EP1454104A1

EP1454104A1 - Method and installation for separating a gas mixture containing methane by distillation

Info

Publication number: EP1454104A1
Application number: EP01270739A
Authority: EP
Inventors: Henri Paradowski
Original assignee: Technip France SAS
Current assignee: Technip Energies France SAS
Priority date: 2000-12-13
Filing date: 2001-12-13
Publication date: 2004-09-08
Anticipated expiration: 2021-12-13
Also published as: US6578379B2; US20020095062A1; FR2817766A1; EA200300676A1; DZ3452A1; EP1454104B1; NO20032460D0; AU1930002A; EA004469B1; WO2002048627A1; NO335827B1; FR2817766B1; BR0116093A; NO20032460L; CA2429319C; CN100389295C; CA2429319A1; AU2002219300B2; BR0116093B1; AR043699A1

Abstract

The invention concerns a method and an installation for separating a gas mixture and gases obtained by said installation. The invention concerns a method and an installation for cryogenic separation of constituents of a natural gas under pressure (14) with a first phase separator (B1) whereof the constituents of each of the phases are separated in a distillation column (C1). Part of the gas fraction (5) derived from the head of the column (C1) is recycled at the last stage thereof. The method further comprises diverting (9) part of a first head fraction (3) derived from the first phase separator. Additionally, the method comprises separating a first base fraction (4) derived from the first separator, in a second separator (B2). The invention also relates to other embodiments.

Description

"Process and installation for separation of a gaseous mixture containing methane by distillation, and gases obtained by this separation"

The present invention relates, generally and according to a first of its aspects, to a separation process making it possible to separate the constituents of natural gas into a first fraction of gas, rich in methane and essentially free of C ₂ and higher hydrocarbons, and a second fraction of gas, rich in C ₂ and higher hydrocarbons and essentially devoid of methane. More specifically, the invention relates, according to its first aspect, to a process of separation of a mixture cooled under pressure containing methane and C ₂ and higher hydrocarbons, into a light final fraction enriched in methane and a heavy final fraction enriched in C ₂ and higher hydrocarbons, comprising a first step (I) in which (la) the pressure-cooled mixture is separated, in a first balloon, into a first fraction of the head which is relatively more volatile, and a first fraction of the foot relatively less volatile, in which (Ib) the first fraction of the bottom is introduced into a middle part of a distillation column, in which (the) is collected, in a lower part of the column, as the second fraction of the bottom , the heavy final fraction enriched in C ₂ and higher hydrocarbons, into which (Id) is introduced, after having expanded it in a turbine, the first overhead fraction in a upper part of the distillation column, in which (the) a second head fraction enriched in methane is collected in the upper part of the column, in which (If) the second head fraction is then subjected, for the obtaining the light final fraction, compression and cooling, and in which (Ig) a light final fraction is taken from a first sampling fraction, this process comprising a second step (II). in which (11a) the first sampling fraction is introduced, after cooling and liquefaction, in the upper part of the distillation column.

Such a method is known from the prior art. Thus, US Pat. No. 5,881,569 discloses a process in accordance with the preamble described above. The extraction of ethane contained in natural gas can be carried out using known methods, as described in patents US-4140504, US-4157904, US-4171964 and US-4278547. Although the processes described in these patents have a certain interest, they do not make it possible to obtain, at best, in practice, that an ethane recovery rate of the order of 85%. They involve liquid / gas separators, heat exchangers, regulators (usually in the form of turbines), compressors and distillation columns.

More recently, other methods have been made public, in particular by patents US-4,649,063, US-4,854,955, US-5,555,748 and US-5,568,737. If these more recent processes can make it possible to obtain fairly satisfactory extraction yields of ethane and other hydrocarbons, these processes require, for obtaining fractions enriched in methane or in C ₂ and higher hydrocarbons, relatively energy expenditure important. In this context, the present invention aims to reduce the energy consumption during the production of fractions enriched in methane or C ₂ and higher hydrocarbons, while maintaining very high extraction yields compared to the processes of prior art.

To this end, the method of the invention, moreover in accordance with the generic definition given by it the preamble above, is essentially characterized in that it further comprises a third step in which the first fraction of the foot is subjected to one. plurality of substeps comprising reheating, passage through a second balloon, and separation into a relatively more volatile third fraction of the head, and a relatively less volatile third fraction of the foot, into which the third fraction of the foot is introduced into the middle part of the distillation column, and into which the third overhead fraction is introduced, after cooling and liquefaction, in the upper part of the distillation column.

Another method, as described in US Pat. No. 5,566,554, uses two liquid / gas separators, a liquid fraction of which collected at the bottom of the first separator is heated and then introduced into a second separator. This technique makes it possible in particular to improve the extraction of the methane contained in the fraction of the bottom coming from the first separator and above all to use the expansion of this fraction of the bottom to cool in a heat exchanger the flow of natural gas to be treated which enters in the installation.

On the other hand, this known method does not make it possible to obtain a thorough extraction of ethane because the amount of reflux generated by the technique is low and the ethane content of this reflux is relatively high.

The present invention overcomes these problems by implementing two means.

On the one hand, the invention provides for the derivation of a portion of the column head fraction rich in methane and its reintroduction on the last stage of the column after compression and cooling. This makes it possible to obtain a reflux in sufficient quantity and of excellent quality, since the C ₂ content is very low, for example less than 0.1% mol.

On the other hand, the invention provides for the diversion to the column of part of the first fraction of head from the first separator before the expansion step in the turbine. This second derivative fraction is cooled and liquefied before introduction into the. column. This procedure makes it possible to limit the quantity of recycled and liquefied gas mentioned above and to reduce the associated compression costs.

The invention can also provide that a second sampling fraction is taken from the first overhead fraction, and that this second sampling fraction is introduced, after cooling and liquefaction, into the upper part of the distillation column.

According to a possible embodiment of the invention, the second sampling fraction is cooled and partially condensed then separated in a third flask into a fourth relatively more volatile overhead fraction, which is cooled and liquefied and then introduced into the upper part of the distillation column, and in a fourth fraction of the foot which is relatively less volatile, which is reheated and then separated in a fourth flask into a fifth fraction of the head which is relatively more volatile which is cooled and liquefied and then introduced into the upper part of the distillation column, and a fifth fraction of the foot which is relatively less volatile which is heated and then sent to the second balloon.

The invention may further provide that the lower part of the distillation column comprises a plurality of stages connected in pairs to one or a plurality of lateral reboilers. The invention can also provide for the second overhead fraction, to obtain the light final fraction, either, after leaving the distillation column, successively subjected to reheating, to a first compression in a first compressor coupled to the expansion turbine, to a second compression in a second compressor, and to cooling. The invention can also provide that the upper part of the distillation column comprises at least two successive stages, the first of which is the lowest and that the fifth head fraction is introduced above the first stage.

The invention can also provide that the upper part of the distillation column comprises at least three successive stages, the first of which is the lowest and that the fifth head fraction is introduced above the second stage.

The invention can also provide that the upper part of the distillation column comprises at least two successive stages, the first of which is the lowest and that the second sampling fraction is introduced above the first stage.

The invention may also provide that the upper part of the distillation column comprises at least three stages, the first of which is the lowest, into which the first sampling fraction is introduced into a lower part of the last stage, and that the third head fraction is introduced below the top floor.

The invention can finally provide that the third overhead fraction is introduced on the first stage of the upper part of the distillation column.

The invention may also provide that the middle part of the distillation column comprises at least two successive stages, the first of which is the lowest and in which the third fraction of the bottom is introduced at least on the first stage, and that the first fraction head is introduced above the first floor.

According to a second of its aspects, the invention relates to a gas enriched in methane obtained by the present process as well as a liquefied gas enriched in C ₂ and higher hydrocarbons, obtained by the present process. According to a third of its aspects, the invention relates to an installation for separating a pressure-cooled mixture containing methane and C ₂ and higher hydrocarbons, into a light final fraction enriched in methane and a heavy final fraction enriched in hydrocarbons. in C ₂ and above, comprising means for carrying out a first step (I) in which (la) the said mixture cooled under pressure is separated, in a first flask, into a first fraction of the head which is relatively more volatile, and a first fraction of relatively less volatile base, in which (Ib) the first fraction of the base is introduced into a middle part of a distillation column, in which (the) is collected, in a lower part of the column, as a second fraction of foot, the heavy final fraction enriched in C ₂ and higher hydrocarbons, into which (Id) is introduced, after having expanded it in a turbine, the first f overhead reaction in an upper part of the distillation column, in which (the) a second head fraction enriched in methane is collected in the upper part of the column, in which (If) the second fraction of head, for obtaining the light final fraction, compression and cooling, and in which (Ig) a light final fraction is taken from a • first sampling fraction, this installation comprising means for performing a second step (II) into which (lia) the first sampling fraction is introduced, after cooling and liquefaction, in the upper part of the distillation column, this installation comprising means for performing a third step (III) in which (Illa) is subjects the first fraction of a foot to a plurality of substeps including reheating, passage through a second balloon, and separation into a third fraction of t relatively more volatile you, and a third bottom fraction relatively less volatile, in which (IIIb) the third fraction of the bottom is introduced into the middle part of the distillation column, and in which (IIIc) is. introduces the third overhead fraction, after cooling and liquefaction, in the upper part of the distillation column.

The invention will be better understood and other objects, characteristics, details and advantages thereof will appear more clearly during the description which follows with reference to the appended schematic drawings, given solely by way of non-limiting example and wherein :

FIG. 1 represents a functional block diagram of an installation in accordance with a possible embodiment of the invention; and

FIG. 2 represents a functional block diagram of an installation in accordance with another preferred embodiment of the invention.

On these two figures, one can read in particular the symbols “FC” which means “flow controller”,

"GT" which means "gas turbine", "LC" which means "liquid level controller", "PC" which means "pressure controller", "SC" which means "speed controller" and "TC" which means "temperature controller".

For the sake of clarity and conciseness, the pipes used in the installations of FIGS. 1 and 2 will be indicated by the same reference signs as the gaseous fractions which circulate there. Referring to Figure 1, the installation shown is intended to treat a dry natural gas, in particular to isolate a fraction composed mainly of methane essentially free of C ₂ and higher hydrocarbons on the one hand, and a fraction composed mainly of C ₂ and higher hydrocarbons essentially free of methane, on the other hand. Dry natural gas 14 is first separated into a fraction 15 which is cooled in a heat exchanger El, and into a fraction 16 which is sent into a pipe. The circulation of fraction 16 is regulated by a controlled valve 17, the opening of which varies as a function of the temperature of fraction 45. At the outlet of the exchanger El, fraction 15 is mixed with fraction 16 to give a fraction 18 cooled. The fraction 18 is then introduced into a liquid / gas separator tank B 1 in which this fraction 18 is separated into a first fraction of the top 3 which is relatively more volatile, and a first fraction of the bottom 4 which is relatively less volatile.

The first overhead fraction 3 is expanded in a turbine Tl to provide a relaxed fraction 19 which is introduced into the middle part of a distillation column C1. Next, on the one hand, it is collected in a lower part of the column of distillation Cl, as the second fraction of foot 2, the final heavy fraction 2 enriched in hydrocarbons in C ₂ and higher. This heavy final fraction 2 is transported in a pipe comprising a controlled opening valve 60, the opening of which depends on the level of liquid contained at the bottom of the column C1. On the other hand, it is collected in an upper part of the distillation column Cl, a second overhead fraction 5 enriched in methane. This second overhead fraction 5 is then reheated in the exchanger El to provide the reheated fraction 20, then is subjected to a first compression in a first compressor K1 coupled to the turbine Tl to provide a compressed fraction 21. The fraction 21 is then subjected to a second compression in a second compressor K2 powered by a gas turbine whose speed is regulated by a speed controller slaved to a pressure controller connected to the pipe carrying the second head fraction 5, to provide another compressed fraction 22. The latter is then cooled by air in a heat exchanger A1 to provide a compressed and cooled fraction 23.

Fraction 23 is then divided into a first sampling fraction 6 and a light final fraction 1 enriched in methane. The first sampling fraction 6 is then cooled and liquefied in the heat exchanger El to give a cooled fraction 24 which is conveyed in a pipe comprising a controlled valve 25 with opening dependent on the flow rate, then is introduced into the upper part of the column distillation Cl.

Is taken from ^"the first overhead fraction .3 second sample fraction 9 is cooled and liquefied in the heat exchanger El to provide a cooled fraction 26. The latter is conveyed in a conduit comprising a valve 27 controlled to open dependent on the flow rate, then is introduced into the upper part of the distillation column C1. The first fraction of bottom 4 is transported in a pipe which includes a controlled valve 28 whose opening depends on the level of liquid in the bottom of the separator flask Bl. The first bottom fraction 4 is then reheated in the exchanger El to provide a reheated fraction 29. The fraction 29 is then introduced into a liquid / gas separator flask B2 to be separated into a third overhead fraction 7 which is relatively more volatile , and a third fraction of foot 8 relatively less volatile. The third fraction of foot 8 is transported in a pipe q ui comprises a controlled valve 30, the opening of which depends on the level of liquid in the bottom of the separator flask B2. The third bottom fraction 8 is then introduced into the middle part of the distillation column C1. The third top fraction 7 is cooled and liquefied in the exchanger El to give a cooled fraction 31. The latter is conveyed in a pipe comprising a controlled valve 32 with controlled opening as a function of the pressure, then is introduced into the distillation column C1.

The distillation column C1 has in its lower part several stages which are linked in pairs by heating circuits 33, 34, 35 which are individually connected to the heat exchanger El.

Each of these heating circuits constitutes a lateral reboiler. The regulation of the fluid circulation temperature in each of these circuits 33, 34,

35 is carried out using controlled opening valves positioned on bypass pipes which do not pass through the exchanger El. The opening of these valves is controlled by temperature controllers connected to the pipes. These controllers, respectively 36, 37, 38, are positioned downstream of the fraction mixing zone after they have passed through the exchanger E1 and / or the bypass lines.

Referring now to FIG. 2, it can be seen that most of the elements contained in FIG. 1 are found in FIG. 2, except in particular for the addition of a circuit comprising two separation tanks.

Thus, in the same way as for FIG. 1, the installation shown is intended to treat a dry natural gas, in particular to isolate a fraction thereof composed mainly of methane essentially free of C ₂ and higher hydrocarbons on the one hand , and a fraction composed mainly of C ₂ and higher hydrocarbons essentially free of methane, on the other hand.

Dry natural gas 14 is first separated into a fraction 15 which is cooled in a heat exchanger El, and into a fraction 16 which is sent into a pipe. The circulation of fraction 16 is regulated by a controlled valve 17, the opening of which varies as a function of the temperature of fraction 45. At the outlet of the exchanger El, the fraction 15 is mixed with the fraction 16 to give a cooled fraction 18. The fraction 18 is then introduced into a flask, liquid / gas separator B 1 in which this fraction 18 is separated into a first fraction of head 3 relatively more volatile, and a first fraction of foot 4 relatively less volatile. The first overhead fraction 3 is expanded in a turbine Tl to provide a relaxed fraction 19 which is introduced into the middle part of a distillation column C1. Next, on the one hand, it is collected in a lower part of the distillation column Cl, as the second fraction of foot 2, the final heavy fraction 2 enriched in C ₂ and higher hydrocarbons. This heavy final fraction 2 is transported in a pipe comprising a controlled opening valve 60, the opening of which depends on the level of liquid contained at the bottom of the column C1. On the other hand, a column is collected in an upper part of the column. distillation Cl, a second overhead fraction 5 enriched in methane. This second top fraction 5 is then reheated in the exchanger El to provide a reheated fraction 20, then is subjected to a first compression in a first compressor K1 coupled to the turbine T1 to provide a compressed fraction 21. The fraction 21 is then subjected to a second compression in a second K2 compressor powered by a gas turbine, the speed of which is regulated by a speed controller controlled by a pressure controller connected to the pipe carrying the second head fraction 5, to provide another compressed fraction 22. The latter is then cooled by air in a heat exchanger A1 to provide a compressed and cooled fraction 23.

Fraction 23 is then divided into a first sampling fraction 6 and a light final fraction 1 enriched in methane. The first sampling fraction 6 is then cooled in the exchanger thermal El to give a cooled fraction 24 which is conveyed in a pipe comprising a controlled valve 25 with opening dependent on the flow rate, then is introduced into the upper part of the distillation column Cl.

A second sampling fraction 9 is taken from the first overhead fraction 3 which is cooled in one heat exchanger El to provide a cooled fraction 26. The latter is conveyed in a pipe which, unlike FIG. 1, comprises a controlled valve 39 with opening dependent on the flow rate. The cooled fraction 26 is then introduced into a liquid / gas separator flask B3 to be separated into a fourth overhead fraction 10 relatively more volatile, and a fourth bottom fraction 11 relatively less volatile.

The fourth overhead fraction collected is then cooled in the exchanger El to give a cooled and liquefied fraction 40. The cooled and liquefied fraction 40 is then conveyed in a pipe comprising a controlled valve 27 with opening dependent on the flow rate, then is introduced into the upper part of the distillation column C1. The fourth fraction of the bottom 11 is transported in a pipe which includes a controlled valve 41 whose opening depends on the level of liquid in the bottom of the separator flask B3. The fourth fraction of the foot 11 is then reheated in the exchanger El to give a reheated fraction 42. This reheated fraction 42 is separated in a fourth flask B4 into a fifth relatively more volatile head fraction 12 and a fifth relatively less foot fraction volatile 13. The fifth overhead fraction 12 is cooled and liquefied in one exchanger El to produce a cooled and liquefied fraction 43. The latter is then transported in a pipe which comprises a controlled valve 44, the opening of which depends on the pressure in the pipe, then is introduced into the upper part of the distillation column C1. The fifth fraction of the foot relatively less volatile 13 is transported in a pipe comprising an opening valve 62 controlled by a liquid level controller contained in the flask B4.

The first fraction of foot 4 is transported in a pipe which includes a controlled valve 28, the opening of which depends on the level of liquid in the bottom of the separating flask Bl. The first fraction of foot 4 and the fifth fraction of foot 13 are then combined to give a mixed fraction 63 which is reheated in the heat exchanger El to provide a reheated fraction 29. The fraction 29 is then introduced into a liquid / gas separator flask B2 to be separated into a third overhead fraction 7 which is relatively more volatile, and a third bottom fraction 8 which is relatively less volatile.

The third fraction of the bottom 8 is transported in a pipe which includes a controlled valve 30 whose opening depends on the level of liquid in the bottom of the separator flask B2. The third bottom fraction 8 is then introduced into the middle part of the distillation column C1. The third top fraction 7 is cooled and liquefied in the exchanger El to give a cooled and liquefied fraction 31. The latter is conveyed in a pipe comprising a controlled opening valve 32 as a function of the pressure, then is introduced into the distillation column Cl.

The distillation column C1 has in its lower part several plates which are linked in pairs by heating circuits 33, 34, 35 which are individually connected to the heat exchanger El. Each of these heating circuits constitutes a lateral reboiler. The temperature regulation of fluid circulation in each of these circuits 33, 34, 35 is carried out using controlled opening valves positioned on bypass pipes which do not. do not pass through the exchanger El. The opening of these valves is controlled by temperature controllers connected to the pipes. These controllers, respectively 36, 37, 38, are positioned downstream of the fraction mixing zone after they have passed through the exchanger E1 and / or the bypass lines. The ethane extraction process using an installation according to diagram 1 makes it possible to recover more than 99% of the ethane contained in a natural gas.

According to a modeling of the installation in operation of diagram 1, the load of dry natural gas (14) at 24 ° C and 62 bar whose flow rate is 15,000 kmol / h, and composed of 0.4998% mol of C0 ₂ , .3499 mol% N ₂ 89.5642% mol of methane, _5/2579 mol% of ethane, 2.3790 mol% of propane, 0.5398 mol% of isobutane, 0.6597 mol% n-butane, 0.2399 mol% of isopentane, 0.1899 mol% of n-pentane, 0.1899 mol% of n-hexane, 0.1000 mol% of n-heptane, 0.0300 mol% of n -octane is cooled and partially condensed in the heat exchanger El to -42 ° C and 61 bar to form fraction 18. The liquid and gaseous phases are separated in the flask Bl. The first overhead fraction 3 which is a current of 13,776 kmol / h, is divided into two currents:

(a) the main stream 45, which has a flow rate of 11,471 kmol / h, is expanded in the turbine Tl to a pressure of 23.20 bar. The dynamic expansion makes it possible to recover 3087 kW of energy and allows this current to be cooled down to a temperature of -83.41 ° C. This stream 19, which is partially condensed, is sent to the column Cl. The stream 19 enters this column on a stage 46 which is the tenth stage starting from the highest stage of the column Cl. Its pressure inlet is 23.05 bar and its temperature is -83.57 ° C. (b) the secondary stream 9 of 2305 kmol / h, which is liquefied and cooled to -101.40 ° C in the exchanger El to form the fraction 26. This fraction 26 which. comprises 4.55 mol% of ethane is expanded at 23.20 bar at a temperature of -101.68 ° C and is then introduced into a stage 47 of column C1 which is the fifth stage starting from the most high from the column.

The first fraction of foot 4 of balloon Bl, the flow rate of which is 1224 kmol / h and which comprises 54.27% mol of methane and 13.24% mol of ethane, is expanded to a pressure of 40.0 bar and then is reheated in the exchanger El from -52.98 ° C to -38.00 ° C to obtain fraction 29. The latter is introduced into the separation flask B2. The top fraction 7 after the ball B2 with a flow rate of 439 kmol / h and the ethane content is 6.21 mol%, is cooled and ^'liquefied -38.00 ° C - 101.40 ° C , to obtain fraction 31. The latter is then expanded to 23.2 bar and -101.47 ° C, then introduced into column C1 on a stage 48 which is the sixth stage starting from the highest stage of the column.

The bottom fraction or bottom fraction 8, whose flow rate is 784 kmol / h and the ethane content is 17.18% mol, is expanded to 23.2 bar and -46.46 ° C and then introduced into the column C1 on a stage 49 which is the twelfth stage starting from the highest stage of the column.

Column C1 produces the top fraction 5 at a pressure of 23 bar and a temperature of -103.71 ° C with a flow rate of 15510 kmol / h. This top fraction 5 only contains 0.05 mol% of ethane.

The overhead fraction 5 is heated in the exchanger El to provide a fraction 20 at a temperature of 17.96 ° C and a pressure of 22.0 bar. This fraction 20 is compressed in the compressor K1 coupled to the turbine T1. The power recovered by the turbine is used to compress fraction 20 to give the compressed fraction 21 at a temperature of 38.80 ° C and a pressure of 27.67 bar. This last fraction is then compressed in the main compressor K2 to give fraction 22 at a pressure of 63.76 bar and a temperature of 118.22 ° C. The compressor K2 is driven by the gas turbine GT. The fraction 22 is then cooled in the air cooler A1 to provide the fraction 23 at a temperature of 40.00 ° C and a pressure of 63.06 bar. Fraction 23 is then separated on the one hand into the main fraction 1 at a rate of 13,510 kmol / h which is then sent in a gas pipeline to be then delivered to industrial customers, and on the other hand into the bypass fraction 6 at a rate of 2000 kmol / h. Fraction 1 is composed of 99.3849 mol% of methane and 0.0481% mol of ethane, 0.0000% mol of propane and higher alkanes, 0.1785% mol of C0 ₂ and 0.3885% mol of N ₂ .

The bypass fraction 6 is recycled to the heat exchanger El to provide the fraction 24 cooled to -101.40 ° C under 62.06 bar. The fraction 24 is then expanded to 23.2 bar and -104.18 ° C to be then introduced into the column C1 at a stage 50 which is the first stage starting from the highest stage of the column. Column C1 produces at the bottom the second fraction of foot 2 which contains 99.18% of the ethane contained in the charge of dry natural gas 14, and 100% of the other hydrocarbons initially contained in this charge 14. This fraction 2, available at 19.16 ° C and 23.2 bar contains 3.4365 mol% of C0 ₂ , 0.0000 mol% of N ₂ , 0 _and 5246 mol% of methane, 52.4795 mol% of ethane, 23.9426 mol% of propane, 5.4324% mol of isobutane, 6.6395% mol of n-butane, 2.4144% mol of isopentane, 1.9114% mol of -ripentane, 1.9114% mol of n- hexane, 1.0060 mol% of n-heptane, 0.3018 mol% of n-octane.

Column C1 is provided with lateral reboilers in its lower part, which is located below the stage where fraction 8 is introduced, and comprises a plurality of stages.

Thus, the liquid collected on a tray 52, available at a temperature of -52.67 ° C and a pressure of 23.11 bar, located below a stage 51 which is the thirteenth stage starting from the stage the higher in the column, is led into the lateral reboiler 33. This consists of an integrated circuit in the exchanger El, the flow rate of which is 2,673 kmol / h. This lateral reboiler 33 has a thermal power of 3836 kW. The liquid collected on the tray 52 is then heated to -19.79 ° C and then returned to the column C1 on a tray 53 which corresponds to the bottom of the fourteenth stage starting from the highest stage of the column. The liquid withdrawn from the tray 52 is composed in particular of 24.42% mol of methane and 44.53% mol of ethane.

Likewise, the liquid collected on a tray 55, available at a temperature of 2.84 ° C. and a pressure of 23.17 bar, situated below a stage 54 which is the nineteenth stage starting from the highest stage of the column, is led into the lateral reboiler 34. This consists of an integrated circuit in the exchanger El whose flow rate is 2049 kmol / h. This lateral reboiler 34 has a thermal power of 1500 kW. The liquid collected on the tray 55 is then reheated to 11.01 ° C and then returned to the column C1 on a tray 56 which corresponds to the bottom of the twentieth stage starting from the highest stage of the column. The liquid withdrawn from the tray 55 is composed in particular of 2.84% mol of methane and 57.29% mol of ethane.

Finally, the liquid collected on a tray 58, available at a temperature of 13.32 ° C and a pressure of 23.20 bar, located below a stage 57 which is the twenty-second stage starting from the stage the highest in the column, is led into the column bottom reboiler or lateral reboiler 35. This consists of an integrated circuit in the exchanger El whose flow is 1794 kmol / h. This lateral reboiler 35 has a thermal power of 1146 kW. The liquid collected on the tray 58, composed in particular of 0.93% mol of methane, and 55.89% mol of ethane, is then reheated to 19.16 ° C and then returned to the bottom of the column Cl- in an enclosure 59 which corresponds to the bottom of the twenty-third stage starting from the highest stage of the column. The liquid leaving the tray 58 has the same composition as the product at the bottom of the column 59 and that the product 2 drawn off at the bottom of the column C1.

All of the heat exchanges take place in one cryogenic exchanger E1 which is preferably composed of a battery of exchangers with brazed aluminum plates. The ethane extraction process using an installation according to diagram 2 makes it possible to recover more than 99% of the ethane contained in a natural gas.

According to a modeling of the installation in operation of diagram 2, the load of dry natural gas 14, at a temperature of 24 ° C and a pressure of 62 bar whose flow rate is 15,000 kmol / h, and composed of 0.4998 mol% of C0 ₂ , 0.3499 mol% of N ₂ , 89.5642 mol% of methane, 5.2579 mol% of ethane, 2.3790 mol% of propane, 0.5398 mol% of isobutane, 0 , 6597 mol% of n-butane, 0.2399 mol% of isopentane, 0.1899 mol% of n-pentane, 0.1899 mol% of n-hexane, 0.1000 mol% of n-heptane, 0, 0300 mol% of n-octane is cooled and partially condensed in the heat exchanger El to -42 ° C and 61 bar to form fraction 18. The liquid and gaseous phases are separated in the flask Bl. The first head fraction 3 which is a current of 13,776 kmol / h, is divided into two currents:

(a) the main stream 45 with a flow rate of 11,471 kmol / h, which is expanded in the turbine Tl to a pressure of 23.20 bar. The dynamic expansion makes it possible to recover 3087 kW of energy and allows this current to be cooled down to a temperature of -83.41 ° C. This stream 19, ^' which is partially condensed, is sent to the column Cl. It enters this column on a stage 46 which is the tenth stage starting from the highest stage of column Cl. Its inlet pressure is 23.05 bar and its temperature is -83 57 ° C. (b) the secondary stream 9, with a flow rate of 2305 kmol / h, which is liquefied and cooled to -62.03 ° C in the exchanger El to form fraction 26. This fraction 26 which includes 4, 5% mol of ethane is expanded to 46 bar at a temperature of -72.68 ° C and is then introduced into the third separator flask B3 where the vapor and liquid phases are separated into the fourth overhead fraction 10 and the fourth fraction of foot 11.

The fourth head fraction 10, the flow rate of which is 1,738 kmol / h, comprises 96.15% mol of methane and 2.61% mol of ethane. The latter is then liquefied and cooled to -101.4 ° C in the exchanger El to give the fraction 40. The fraction 40 is then expanded to 23.2 bar at a temperature of -102.99 ° C to be introduced into column C1 has a stage 47 which is the fifth stage starting from the highest stage of the column.

The fourth fraction of foot 11, whose flow rate is 567 kmol / h, comprises 82.11% mol of methane and 10.48% mol of ethane. The latter is then reheated in the exchanger El to a temperature of -55.00 ° C and a pressure of 44.50 bar to be introduced into the fourth separator flask B4 where the liquid and gaseous phases are separated into the fifth fraction of head 12 and the fifth fraction of foot 13.

The fifth overhead fraction 12, the flow rate of which is 420 kmol / h, comprises 91.96% mol of methane and .6.05% mol of ethane. The latter is then liquefied and cooled to -101.4 ° C in the exchanger El to give the fraction 43. The fraction 43 is then expanded to 23.2 bar at a temperature of -101.57 ° C to be introduced into column C1 has a stage 61 which is the sixth stage starting from the highest stage of the column. The fifth fraction of foot 13, the flow rate of which is 146 kmol / h, comprises 53.85% mol of methane and 23.22% mol of ethane. The latter is then mixed with the. first fraction of foot 4 to give fraction 63. Fraction 63 is then heated in the exchanger El from -53.70 ° C to -38.00 ° C and at a pressure of 39.5 bar to give fraction 29 .

The first fraction of foot 4 of balloon B1, the flow rate of which is 1224 kmol / h and which comprises 13.24% mol of ethane, is expanded to a pressure of 40 bar before being mixed with fraction 13.

The fraction 29 is then introduced into the separation flask B2. The overhead fraction 7 from balloon B2, the flow rate of which is 494 kmol / h and the ethane content is 6.72% mol, is cooled and liquefied from - 38 ° C to -101, 4 ° C, to obtain fraction 31. The latter is then expanded to 23.2 bar and then introduced into column C1 on a stage 48 which is the seventh stage starting from the highest stage of the column. The bottom fraction or bottom fraction 8, whose flow rate is 876 kmol / h and the ethane content is 18.58% mol, is expanded to 23.2 bar and -46.76 ° C and then introduced into the column C1 on a stage 49 which is the twelfth stage starting from the highest stage of the column.

Column C1 produces the top fraction 5 at a pressure of 23 bar and a temperature of -103.61 ° C, with a flow rate of 15,308 kmol / h. This top fraction 5 only contains 0.05 mol% of ethane. The top fraction 5 is heated in the exchanger El to provide the fraction 20 at a temperature of 17.48 ° C. and a pressure of 22 bar. This fraction 20 is compressed in the compressor K1 coupled to the turbine Tl. The power recovered by the turbine is used to compress the fraction 20 to give the compressed fraction 21 at a temperature of 38.61 ° C and a pressure of 27.76 bar. This last fraction is then compressed in the main compressor K2 to give fraction 22 at a pressure of 63.76 bar and a temperature of 117.7 ° C. The compressor K2 is driven by the gas turbine GT. The fraction 22 is then cooled in the air cooler A1 to provide the fraction 23 at a temperature of 40.00 ° C and a pressure of 63.06 bar.

Fraction 23 is then separated on the one hand into the main fraction 1 at a rate of 13,517 kmol / h which is then sent in a gas pipeline to be then delivered to industrial customers, and on the other hand into the bypass fraction 6 at a rate from 1790 kmol / h. Fraction 1 is composed of 99.3280 mol% of methane and 0.0485 mol% of ethane, 0.0000 mol% of propane and higher alkanes, 0.2353 mol% of C0 ₂ and 0.3882 mol% of N ₂ .

The bypass fraction 6 is recycled to the heat exchanger El to provide the fraction 24 cooled to -101.4 ° C under a pressure of 62.06 bar. The fraction 24 is then expanded to 23.2 bar for a temperature of -104.17 ° C to be then introduced into the column C1 at a stage 50 which is the first stage starting from the highest stage of the column .

Column C1 produces at the bottom the second fraction of foot 2 which contains 99.18% of the ethane contained in the charge of dry natural gas 14, and 100% of the other hydrocarbons initially contained in this charge 14. This fraction 2, available at 19.90 ° C and 23.2 bar contains 2.9129 mol% of C0 ₂ , 0.0000 mol% of N ₂ , 0.5274 mol% of methane, 52.7625 mol% of ethane, 24.0733 mol% of propane, 5.4620 mol% of isobutane, 6.6758 mol% of n-butane, 2.4276% mol of isopentane, 1.9218% mol of n-pentane, 1.9218% mol of n -hexane, 1.0115 mol% of n-heptane, 0.3034 mol% of n-octane.

Column C1 is provided with lateral reboilers in its lower part, which is located below the stage where fraction 8 is introduced, and comprises a plurality of stages. Thus, the liquid collected on a tray 52, available at a temperature of -51.37 ° C and a pressure of 23.11 bar, located below a stage 51 which is the thirteenth stage starting from the stage the higher of the column, is led into the lateral reboiler 33. This consists of an integrated circuit in the exchanger El whose flow rate is 2560 kmol / h. This lateral reboiler 33 has a thermal power of 3465 kW. The liquid collected on the tray 52 is then heated to -19.80 ° C. and then returned to the column C1 on a tray 53 which corresponds to the bottom of the fourteenth stage starting from the highest stage of the column. The liquid withdrawn from the ^"plate 52 is composed in particular 23.86 mol% methane and 45.10 mol% ethane. Similarly, the liquid collected on a tray 55, available at a temperature of 3.48 ° C and a pressure of 23.17 bar, located below a stage 54 which is the nineteenth stage starting from the highest stage of the column, is led into the lateral reboiler 34. This consists by an integrated circuit in the exchanger El, the flow rate of which is 2044 kmol / h. This lateral reboiler 34 has a thermal power of 1500 kW. The liquid collected on the plate 55 is then heated to 11.71 ° C. and then returned to column C1 on a plate 56 which corresponds to the bottom of the twentieth stage starting from the highest stage of the column. The liquid present on the plate 55 is composed in particular of 2.92% mol of methane and of 57.92 % mol of ethane.

Finally, the liquid collected on a tray 58, available at a temperature of 14.09 ° C and a pressure of 23.20 bar, located below a stage 57 which is the twenty-second stage starting from the stage the highest in the column is led into the column bottom reboiler or lateral reboiler 35. This consists of an integrated circuit in the exchanger El, the flow rate of which is 1788 kmol / h. This lateral reboiler 35 has a thermal power of 1147 kW. The liquid collected on the tray 58 is then heated to 19.90 ° C. and then returned to the bottom 59 of the column Cl. The liquid withdrawn from the tray 58 is composed in particular of 0.94% mol of methane and 56.35% mol of ethane . In the case of using an installation according to the method described in diagram 2, for an ethane recovery identical to that obtained when using an installation according to diagram 1, a reduction in the power of the K2 compressor from 12355 kW to 12130 kW is obtained. Likewise, a reduction in the flow rate of recycled gas in the circuit comprising fraction 6 from 2000 kmol / h to 1790 kmol / h makes it possible to reduce the heat exchanges during the cooling of fraction 6 to obtain fraction 24. There is also a reduction in the carbon dioxide content of the C ₂ + cut:

- According to diagram 1: 3; 4365% mol

- According to diagram 2: 2.9129% mol

This lower level of C0 ₂ thus makes it possible to facilitate a subsequent treatment aimed at at least partially eliminating the carbon dioxide present in the C ₂ cut, drawn off at the bottom of column Cl.

The invention therefore presents an advantage for limiting energy expenditure during the production of purified gases. This object is achieved while allowing a high selectivity of separation of methane and other constituents during the implementation of the process.

Thus, the results obtained by the invention provide significant advantages constituted by a substantial simplification and economy in the production and technology of the equipment and methods of their implementation as well as in the quality of the products obtained by these methods.

Claims

1. Process for the separation of a pressure-cooled mixture containing methane and C ₂ and higher hydrocarbons, into a light final fraction (1) enriched in methane and a heavy final fraction (2) enriched in C ₂ hydrocarbons and upper, comprising a first step (I) in which (la) the said pressure-cooled mixture is separated, in a first balloon (B1), into a first fraction of head (3) relatively more volatile, and a first fraction of foot ( 4) relatively less volatile, in which (Ib) the first fraction of the bottom (4) is introduced into a middle part of a distillation column (Cl), in which (le) is collected, in a lower part of the column , as the second bottom fraction (2), the heavy final fraction (2) enriched in C ₂ and higher hydrocarbons, into which (Id) is introduced, after having expanded it in a turbine (Tl), the first head fraction (3) in the upper part of the distillation column, in which (the) a second head fraction is collected in the upper part of the column

(5) enriched in methane, in which (If) the second top fraction (5) is then subjected, in order to obtain the light final fraction (1), to compression and cooling, and in which (Ig ) a small final fraction (6) is taken from the light final fraction (1), this process comprising a second step

(II) into which (lia) the first sampling fraction (6) is introduced, after cooling and liquefaction, in the upper part of the distillation column, characterized in that it comprises a third step (III) in which ( Illa) the first fraction of the foot (4) is subjected to a plurality of substeps comprising reheating, passage through a second balloon (B2), and separation into a third fraction of the head (7) which is relatively more volatile, and a third fraction of foot (8) relatively less volatile, in which (Illb) the third fraction of foot (8) is introduced in the middle part of the distillation column, and in which (IIIc) the third fraction of head is introduced (7), after cooling and liquefaction, in the upper part of the distillation column.

2. Method according to claim 1, characterized in that fee the first head fraction (3) a second sample fraction (9), and in that there is introduced the second fraction ^'sample (9), after cooling and liquefaction, in the upper part of the ^" distillation ^" column.

3. Method according to claim 2, characterized in that said second sampling fraction (9) is cooled and partially condensed then separated in a third flask (B3) into a fourth relatively more volatile overhead fraction (10), which is cooled and liquefied then introduced into the upper part of the distillation column, and a fourth fraction of the bottom which is relatively less volatile (11), which is reheated then separated in a fourth flask (B4) into a fifth fraction of the head which is relatively more volatile

(12) which is cooled and then introduced into the upper part of the distillation column, and a fifth fraction of the foot which is relatively less volatile (13) which is reheated and then sent to said second flask.

4. Method according to any one of the preceding claims, characterized in that the lower part of the distillation column comprises a plurality of stages connected in pairs to one or a plurality of lateral reboilers.

5. Method according to any one of the preceding claims, characterized in that the second top fraction (5), in order to obtain the light final fraction (1), is, after leaving the distillation column, successively subjected has a reheating, a first compression in a first compressor (K1) coupled to the expansion turbine (Tl), a second compression in a second compressor (K2), and a cooling.

6. Method according to claim 3, characterized in that the upper part of the distillation column comprises at least two successive stages, the first of which is the lowest and the fifth head fraction (12), is introduced above the first stage .

7. Method according to claim 3, characterized in that the upper part of the distillation column comprises at least three successive stages of which the first is the lowest and ^" the fifth head fraction (10), is introduced above the second floor.

8. Method according to claim 2, characterized in that the upper part of the distillation column comprises at least two successive stages, the first of which is the lowest and the second sampling fraction (9), is introduced above the first stage .

9. Method according to any one of the preceding claims, characterized in that the upper part of the distillation column comprises at least three stages, the first of which is the lowest, into which the first sampling fraction (6) is introduced into a lower part of the last stage, and in that the third head fraction (7), is introduced below the last stage.

10. Method according to any one of the preceding claims, characterized in that the third overhead fraction (7) is introduced into the first stage of the upper part of the distillation column.

11. Method according to any one of the preceding claims, characterized in that the middle part of the distillation column comprises at least two successive stages, the first of which is the lowest and in which the third fraction of the bottom (8) is introduced at least on the first stage, and in that the first head fraction (3) is introduced above the first stage.

12. Gas enriched in methane obtained by the process according to one of the preceding claims.

13. Liquefied gas enriched in C ₂ and higher hydrocarbons obtained by the process according to one of claims 1 to 11.

14. Installation for separating a pressure-cooled mixture containing methane and C ₂ and higher hydrocarbons, into a light final fraction (1) enriched in methane and a heavy final fraction (2) enriched in C ₂ hydrocarbons and upper, comprising means for carrying out a first step (I) in which (la) the said pressure-cooled mixture is separated, in a first flask (B1), into a first fraction of head (3) relatively more volatile, and a first relatively less volatile fraction of the bottom (4), in which (Ib) the first fraction of the bottom (4) is introduced into a middle part of a distillation column (Cl), in which (the) is collected, in a part bottom of the column, as the second bottom fraction (2), the heavy final fraction (2) enriched in C ₂ and higher hydrocarbons, into which (Id) is introduced, after having expanded it in a turbine (Tl ), the first fraction of head e (3) in an upper part of the distillation column, in which (le) is collected, in the upper part of the column, a second overhead fraction (5) enriched in methane, in which (If) is then subjected the second top fraction (5), for obtaining the light final fraction (1), under compression and cooling, and from which (Ig) the first final fraction (1) is taken from a sampling (6), this installation comprising means for carrying out a second step (II) into which (ii) the first sampling fraction (6) is introduced, after cooling and liquefaction, in the upper part of the distillation column, characterized in that it comprises means for carrying out a third step (III) in which (Illa) the first fraction of the bottom (4) is subjected to a plurality us-stages comprising a reheating, a passage in a second balloon (B2), and a separation into a third fraction of head (7) relatively more volatile, and a third fraction of foot (8) relatively less volatile, in which (Illb) the third bottom fraction (8) is introduced into the middle part of the distillation column, and into which (IITc) the third top fraction (7) is introduced, after cooling and liquefaction, in the upper part of the distillation column.