation - PSA or by temperature modulation - TSA) Preferably, the temperature of the physical separation is between 5 ° C and 100 ° C when the pressure is between 1.5 bara and 90 bara. The proposed method may furthermore comprise at least the following characteristics: Process as defined above, characterized in that it comprises step e): recovery, from the cryogenic separation unit, of a stream containing more than 90% of the acid gas initially present in the gas stream to be treated.
    [0004] Process as defined above, characterized in that it comprises the additional step: recovering, from the physical separation unit, a gaseous stream containing more than 95% of the light gas initially present in the gaseous stream to be treated and more than 45% of the ethane initially present in the gaseous stream to be treated. Process as defined above, characterized in that the acidic gas is selected from CO2 and H2S. Process as defined above, characterized in that the acid gas is carbon dioxide and the light gas is methane.
    [0005] Process as defined above, characterized in that the gaseous stream to be treated comprises from 10 mol% to 75 mol% methane, from 25 mol% to 90 mol% carbon dioxide and from 0.1 mol% to 15% molar. molar of ethane. Process as defined above, characterized in that said gaseous stream to be treated further comprises hydrogen sulphide and hydrocarbons having at least three carbon atoms. Process as defined above, characterized in that, at a pressure of between 5 bara and 100 bara, the temperature in the cryogenic separation unit is below -30 ° C and preferably between -40 ° C and - 60 ° C. Process as defined above, characterized in that the physical separation unit is a membrane separation unit comprising at least one membrane. Process as defined above, characterized in that said at least one membrane is a polymer membrane. Process as defined above, characterized in that the physical separation unit is a pressure modulation adsorption unit (PSA).
    [0006] The present invention particularly relates to the purification of a CO 2 stream of natural gas by means of a cryogenic unit followed by a membrane separation, making it possible to maximize the HHV yield by minimizing the loss of hydrocarbons in the CO 2, and more particularly the loss of methane and ethane in CO2, taking advantage of both the advantages of cryogenic separation and membrane separation. An object of the present invention is therefore a process for separating CO2 from natural gas to obtain a methane-rich stream and a methane-free CO2 stream (typically less than 1% by volume methane, preferably less than 0.5% methane). ). This process uses cryogenic separation (typically partial condensation and / or distillation around -40 ° C to -60 ° C) and membrane separation in a second step to both deplete the methane rich stream in CO2 and produce a CO2 stream depleted in ethane so that it is recycled to the cryogenic separation. As a remark, it can for example a separator pot operating at -20 ° C or -30 ° C before distillation in a column may be present. The process typically comprises the following steps: 1) Drying a feed gas comprising methane, carbon dioxide and ethane. 2) First cooling in a heat exchanger and partial condensation to obtain a first liquid and a first gas. 3) Cooling of the first gas in a heat exchanger and partial condensation to obtain a second liquid and a second gas enriched in methane. 4) Mixing the two liquids and expanding the mixture in a valve to introduce it into a first distillation column. 5) Separation of most of the methane remaining in said distillation column to obtain a liquid depleted of ethane at the bottom of the column. 6) Relaxing the liquid from the first distillation column to introduce it into a second distillation column at lower pressure. 7) Compression of the current from the head of the two columns to recycle it to the feed gas. 8) Vaporization of the liquid depleted of methane, preferably at several pressure levels (for example about 5.5 bar, about 11 bar and about 16 bar) to provide at least a portion of the frigories required for steps 2) and 3) for obtain at least one low pressure gas, and optionally a medium pressure gas and a high pressure gas. 9) Compression of the low pressure gas, and possibly medium pressure gas to mix all the gases from the methane depleted liquid to obtain a high pressure gas depleted in methane. 10) Introduction of the methane-enriched gas into a membrane permeation unit to obtain a product gas and a carbon dioxide enriched and ethanol-depleted gas which is compressed to the pressure of the first distillation column and introduced at least partly into the vat of the first distillation column to reboil and extract the ethane from the first distillation column by stripping. This (these) introduction (s) of (the) stream (s) depleted (s) can be done before or after a passage in an exchanger while being mixed or not with another current. The invention utilizes a carbon dioxide enriched and ethanol-depleted stream to stripping the ethane from the first distillation column and thereby minimizing the loss of ethane in the produced carbon dioxide. This is possible by the nature of the additional separation process (membrane separation) which is very selective between carbon dioxide and ethane.
    [0007] Several embodiments are possible: The permeate of the membranes loaded with carbon dioxide and depleted in ethane can be cooled and partially condensed in a dedicated separator pot. The formed liquid can be sent directly expanded and sent to the second distillation column since it is depleted in ethane. The gas is used as the gas injected into the first column to extract by stripping the ethane from the first column. - Several membranes in series can be used. A first membrane is used with a permeate at the pressure of the first distillation column. The amount of permeate being adjusted according to the amount of ethane to be extracted by stripping. The residue of this membrane being sent into a membrane. The number of membranes in series can be increased to obtain different permeate injected at different levels in the distillation column. The advantage of this variant is to obtain very low ethane permeates since the permeation yields through these membranes are low. The invention will be described in more detail with reference to FIG. 2 which illustrates a method according to the invention. A feed stream of gas 1, for example natural gas, is introduced into a pre-treatment unit 2 to remove impurities from said feed stream. The gaseous stream 1 comprises, for example, methane, ethane and carbon dioxide. The pre-treatment unit 2 typically has at least one adsorption unit 34 for removing the water. The gaseous stream 3 thus pretreated is cooled in a heat exchanger 4 at a temperature below -20 ° C and at a pressure of about 50 bara (or for example approximately the pressure of the feed gas). Preferably, the temperature remains above -60 ° C. The gaseous stream 5 thus cooled is partially condensed, for example in a phase separator pot 6, in order to obtain a first liquid stream 7 and a gas stream 8. This gas stream 8 is then cooled to a temperature below - 45 ° C in a heat exchanger 9, then partially condensed in a separator pot 10 to produce 3034509 8 a second liquid stream 11 and a gas stream 23 enriched in methane and depleted in carbon dioxide. The first liquid stream 7 and the second liquid stream 11 are mixed. This mixture 12 is then expanded to a pressure of between 10 bara and 30 bara, for example by means of a valve 13, in order to be introduced into a first distillation column 14 via the main supply 33 of said Column 14. A liquid stream 15 depleted of ethane is collected at the bottom of column 14 (i.e., below the lowest stage of column 14). The liquid stream 15 is expanded, for example by means of a valve 16, at a pressure of between 5 bara and 15 bara and then introduced into a second distillation column 17. The gas streams 18 and 19 collected at the top columns 14 and 17 are introduced into a heat exchanger 4 and then compressed using one or more compressors before being recycled to about the pressure of the gas supply gas to the stream gaseous initial pretreated 3.
    [0008] A liquid depleted of methane 21 is collected at the bottom of the second distillation column 17, and is vaporized to produce a gas stream 22. Preferably, said liquid 21 is vaporized at several pressure levels (for example about 5.5 bar about 11 bar and about 16 bar) to provide at least a portion of the frigories required for the previously described steps to obtain at least one low pressure gas, and optionally a medium pressure gas and a high pressure gas. The gas stream 22 is compressed using a compressor 24 to a pressure between 10 bara and 50 bara to produce a gas called "high pressure" depleted of methane 25.
    [0009] This gas 25 can then be treated in a treatment unit 26 containing at least one distillation column in order to separate the carbon dioxide thus produced 27 from heavy hydrocarbons 28 having more than three carbon atoms, such as propane and butane, initially contained in the gaseous stream 1 to be treated.
    [0010] The gas stream enriched in methane 23 is introduced into a physical separation unit 29. Such a unit 29 is for example a membrane separation unit comprising at least one membrane allowing good separation of carbon dioxide and ethane. The treatment of the gaseous stream 23 by the unit 29 makes it possible to produce a gaseous stream 30 enriched in carbon dioxide and depleted in ethane and a gaseous stream 31 enriched with methane and ethane which can optionally be subsequently mixed with the gaseous stream of 30.degree. heavy hydrocarbons 28.
    [0011] A stream of natural gas 31 enriched in methane, ethane and heavy hydrocarbons but depleted in carbon dioxide and other acid gases is thus produced by the implementation of the method which is the subject of the invention. Indeed, the gaseous stream 30 enriched in carbon dioxide and depleted in ethane is compressed using one or more compressors 20. This pressure 10 is that of the stream supplying the first distillation column 14. The gas stream 30 and The bottom 32 of the column 14 is located below the main supply 33 and is compressed at least partly at the bottom 32 of the first distillation column. This makes it possible to produce a reboiler function for this first column 14 and in particular to extract ethane from this first column 14 because the gaseous stream rising in the column is very low in ethane (typically below 0, 1 ° A mol of ethane and at most five times less ethane than in the feed gas), to the gas stream 18 extracted at the top of the column 14. This introduction 32 of the ethane-depleted gas in the column 14 may be performed before or after a passage in a heat exchanger, said gas being mixed or not with another stream. Another part of the gaseous stream 30 enriched with carbon dioxide and compressed is directly mixed with the gas stream 3 to produce a mixture 3 'introduced into the exchanger 4. In FIG. 2, the cryogenic separation unit (A) comprises at least minus the elements 4, 6, 9, 10, 13, 14, 17. The invention is not limited to only this cryogenic purification configuration. Some examples of modifications for which the invention can still be applied are listed below: - Number of exchangers different: the exchangers 9 and 4 could possibly be combined into a single exchanger or at least three exchangers. 3034509 10 -Number of different distillation columns: the invention also applies to processes comprising only one distillation column, whatever the pressure. - Number of separator pots: the invention can be applied when there are at least three separator pots but it can also be applied with a, see no pot separator. - Different refrigeration system: Figure 2 shows a self-refrigerated diagram, that is to say a scheme where refrigeration is provided by expansion of liquid CO2. It would be possible not to relax the liquid CO2, for example, and instead to pump it, using an external refrigeration system (CO2 cycle, propane cycle or any other refrigeration cycle). Table 1 below summarizes the material balance made throughout the process illustrated in Figure 2.
    [0012] The numbers of the "currents" (first column of the table) are the numbers of Figure 2 current CH4 CO2 H2S C2 C3 iC4 nC4 1 16 818 10 412 891 686 342 200 51 3 '28 464 17 235 1 257 1 553 435 220 54 23 20 624 4 464 229 498 42 6 1 18 11 646 6 824 365 867 92 20 3 21 0 10 934 971 222 350 234 61 19 1 019 3 961 223 241 63 14 2 27 0 9 862 850 207 14 4 0 31 16 818 552 41 479 328 196 51 Table 1: Associated material balance (in Nm3 / h).
    [0013] The distillation columns used in the process according to the invention are, for example, columns chosen according to one of the following two types: column with trays or column with packing (structured or not). The role of the distillation column is to promote the exchange of material and energy between the gas phase and the liquid phase, which increases the separating power of the column. Distillation columns use the difference in volatility of the components of a mixture to separate them. To improve the separation, a large exchange surface between the gas phase and the liquid phase is necessary. To increase the latter, elements are added in the column, such as trays or packings, the latter may be structured or not. In addition to the column and its lining, two heat exchangers can provide / remove the energy required for separation: a boiler located at the bottom of the column where the mixture is heated to boiling and the condenser in column head which allows to liquefy the vapors to recover the purified product in liquid form. Part of the condensate is often reinjected into the column to increase the purity of the desired product, which is reflux. In the case of CO2, it can often happen, as is the case in the example of Figure 2 that there is no condenser as such, because the temperature of the column head is too close the temperature at which CO2 could solidify. In the example of FIG. 2, the heat exchanger 9 and the separator pot 10 are in some respects the role of condenser. The method which is the subject of the present invention mainly makes it possible to minimize the loss of hydrocarbons. This advantage is illustrated below by considering a conventional scheme where the stream from the membrane separation unit is simply mixed with the feed gas and comparing it with the process object of the present invention and by the example described in US Pat. FIG. 2. Conventional diagram Scheme according to the example of the invention illustrated in FIG. 2 Yield C2 45% -47% 70% Yield PCS 93% -94% 95.4% 3034509 12 The yield C2 is defined as the ratio of the molar amount of ethanol in the final product by the molar amount of ethane in the feed gas. The PCS yield is defined as the ratio of Qfinal by Qalim where Qfinal is the product of the higher heating value (in J / Nm3) of the final product multiplied by the molar flow rate of the final product and Qalim is the product of the higher heating value (in J / Nm3) of the feed gas multiplied by the molar flow rate of the feed gas.
    权利要求:
    Claims (11)
    [0001]
    REVENDICATIONS1. A method of treating a gaseous stream (1) containing at least one acid gas, ethane and a light gas selected from methane, carbon monoxide, hydrogen and nitrogen comprising the steps of: Step a ): feeding with said gaseous stream (1) a cryogenic separation unit (A) comprising at least one distillation column (14) for treating said gaseous stream (1), the treatment comprising the partial elimination of the acid gas of said a gaseous stream and producing a gaseous stream depleted in acid gas and said at least one distillation column (14) comprising a main supply means (33) for a liquid stream; Step b): removal of the cryogenic separation unit (A) from at least a portion (23) of the gaseous treated stream depleted in acid gas; Step c): feeding with at least a portion of the gaseous acid-treated gas stream (23) of a physical separation unit (29) separating the acid gas from ethane, wherein said stream is separated to form a residue enriched with light gas and ethane (31) and a stream (30), permeate, enriched with acid gas; Step d): return of the stream (30) enriched in acid gas in the cryogenic separation unit (A) by introducing it separately from the feed defined in step a) of the cryogenic separation unit (A) and below the main feed means (33) of the column (14), for extracting ethane from one of at least one distillation column (14).
    [0002]
    2. Method according to the preceding claim characterized in that it comprises step e): recovering, from the cryogenic separation unit (A), a stream containing more than 90% of the acid gas initially present in the gaseous stream to be treated.
    [0003]
    3. Method according to one of the preceding claims characterized in that it comprises the additional step: f) recovering, from the physical separation unit (29), a gaseous stream containing more than 95% of the light gas initially present in the gaseous stream to be treated and more than 45% of the ethane initially present in the gaseous stream to be treated (1). 3034509 14
    [0004]
    4. Process according to any one of the preceding claims, characterized in that the acidic gas is chosen from CO2 and H2S.
    [0005]
    5. Process according to any one of the preceding claims, characterized in that the acid gas is carbon dioxide and the light gas is methane.
    [0006]
    6. Process according to any one of the preceding claims, characterized in that the gaseous stream to be treated (1) comprises from 10 mol% to 75 mol% of methane, from 25 mol% to 90 mol% of carbon dioxide and from 0 mol% to , 1 mol% to 15 mol% of ethane. 10
    [0007]
    7. Method according to the preceding claim characterized in that said gaseous stream to be treated (1) further comprises hydrogen sulphide and hydrocarbons having at least three carbon atoms.
    [0008]
    8. Process according to any one of the preceding claims, characterized in that, at a pressure of between 5 bara and 100 bara, the temperature in the cryogenic separation unit (A) is less than -30 ° C. and preferably between - 40 ° C and - 60 ° C.
    [0009]
    9. Method according to any one of the preceding claims characterized in that the physical separation unit (29) is a membrane separation unit comprising at least one membrane. 20
    [0010]
    10. Method according to the preceding claim characterized in that said at least one membrane is a polymer membrane.
    [0011]
    11. Method according to one of claims 1 to 9 characterized in that the physical separation unit (29) is a pressure modulation adsorption unit (PSA). 25
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    同族专利:
    公开号 | 公开日
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    WO2016156691A1|2016-10-06|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    US4936887A|1989-11-02|1990-06-26|Phillips Petroleum Company|Distillation plus membrane processing of gas streams|
    US20120065450A1|2009-05-19|2012-03-15|Zaida Diaz|Process that utilizes combined distillation and membrane separation in the separation of an acidic contaminant from a light hydrocarbon gas stream|
    WO2013144671A1|2012-03-27|2013-10-03|Total Sa|Cryogenic separation process of a feed gas stream containing carbon dioxide and methane|
    FR2959512B1|2010-04-29|2012-06-29|Total Sa|PROCESS FOR TREATING NATURAL GAS CONTAINING CARBON DIOXIDE|CN108800753A|2018-06-05|2018-11-13|北京恒泰洁能科技有限公司|The method that methanol-to-olefins Methane offgas produces natural gas and hydrogen|
    FR3090832A1|2018-12-19|2020-06-26|L´Air Liquide, Societe Anonyme Pour L’Etude Et L’Exploitation Des Procedes Georges Claude|Method and apparatus for separating a feed stream comprising at least CO2 as well as at least one light compound|
    FR3090833A1|2018-12-19|2020-06-26|L´Air Liquide, Societe Anonyme Pour L’Etude Et L’Exploitation Des Procedes Georges Claude|Apparatus and method for separating a gas rich in CO2 by distillation and / or partial condensation at subambient temperature|
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    优先权:
    申请号 | 申请日 | 专利标题
    FR1552845A|FR3034509B1|2015-04-02|2015-04-02|PROCESS FOR TREATING NATURAL GAS TO MINIMIZE LOSS OF ETHANE|
    FR1552845|2015-04-02|FR1552845A| FR3034509B1|2015-04-02|2015-04-02|PROCESS FOR TREATING NATURAL GAS TO MINIMIZE LOSS OF ETHANE|
    PCT/FR2016/050549| WO2016156691A1|2015-04-02|2016-03-10|Natural gas treatment method for minimizing ethane loss|
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