The field of the invention relates to a column (extractor) for the liquid-liquid separation of hydrocarbon compounds, such as aromatic compounds (e.g. A6-A11) from extended hydrocarbon cuts (e.g. C6-C11 cut, such as that from an FCC Fluid Catalytic Cracking unit).
A liquid-liquid extraction operation is a key building block of processes performing the separation of hydrocarbon cuts, such as the separation of a mixture of aromatic and non-aromatic compounds. The operating principle is based on the differences in solubility of compounds of a homogeneous liquid feedstock in a suitable solvent (e.g. an aprotic and polar solvent, such as sulfolane or DMSO). The addition of a partially miscible solvent to the feedstock causes the appearance of a second phase to which a portion of the compounds (e.g. aromatic compounds), which are the most soluble constituents, is preferentially transferred.
Typically, liquid-liquid extraction technology uses a liquid-liquid separation column comprising a plurality of perforated trays equipped with one or more weirs per tray, depending on the targeted capacity (mention is made of a one-pass or two-pass tray or a multi-pass tray when there are more than three weirs).
The design rules for a conventional liquid-liquid extraction column consider a reference tray sized according to the maximum flow rates of each phase and the physicochemical properties thereof. This design is then used for the whole column by stacking a plurality of trays, the trays thus all being substantially identical.
The Applicant has identified, however, that the operation of a liquid-liquid extraction column can give rise to substantial variability, notably depending on:
The present invention is directed towards overcoming the abovementioned drawbacks.
In the context described previously, a first object of the present description is to propose a liquid-liquid extraction column allowing:
Surprisingly, the Applicant has identified that particular characteristics of perforated trays, such as the number of holes per tray, allow the hydrodynamics to be controlled along the entire column, ensuring a homogeneous coalesced-layer thickness and thus limiting axial mixing.
This technical solution makes it possible to maintain satisfactory material transfer efficiency on each tray.
According to a first aspect, the abovementioned objects, and also other advantages, are obtained by a liquid-liquid extraction column, comprising the following elements:
According to one or more embodiments, n is between 3 and 30, and x is greater than 1.
According to one or more embodiments, the liquid-liquid extraction column comprises the following elements:
According to one or more embodiments, in the extraction zones Zi where i ranges from 1 to x (i.e. x greater than 1), the ratio of the number of holes per perforated tray in a zone Zi to the number of holes per perforated tray in a zone Zi+1 is between 0.40 and 0.95.
According to one or more embodiments, in the extraction zones Zi where i ranges from 1 to x (i.e. x greater than 1), the ratio of the number of holes per perforated tray in a zone Zi to the number of holes per perforated tray in a zone Zi+1 is between 0.60 and 0.95.
According to one or more embodiments, in the extraction zones Zi where i ranges from 1 to x (i.e. x greater than 1), the ratio of the number of holes per perforated tray in a zone Zi to the number of holes per perforated tray in a zone Zi+1 is between 0.80 and 0.95.
According to one or more embodiments, when x is 1, the ratio of the number of holes per perforated tray of the at least one backwash zone to the number of holes per perforated tray of the zone Z1 is between 0.40 and 0.95, or the ratio of the number of holes per perforated tray in the zone Z1 to the number of holes per perforated tray of the at least one backwash zone is between 0.40 and 0.95.
According to one or more embodiments, the at least one backwash zone is a plurality of zones, from zone Zx+1 to zone (e.g. column bottom zone) Zn, and in which the number of holes per perforated tray is constant from zone Zx+1 to zone Zn.
According to one or more embodiments, the at least one backwash zone is a plurality of zones, from zone Zx+1 to zone (e.g. column bottom zone) Zn, and in which the number of holes per perforated tray increases from zone Zx+1 to zone Zn.
According to one or more embodiments, the at least one backwash zone is a plurality of zones Zj located between the zone Zx+1 and the zone (e.g. column bottom zone) Zn, and in the zones Zj where j ranges from x+1 to n, the ratio of the number of holes per perforated tray in a zone Zj to the number of holes per perforated tray in a zone Zj+1 is between 0.70 and 0.95.
According to one or more embodiments, in the zones Zj where j ranges from x+1 to n, the ratio of the number of holes per perforated tray in a zone Zj to the number of holes per perforated tray in a zone Z1 is between 0.70 et 0.90.
According to one or more embodiments, in the zones Zj where j ranges from x+1 to n, the ratio of the number of holes per perforated tray in a zone Zj to the number of holes per perforated tray in a zone Z1 is between 0.80 et 0.90.
According to one or more embodiments, the number of zones Zi is between 2 and 10 and/or the number of backwash zones is between 1 and 10.
According to one or more embodiments, the number of holes in the perforated trays of the backwash zone Zx+1 is less than, equal to or greater than the number of holes in the perforated trays of the extraction zone Zx.
According to one or more embodiments, the number of holes in the perforated trays of the backwash zone Zx+1 is greater than the number of holes in the perforated trays of the extraction zone Zx.
According to one or more embodiments, each perforated tray has a number of holes of between 3000 and 20 000.
According to one or more embodiments, the ratio of the area of the holes of each tray to the total area of each tray is less than 0.5.
According to one or more embodiments, the diameter of the holes of the trays is between 2 mm and 20 mm.
Embodiments of the liquid-liquid extraction column according to the first aspect and also other characteristics and advantages will become apparent on reading the following description, which is given purely as a non-limiting illustration, and with reference to the following drawings.
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Embodiments of the invention will now be described in detail. In the following detailed description, many specific details are presented in order to provide a deeper understanding of the invention. However, it will be apparent to a person skilled in the art that the invention can be performed without these specific details. In other cases, well-known characteristics have not been described in detail in order to avoid unnecessarily complicating the description.
In the present description, the term “comprise” is synonymous with (means the same as) “include” and “contain”, and is inclusive or open-ended and does not exclude other unrecited elements. It is understood that the term “comprise” includes the exclusive and closed term “consist”. In addition, in the present description, the term “substantially” corresponds to an approximation of ±10%, preferably of ±5%, very preferably of ±2%, of a reference value such as a distance, velocity, flow rate, compound content, temperature, pressure, etc.
With reference to
In addition, in order to increase the yield and purity, two distinct operating zones are defined opposite the injection point of the liquid 2 to be separated:
Specifically with reference to
With reference to
According to one or more embodiments, the perforated trays Pi are one-pass (e.g. one type of weir) or two-pass (e.g. two types of weirs) or multi-pass trays.
The Applicant has identified that the operation of a liquid-liquid extraction column can give rise to significant variations in flow rate and in the physicochemical properties of the phases circulating in the column, and that the use of trays which differ according to their position in the column can lead to ensuring homogeneous efficiency of the column, contrary to the prior art.
According to the invention, with reference to
According to the invention, each extraction and backwash zone comprises at least two trays, each extraction and backwash zone defining the structural characteristics of the perforated trays Pi present in said extraction and backwash zones. Thus, according to the invention, the perforated trays Pi of the same extraction or backwash zone have substantially the same number of holes 9 per perforated tray Pi.
According to one or more embodiments, with reference to
Advantageously, the number of zones Zi and Zj can be defined relative to the flow rate variability and the physicochemical properties of the phase passing through said zones Zi and Zj.
According to one or more embodiments, the total number n of zones is between 2 and 30, preferably between 3 and 30, very preferably between 4 and 24, such as between 4 and 18, in particular between 4 and 8.
In the present description, i, j, x and n are natural integers.
The number of extraction zones Zi can be defined relative to the phase that has the most flow rate variability in the column. According to one or more embodiments, the number of zones Zi (number of zones Z1 to Zx) is between 1 and 10, preferably between 2 and 10, very preferably between 2 and 6, such as between 2 and 4.
The number of backwash zones Zj can be defined relative to the phase that has the most flow rate variability in the column. According to one or more embodiments, the number of backwash zones (number of zones Zx+1 to Zn) is between 1 and 10, preferably between 1 and 6, very preferably between 1 and 4. According to one or more embodiments, the number of backwash zones (number of zones Zx+1 to Zn) is greater than or equal to 2.
According to one or more embodiments, the number of trays per zone Zi and Zj can be determined by the number of actual stages required for the separation divided by the number of zones Zi and Zj.
Control of the flow rate variation of the dispersed phase Advantageously, the liquid-liquid extraction column 1 according to the invention comprises perforated trays Pi comprising a variable number of holes 9 so that the axial velocity (parallel to the central axis Z of the column) of the dispersed phase through the perforations remains substantially constant in the column. Indeed, due to the fluctuation of the flow rate of the dispersed phase and the physicochemical properties of the dispersed phase as it passes through the column, the variation of the number of holes in the perforated trays Pi ensures that a minimum thickness of coalesced layer is maintained and that the hydraulic injection conditions in the column are identical. This solution also reduces the axial mixing of the continuous phase.
Specifically, in order to keep the axial velocity of the dispersed phase through the perforations substantially constant in the column, the liquid-liquid extraction column 1 according to the invention is divided into:
According to the invention, when x is equal to 1, the number of holes in the perforated trays Pi of the at least one backwash zone (e.g. zone Z2) is greater or less than the number of holes in the perforated trays Pi of zone Z1. According to one or more embodiments, when x is equal to 1, the ratio of the number of holes in the perforated trays Pi of the at least one backwash zone (e.g. the zone Z2) to the number of holes in the perforated trays Pi of the zone Z1 is between 0.40 and 0.95, preferably between 0.60 and 0.95, very preferably between 0.80 and 0.95. According to one or more embodiments, when x is equal to 1, the ratio of the number of holes in the perforated trays Pi of the zone Z1 to the number of holes in the perforated trays Pi of the at least one backwash zone (e.g. the zone Z2) is between 0.40 and 0.95, preferably between 0.60 and 0.95, very preferably between 0.80 and 0.95.
According to the invention, when x is greater than 1, in the extraction zones Zi where i ranges from 1 to x (in the extraction sector 7), the number of holes in the perforated trays Pi increases as the value i increases. According to one or more embodiments, in the zones Zi where i ranges from 1 to x, the ratio of the number of holes in the perforated trays Pi of a zone Zi to the number of holes in the perforated trays Pi of a zone Zi+1 is between 0.40 and 0.95, preferably between 0.60 and 0.95, very preferably between 0.80 and 0.95.
According to one or more embodiments, in the zones Zj where j ranges from x+1 to n (in the backwash sector 8), the number of holes 9 in the perforated trays Pi is substantially constant.
According to one or more embodiments, in the zones Zj where j ranges from x+1 to n, the number of holes 9 in the perforated trays Pi increases as the value i increases. According to one or more embodiments, in the zones Zj where j ranges from x+1 to n, the ratio of the number of holes 9 in the perforated trays Pi of a zone Zj to the number of holes 9 in the perforated trays Pi of a zone Zj+1 is between 0.70 and 0.95, preferably between 0.70 and 0.90, very preferably between 0.80 and 0.90.
According to one or more embodiments, the number of holes 9 in the perforated trays Pi of the backwash zone Zx+1 is less than, equal to or greater than the number of holes 9 in the perforated trays Pi of the extraction zone Zx. According to one or more embodiments, the ratio of the number of holes in the perforated trays Pi of the backwash zone Zx+1 to the number of holes in the perforated trays Pi of the extraction zone Zx is between 0.40 and 0.95, preferably between 0.60 and 0.95, very preferably between 0.80 and 0.95. According to one or more embodiments, the ratio of the number of holes in the perforated trays Pi of the extraction zone Zx to the number of holes in the perforated trays Pi of the backwash zone Zx+1 is between 0.40 and 0.95, preferably between 0.60 and 0.95, very preferably between 0.80 and 0.95.
According to one or more embodiments, each perforated tray Pi has a number of holes of between 3000 and 20 000. According to one or more embodiments, for each tray Pi, the ratio of the hole area to the total tray area is less than 0.5. According to one or more embodiments, the ratio of the hole area to the total tray area is between 0.005 and 0.2, such as between 0.01 and 0.1. According to one or more embodiments, the hole size of all the trays in the column is substantially constant. According to one or more embodiments, the diameter of the holes 9 in the trays Pi is between 2 mm and 20 mm, preferably between 4 mm and 15 mm, very preferably between 5 mm and 10 mm.
This example is directed towards describing the effect of adjusting the number of holes on the homogeneity of the axial velocities of the dispersed phase and the height of the coalesced layer.
The column has a diameter of 2.9 m and comprises a succession of 108 perforated trays. The feedstock is injected at intermediate tray No. 47. The heavy solvent is injected at the top of the column at tray 1. The counter solvent is injected at the bottom of the column at tray 108.
Three zones are defined to adjust the number of holes to the variations of flow rate of the dispersed phase along the column:
In the extraction sector 7 between the head tray X=1 and the feed tray X=47, the number of holes in zone Z1 is less than the number of holes in zone Z2: the ratio of the number of holes in zone Z1 to the number of holes in zone Z2 is 0.83.
In the backwash sector 8 between the tray x=48 and the bottom tray x=108, the number of holes in zone Z2 is less than the number of holes in zone Z3: the ratio of the number of holes in zone Z2 to the number of holes in zone Z3 is 0.80.
The adjustment of the number of perforations thus ensures constant performance regardless of variations in the flow rate of the dispersed phase along the column.
The column has a diameter of 2.9 m, a height of 42 m and is composed of a succession of 108 perforated trays. The feedstock is injected at intermediate tray No. 47. The heavy solvent is injected at the top of the column at tray 1. The counter solvent is injected at the bottom of the column at tray 108.
No adjustment is made: the number of holes is constant (5012 holes) and the characteristics of the trays are identical in all points.
Moreover, the non-adjustment of the number of holes leads to velocity heterogeneities through the perforations of the trays: the velocity distribution along the column can vary between 60% and 115% of the reference velocity (standard deviation=0.15). Such functioning leads to a decrease in the interfacial area of more than 50% in the low velocity zones, and thus to degradation of the column efficiency.
Number | Date | Country | Kind |
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FR2114008 | Dec 2021 | FR | national |
Filing Document | Filing Date | Country | Kind |
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PCT/EP2022/085391 | 12/12/2022 | WO |