General rotor for all systems for subjecting fluids to centrifugal acceleration

Abstract

A rotor for all systems for circulating various single-phase fluids or multiphase fluids, ranging from organic or inorganic solvents to CO2 in liquid or supercritical phase in cells connected to each other by passages, subjected to adjustable centrifugal acceleration and comprising precise temperature control for chemical or biochemical reactions and extraction, purification and separation reactions, and for use in chemical and biochemical reactors, this rotor is formed by one or more discs stacked one on top of the other, each disc being made of a circular sector (A3) comprising a circular half-sector (10) and a circular half-sector (11), each circular half-sector being the mirror image of the other with respect to the plane (28) of the circular half-sector (10) after the two circular half-sectors are assembled opposite each other in a sealed manner. When the half-sectors (10 and 11) are joined, the half-channels of the half-sectors with their respective junctions (18A and 19B) form a junction channel.

Description

TECHNICAL FIELD

[0001] The present invention relates to a general rotor for all systems in which a fluid is subjected to centrifugal acceleration, intended to perform any operation requiring the circulation of a single-phase fluid or of a multiphase fluid, for chemical and biochemical reactions, extraction, purification or separation. BACKGROUND

[0002] The following devices have been known for many years: devices consisting of reactors for performing chemical and biochemical reactions, devices for performing extraction operations, devices for performing purification operations, devices for performing separation operations, such as those performed by centrifugal partition chromatography (CPC).

[0003] A first drawback of the prior art relating to operations performed by centrifugal partition chromatography (CPC), extraction operations, purification operations and separation operations is due to the actual design of the cells and of the junction channels connecting the cells in series, hollowed in the thickness of the discs, which makes it necessary to install a sealing element, generally flexible, between each disc, for example Thus, the plane of each cell and of each channel is closed along the plane of the disc, therefore perpendicular to the main axis of each cell. Even if the cells have a rounded shape to facilitate the uniformity of the dispersion, for a better exchange of material between the two phases, due to the elasticity of the sealing element partially inserted into the cell, the plane of the sealing element is at right angles, or even acute, to the cell, which is not conducive to the uniform dispersion of the liquid, and therefore this is a major drawback. Finally, the plane of these flexible sealing elements has, firstly, a certain porosity which leads to the adsorption and subsequent desorption of certain molecules, which can limit the purity of the molecules of interest. Secondly, the plane of the flexible sealing element is subjected to the continuous variation of the pressure of the liquid, deforms and modifies the geometry of the cell over time, leading to the aging of the sealing element, even if measures are attempted to limit this aging.

[0004] A second disadvantage of the prior art relating to centrifugal partition chromatography (CPC) and extraction operations, purification operations and separation operations is due to the fact that the cells are connected to each other by band-shaped channels. It can easily be calculated and verified that, for a given section, a duct of this shape causes a much higher head loss than a duct of the same cylindrical cross-section or of a geometry very close to it. In order to limit the excessive pressure and in some cases for reasons of processing difficulty, it is necessary to increase the thickness of these rectangular channels, thus increasing the excessive volume of said channels. Said channels do not participate in the separation process through which the products to be separated pass, but said channels do increase the passage time by an equivalent amount, and therefore the separation time and the consumption of solvents.

[0005] A third drawback of the prior art relating to centrifugal partition chromatography (CPC) and to extraction operations, purification operations and separation operations is due to the fact that the mass of the rotor disc and therefore the thermal capacity of the rotor disc are not conducive to precise thermal regulation and, more specifically, to the shortest possible thermal time constant, especially during reactor operation. The temperature of the fluid passing through the unit during a reaction, which can be endothermic or exothermic, if not strictly controlled, can greatly harm performance or even trigger safety problems.

[0006] A fourth drawback of the prior art relating to centrifugal partition chromatography (CPC) and to extraction operations, purification operations and separation operations is due to the fact that, in the case of the rotors of the prior art, if the injection volume increases beyond a certain value with respect to the volume of the unit, a hydraulic shock phenomenon, usually called "water hammer", can occur, which partially or totally disrupts the hydrodynamic balance of the first unit, propagates to the last unit of the rotor and ends the manoeuvre.

[0007] According to the techniques used so far, the rotors used in centrifugal partition chromatography (CPC) devices for separating components comprise a series of units over the thickness of the rotor and over the entire circumference of the rotor, arranged in series in the radial direction or in an oblique direction by a set of thin curved ducts connected to the inlet and outlet of each unit, the circuits of all the discs being in communication with each other. The rotation of the stack generates a huge centrifugal acceleration field, which makes it possible, for example, to maintain a liquid phase, called stationary, the mobile phase, if lighter than the stationary phase, penetrating through the stationary phase in a so-called ascending mode, or, if the mobile phase is heavier than the stationary phase, in a so-called descending mode. In this type of device consisting of a series of one or more units in series, a separation is performed on the electrical charge components in a liquid solution comprising at least two components with different partition coefficients, since the electrical charge components are driven at unequal speeds by the mobile phase, which can be any of the liquid phases in the liquid phase.

[0008] The rotors used in these known centrifugal partition chromatography (CPC) devices can be used in all applications requiring a centrifugal acceleration field and very good thermal regulation, in addition to performing purifications, separations and extractions with conventional solvents, but especially with CO2 in the liquid phase or in the supercritical phase in centrifugal partition chromatography (CPC), which are techniques in which molecules are purified and / or separated between two liquid phases, which takes place in each unit, where the good dispersion of the mobile phase arriving through the inlet channel of each unit facilitates the mass transfer.

[0009] When it is wished to build an industrial production device, the person skilled in the art knows how to scale up according to the separation performed on a laboratory device, i.e. the number of units, the volume of said units, the flow rate of the mobile phase, the hydrostatic pressure generated, etc.

[0010] However, since these parameters are relatively numerous and are inevitably subject to errors, the device will operate, but will not be precisely in its optimum state, or will not simply be modified by the techniques of the prior art.

[0011] The devices of the prior art consist of a rotor whose number of cells and volume are defined before the rotor is constructed and cannot be modified afterwards, which excludes the possibility of optimizing for the various applications that can exist. To simplify things, we will stick to the field of CPC separation, i.e.: if the user has a rotor of the prior art consisting of 500 cells and wishes to perform a given separation for which the optimum is 500 cells, everything will work fine. However, for another separation that would require 1000 cells, the separation will only be partially solved. Conversely, in the case of performing another separation using this same rotor with 500 cells, although a rotor with 200 cells would be optimal, the duration of the separation will be multiplied by approximately 2.5, which leads to a loss of time, an increase in solvent consumption and a decrease in productivity at the same rate.

[0012] With regard to the rotor for separation, more particularly in centrifugal partition chromatography (CPC), the present invention essentially provides a significant advantage over known centrifugal partition chromatography (CPC) devices, not only due to the dual use of the rotor, but also due to the ease of use of the rotor and its ease of adaptation to specific operating conditions.

[0013] The present invention provides a universal rotor, making it possible to:

[0014] - first, separate one or more components having different partition coefficients from a liquid mixture, and

[0015] - second, perform a chemical reaction between several components.

[0016] The rotor according to the present invention can also be applied successively to both of the above-mentioned implementations, i.e. a reaction between two or more compounds, then separation of the desired product in the reaction mixture resulting from the chemical reaction or separation of the components contained in the mixture, then chemical reaction of the components obtained with another product.

[0017] Thus, it can be considered to use the present invention for each of these two applications, and for the successive use of these two applications. SUMMARY

[0018] The present invention provides a general rotor for operations requiring a fluid to be subjected to centrifugal acceleration involving the circulation of a single-phase fluid or a multiphase fluid, for processes including purification, extraction, separation, centrifugal partition chromatography (CPC), liquid-liquid extraction, chemical reactions and biochemical reactions, in particular for continuous operations.

[0019] The rotor according to the present invention can be implemented as a chemical reactor and / or a biochemical reactor, a liquid-liquid extractor, in purification operations, centrifugal partition chromatography (CPC), etc.

[0020] The liquid or solvent phase can include, among others, organic solvents, ionic solvents, NADES (natural deep eutectic solvents), CO2 in liquid or supercritical phase circulating in cells connected to each other by passages, and applied in different fields, such as the field of chemical and biochemical reactions, the field of extraction, the field of purification, the field of separation.

[0021] The present invention provides a general rotor for operations requiring a fluid to be subjected to centrifugal acceleration involving the circulation of a single-phase fluid or a multiphase fluid, for processes including purification, extraction, separation, centrifugal partition chromatography (CPC), liquid-liquid extraction, chemical reactions and biochemical reactions, in particular for continuous operations.

[0022] - said rotor is formed by one or more discs stacked one on top of the other,

[0023] - each of said discs comprises a holder in which an annulus (A1) consisting of one or more assemblies of circular sectors is inserted,

[0024] - in the case of a single circular sector, a space is provided between the two ends of said single circular sector,

[0025] in the case of several circular sectors, a space is arranged between the ends of two adjacent circular sectors,

[0026] - in said space, a coupling connector is inserted,

[0027] - said coupling connector has branching means consisting of passages required by the liquid phase, which enters through an inlet into said coupling connector to be guided to travel through the network of cells up to the outlet of said coupling connector, which is in direct contact with the inlet of the coupling connector of the next disc, and so on up to the outlet of the last disc, which is connected to the outlet of said rotor.

[0028] According to one embodiment of the present application, the rotor is formed by a single circular sector, which comprises a continuous network of cells and is interconnected by channels, both arranged in a plane approximately at the midpoint of the rotor thickness, characterized in that between the two end portions of the rotor there is at least one gap for arranging a junction connector in a sealed manner, which comprises at least one inlet and at least one outlet intended to allow the entry of the liquid mixture into the network of cells and the exit of the mixture from the network of cells, respectively.

[0029] According to another embodiment of the present application, the circular sector is made of two circular half-sectors, each of which is a mirror image of the other, which comprise half-cells and half-channels on their mirror planes, the two half-sectors being assembled face-to-face, preferably by diffusion welding, in a sealed manner to become a circular sector.

[0030] According to yet another embodiment of the present application, the circular sector is preferably made in one piece, for example directly by additive construction.

[0031] According to yet another embodiment of the present application, the single circular sector comprises one or more ducts having a substantially rectangular cross-section in its thickness, each of which is arranged in a circular pattern, usually three, is delimited by concentric walls, and is arranged so that the average radius of each of the ducts arranged in a circular pattern substantially corresponds to the average radius corresponding to the average radius of the corresponding network of cells arranged in a circular pattern, for each network of cells to circulate the temperature control fluid or thermostatic fluid in the ducts in the same way as possible.

[0032] According to one embodiment of the present application, the junction connector comprises the necessary branches so that the incoming temperature control fluid or thermostatic fluid passes through all the ducts connected in series that make up each of the circular sectors that constitute the ring, and then, guided by the junction connector, it passes to the junction connector of the next disc, so as to pass through the ducts connected in series in the same way, and in this way until the outlet of the rotor.

[0033] According to yet another embodiment of the present application, the junction connector also comprises an inlet that allows the entry of the temperature control fluid or thermostatic fluid and an outlet that allows the exit of the temperature control fluid or thermostatic fluid, for the temperature control fluid or thermostatic fluid to pass through at least one temperature control fluid duct or thermostatic fluid duct.

[0034] According to one embodiment of the present application, the cells and channels have walls as thin as possible and are provided with fins, which are themselves integral with the internal walls of the circular sector.

[0035] According to another embodiment of the application, the junction connector comprises at least one inlet and at least one outlet, respectively for allowing the entry of a liquid mixture into the network of cells and the exit of said mixture from the network of cells, so that between the outlet and the inlet, the liquid phase crosses all the cells and channels of the corresponding disc.

[0036] According to yet another embodiment of the application, a junction connector (B6) can be installed instead of the junction connector (A6), in which case a single or multiple way ball valve comprising an "open" position and a "bypass" position is added to the junction connector (B6), so that the position can be chosen so that in the "open" position of said valve, the liquid phase entering at (31) is directed to (32) of said valve, then enters the inlet (13) of the adjacent circular sector, to cross the entire network of cells of the disc and reach (14) of the last circular sector, and then (35), and then (36) of the junction connector, to enter the next adjacent disc at (31) of the junction connector of the next adjacent disc, but if the ball of said valve (42) is in the "bypass" position, the liquid phase entering at (31) is directed directly to (36) without crossing the cells of the relevant disc, the latter being a short circuit, allowing the user to gradually adjust the number of cells in each of their various applications by the number of cells contained in the disc.

[0037] According to yet another embodiment of the application, each circular sector of the ring is formed by two circular half-sectors superimposed face to face or by a stack of such superimpositions, each of these half-sectors comprising half-cells, the angle (20) of these half-cells being replaced by a chamfer forming a rounded surface.

[0038] According to another embodiment of the application, in order to increase the productivity of said rotor in the CPC mode in ascending mode, "n" first cells of said rotor have a volume that decreases according to a determinable function ranging from (V7) to (V), with (V7 > V), V being the constant volume of the majority of the cells of said rotor.

[0039] The application also relates to the use of the universal rotor in an operating context requiring the circulation of a single-phase fluid or of a multiphase fluid, in an operation requiring the fluid to be subjected to centrifugal acceleration for purification, extraction, separation, centrifugal partition chromatography (CPC), liquid-liquid extraction.

[0040] The application also relates to the use of the universal rotor in an operating context requiring the circulation of a single-phase fluid or of a multiphase fluid, in an operation requiring the fluid to be subjected to centrifugal acceleration for chemical or biochemical reactions.

[0041] The application will be better understood by reading the following description of a preferred embodiment given as a simple, non-limiting example, and in connection with the following drawings. BRIEF DESCRIPTION OF DRAWINGS

[0042] Figure 1 A ring Al according to the application is shown schematically in exploded view, consisting of 4 circular sectors 2 to 5 and a junction connector 6.

[0043] Figure 2 is an exploded schematic view of the ring Al to be inserted into a centring holder with axis 8 to form a disc A2.

[0044] Figure 3 is an exploded schematic view of an example of a circular sector A3 according to the application, consisting of an assembly of two circular half-sectors 10 and 11 forming the circular sector.

[0045] Figure 4 is a schematic view of an example of a static junction connector A6 according to the application, adjacent to two circular sectors of two unit networks with different volumes, and of a path 37-38 for circulation of a fluid used to control the temperature in the rotor.

[0046] Figure 5 is a schematic view of another example of a junction connector B6 with two-position valves according to the application, adjacent to two circular sectors of two unit networks with different volumes, and of a path for circulation of a temperature control fluid for the temperature of the rotor.

[0047] Figure 6A is a schematic view of three cross-sections showing an example of a rotor according to an embodiment of the application, limited to 6 discs, so as not to hinder the drawings showing in detail the various fluid paths of the moving phase and of the thermal phase.

[0048] Figure 6B is a schematic cross-sectional view of a two-position valve installed in a junction connector, in a plane perpendicular to the axis of the two-position valve and passing through one of the distribution channels.

[0049] Figure 7 is a schematic view of an example of the structure of a rotor on a vertical axis according to an embodiment of the application.

[0050] Figure 8 is a schematic view of an example illustrating the possibility of simply adding or removing discs from a rotor according to the application, to adapt the geometry of the rotor to various applications, to perform after-sales service or for any other reason.

[0051] Figure 9This is a schematic diagram of an example arrangement of cells in a CPC rotor, which allows for an increase in injectable volume. Detailed Implementation

[0052] Figure 1 An example of a ring A1 of a rotor according to the invention, consisting of four circular sectors 2, 3, 4, 5 and a connecting connector 6, is shown.

[0053] The following describes it in more detail Figure 2 , Figure 3 , Figure 4 , Figure 5 Figure 6 shows one or more concentric unit networks formed on the surface of a circular semi-sector. The face-to-face assembly of these concentric unit networks forms the circular sector A3. These units are interconnected in series via channels. Figure 3 .

[0054] Figure 1 The ring A1 shown includes a set of open circular sectors 2 to 5, each circular sector having two ends and including at least one cell network concentric with the axis of the circular sector, the cell network being formed on a plane approximately at the midpoint of the thickness of the circular sector. Figure 1 In the example shown, ring A1 is formed by multiple distinct circular sectors 2 to 6, more precisely by four distinct circular sectors 2 to 5 connected to connector 6. Each circular sector comprises a portion of one or more unit networks assembled in pairs in a sealed manner to ensure the continuity of the unit networks, as will be described in more detail below. Of course, the number of circular sectors can vary. In particular, the device may include a single circular sector, which then comprises all or more unit networks of ring A1.

[0055] In the case of several circular sectors 2 to 5, the two ends of circular sectors 2 and 5 correspond to an end of the first circular sector 2 that is not connected to other circular sectors and an end of the last circular sector 5 that is not connected to other circular sectors.

[0056] In the case of a single circular sector, the two ends of the circular sector correspond to the ends of a component of several circular sectors.

[0057] The coupling connectors 6 are interposed in a sealed manner between the two ends of the assembly of circular sectors 2 to 5. In one embodiment of the application, this coupling connector makes it possible to allow the injected sample and the mobile phase to enter into the ring Al, and then, after they have passed through all the cells, to direct them into the coupling connector of the adjacent ring, which in turn performs the same function, and so on until the last ring of the rotor constituted by the stack of discs. The various components of the sample entrained by the mobile phase are separated during their passage through the cells and channels, for example in the case of a CPC separation application, and then detected and / or collected by one of the well-known means used in liquid / liquid centrifugal partition chromatography CPC or for applications performed in other fields. According to the application, the coupling connector can have other functions, which will be presented in the detailed description of Figure 4 and Figure 5 .

[0058] Figure 2 A non-limiting embodiment of the assembly of the ring Al in a support or centring retainer to form the rotor disc A2 is shown in exploded view. The mechanical tolerance between the inner diameter of the centring retainer and the outer diameter of the ring Al must be such that the ring Al is tightly clamped by the centring retainer 7 to ensure good mechanical strength and good sealing between the various components making up the ring Al. For example, the insertion operation can be carried out by the method of thermal expansion by the temperature difference between the two parts to be assembled. The openings 9 are arranged on the plane of the centring retainer to be able to extract the ring Al using a press. The central hole 8 of the centring retainer is a sliding fit with minimal play for optimal centring on the rotor shaft 85 and allows the central hole 8 to slide on said shaft of said rotor, see Figure 7 and Figure 8 Each rotor disc A2 previously filled with liquid is statically and dynamically balanced until the acceleration is slightly greater than the maximum expected acceleration at the time the device was designed.

[0059] Figure 3A3 according to one embodiment of the application is shown in exploded view, the circular sector A3 being composed of a first circular half-sector 10 and a second circular half-sector 11, each circular half-sector being the mirror image of the other with respect to the plane 28 of said circular half-sector 10; the result is the circular sector A3 after the first circular half-sector 10 and the second circular half-sector 11 have been assembled face to face in a leak-proof manner. In this embodiment of the application, the circular sector comprises two networks, each network having twenty cells, one of the two networks being composed of cells 26 having a volume V and the other network being composed of cells 27 having a volume 8V. For a better understanding of the figures, it will be noted that, for example, a cell 27 is composed of an assembly of a first half-cell 27A formed on the first circular half-sector 10 and of a second half-cell 27B formed on the second circular half-sector 11. The same applies to the channels. Said half-cells are not necessarily images of each other, since they can be asymmetrical, provided that they have strictly the same profile at the contact plane 28 between the two half-sectors.

[0060] See along Figure 3The section taken by the line B-B intercepts the passage 18 and 19 of the respective junction unit of the network, which has a cross section adapted to the necessary flow rate required for the operation of the unit. The two circular sectors are positioned facing each other as precisely as possible, for example by means of two lugs 22 inserted into two cylindrical holes of the circular sector 10 in interference fit. In the second mirror circular sector 11, two holes are formed for the sliding fit, one of which is cylindrical and the other is elliptical, corresponding to the position of the lugs inserted into the circular sector 10, to perform the unconstrained assembly of the two circular sectors, for example by diffusion welding. Preferably, the lugs are made of a material with the same material grade as that used to make the circular sectors, or with a thermal expansion coefficient as close as possible to that of the material used to make the circular sectors, to prevent any mechanical stresses from deforming due to thermal expansion during the welding operation. When operating in the descending mode, the mobile phase and the sample enter into the circular sector A3 via the inlet 13 or 15 and through the inter-sector seal or gasket 17 corresponding to the selected network of units. The respective outlets are 14 and 16, respectively. The gasket 23 forms a seal between the circular sector and the junction connector 6 for possible circulation of the thermal fluid inside the two circular sectors, see reference 12, which in this particular embodiment occurs in three separate conduits 12A, 12B and 12C separated by the walls 12F, 12AB, 12BC and 12D, each having a pattern with the same center as one of the three networks of units arranged in a circular pattern. These units have thin walls and are equipped with fins, which make it possible to reduce the thermal resistance between the temperature control fluid or thermostatic fluid and the liquid phase passing through the units and the passages, while increasing the mechanical strength of the units.

[0061] According to the present application, the units are made with rounded surfaces or chamfers 20 instead of having sharp corners, which significantly reduce the fluid dynamic operation and therefore the performance of the device, as shown in detail in the enlarged view of the half-unit 27A. This way can be advantageously applied to all conceivable geometries of the units, whether they are symmetrical or asymmetrical and their various applications. The cross section of the passages 18 and 19 of the junction units is advantageously circular, also for good fluid dynamic operation. However, in the case of conventional machining of the passages, for reasons of ease of machining and / or passage surface state, it would be possible to have the passages 18 and 19 with a polygonal cross section, for example square, noting the rounding of all the angles to obtain a cross section as close as possible to a circular cross section.

[0062] Figure 4An embodiment of a coupling connector with fixed configuration is shown, in this case, the fixed configuration connector A6 comprises one or more inlets 29 to 31 for the liquid phase and the corresponding outlets 30 to 32, which are connected in descending mode to the ports 15 and 13 of the circular sector A3 adjacent to the coupling connector, respectively. The mobile phase passes through the network of selected cells 26 or 27 and the network of channels 18 or 19 that couple them with the circular sector, exits at the ports 16 or 14 connected to the inlets 15 and 13 of the next circular sector, and so on until the last circular sector of the ring adjacent to the second end of the coupling connector, where the mobile phase enters at the ports 33 or 35, exits through the ports 34 or 36 of the coupling connector, and enters the adjacent coupling connector of the next disc at the ports 29 or 31, and in this way advances from one disc to another until the last disc of the rotor, where the outlets 34 or 36 are connected to the outlets 54 or 56 of the rotor.

[0063] When selecting the inlet / outlet of the network of cells, it is recommended to seal the other network at the flange of the rotor by means of two stops to avoid any loss of liquid phase during operation, which could cause dynamic imbalances when the rotor is rotating.

[0064] To help understanding, Figure 4 With Figure 5 The coupling connectors A6 and B6 between two circular sectors have been illustrated, the circular sector on the left is translucent to better explain the exemplary embodiment, here with fins and concentric walls 12AB and 12BC, the circular sector on the right is opaque to show the connection between the network of channels and cells of the coupling connector with the circular sectors A3 (2 and 5).

[0065] Figure 3 , Figure 4 And Figure 5and the junction connector A6 or B6, taken along the line C-C, in cross section, comprises an inlet 37 for the injection of a temperature control fluid or a thermostatic fluid which is conducted through a channel 37B into the conduit 12A of the first circular sector delimited by the concentric walls 12F and 12AB, then through the channels of the successive circular sectors up to the junction connector, through a channel 37C which leads into the conduit 12B delimited by the walls 12AB and 12BC, through the conduit 12B up to the junction connector which conducts the temperature control fluid or the thermostatic fluid, via a channel 37D thereof, to the inlet of the conduit 12C delimited by the concentric walls 12BC and 12E, through said conduit up to the junction connector and out through a connection 38 which is arranged on the same axis as the inlet 37 and on the opposite end to the inlet 38 of the junction connector of the next disc in the stack, the temperature control fluid or the thermostatic fluid continuing through the stack until it reaches the outlet of the last rotor disc which leads it to the outlet 58 or 59.

[0066] Figure 5 A second main embodiment of the junction connector 6 according to the application is shown, in this case B6. The junction connector B6 has all the functions of the junction connector A6 of Figure 4 , with the same reference numerals, with the exception of a valve 42, for example of the ball valve type 41, which has two positions: Run and Bypass.

[0067] In the Run position, the mobile phase which enters the junction connector through the port 29 or 31 is directed by the valve at the port 30 or 32 to enter the first adjacent circular sector via the port 15 or 13 (respectively 29, 30, 15 or 29, 31, 13) and then pass through the entire selected network of discs to the inlet 33 or 35 of the circular sector and to the outlet 34 or 36 of the disc and then into the adjacent junction connector of the next disc. Figure 3 ) of the disc and then into the adjacent junction connector of the next disc.

[0068] In the Bypass position, the mobile phase which has previously filled the relevant cell network is trapped therein. The mobile phase which enters at the port 29 or 31 of said junction connector is directed directly by the ball valve towards the outlet 34 or 36 of the junction connector which is adjacent to the next junction connector of the stack. This embodiment makes it possible for the user to adjust the number of active cells of the rotor step by step to be consistent with the number of cells contained in the disc, by turning the ball valve 41 by a quarter turn in one direction or the other by means of a screwdriver introduced into the slot 43. The operation of this main embodiment of the application is shown in more detail in the discussion below of Figure 6A and Figure 6B .

[0069] Figure 6A A top view of the rotor according to the application is shown, showing the disc selection valve, and then in three cross-sectional views taken along E1-E1, E2-E2 and E3-E3 as non-limiting examples, the rotor according to the application is shown, formed only by 6 discs Dl, D2, D3, D4, D5 and D6, so as not to overload the drawings.

[0070] By way of non-limiting example, the discs discussed here comprise two concentric independent networks of 80 cells, each of the two networks being formed by cells of different volumes and junction channels, the respective cross-sections of which are adapted to the flow rates required by the cells. By way of non-limiting example, in the present example, the smaller cell volume is V and the other cell volume is 8V.

[0071] The junction connectors 6, whether they are Figure 4 of fixed configuration A6, or associated with Figure 5 the switching valve B6, are directly interchangeable.

[0072] The cross-section E1-E1 is taken along a cutting plane defined by the generatrix of the rotor, which intersects the axis of the valve 41 and the axis of the rotor.

[0073] The cross-section E2-E2 is taken along a cutting plane perpendicular to the cutting E1-E1, passing through the axis of the channels, passing through the switching valve hydraulically connected to the inlets and outlets 56 and 57 and / or 54 and 57 according to the network used.

[0074] The cross-section E3-E3 is taken along a cutting plane perpendicular to the cutting E1-E1 and passing through the axis of the inlets and outlets 58 and 59 of the temperature control fluid or thermostatic fluid.

[0075] The cross-section E1-E1 is an assembly view comprising a double-channel ball valve suitable for the two networks of cells of different volumes V and 8V of the present embodiment. For the use of the double-channel ball valve, the network corresponding to the volume of the selected cell is selected, for example by connecting the movement arriving from the following down mode to the inlet 56, and then the outlet 57 is, for example, the outlet of the rotor to be connected to the detector and fraction collector. It is recommended to connect plugs at the ports 54 and 55 to prevent the escape of the phases in the respective network of cells, so that there is no risk of dynamic imbalance of the rotor when it is rotating. The cross-section E1-E1 also shows the inlet 58 and outlet 59 intended for the circulation of the temperature control fluid or thermostatic fluid used for the rotor.

[0076] The cross-section E2-E2 more precisely shows the hydraulic operation of the "pass" - "bypass" valve, in Figure 6BThe valves mounted on discs D4 and D5 are shown in greater proportion. It can be observed that, as for discs Dl, D2, D3 and D4, the ball valve 41 of the rotor disc is arbitrarily positioned to "pass through" and, as for discs D5 and D6, the ball valve 41 of the rotor disc is arbitrarily positioned to "bypass", which illustrates by way of example only the operation according to the application in which it is desired to use only 4 active unit discs, or 320 active units of the 480 units of the rotor.

[0077] Cross section E3-E3 shows a plane parallel to cross section E2-E2 and passing through the axis of the connector 58-59. The temperature control liquid or thermostatic fluid enters, for example, through the connector 58, then reaches the inlet 37 of the first junction connector A6 or B6. The diverter 60 directs the temperature control liquid or thermostatic fluid towards the temperature control liquid or thermostatic control channel 12A of the adjacent circular sector in the direction of the arrow. After the temperature control liquid or thermostatic fluid has passed through all the conduits 12A, 12B to 12C of the circular sector of the disc, it reaches the conduit 12C, is directed at the port 38 of the diverter 60 of the junction connector and passes directly from the outlet 38 to the inlet 37 of the adjacent junction connector of the next disc until it reaches the outlet 59 of the rotor.

[0078] Figure 6B The path of the mobile phase from the outlet 34 or 36 of the disc D3 is shown in detail. The mobile phase from the valve positioned to "pass through" of the disc D4 enters at the port 46, is then directed through the channel 45 to the port 47 at the inlet of the unit network of the disc D4, then exits at the port 43. The mobile phase travels through the channel 45, reaches the port 49, passes through the connection 49 / 50 and then directly through the channel of the ball 44 of the valve in the "bypass" position of D5 to exit directly at the port 53, which is connected to the inlet 29 or 31 of the junction connector of the adjacent disc D6, which is also in the "bypass" position, so the mobile phase is directed directly to the outlet 55 or 57 of the rotor.

[0079] In this example, the mobile phase thus passes through 320 units of the rotor comprising 480 units. Rotors with more units can be produced to expand the field of application. It can be seen that, for example, by turning the ball 41 of the valve 42 a quarter of a turn, the number of units used in such a rotor can be modified by a number of units corresponding to the number of units contained in each disc and thus make it possible to operate with 80, 160, 240, 320 or 400 units of such a rotor, depending on the requirements of the separation to be performed. If the light mobile phase is connected to the inlet 57, the path in the unit network remains the same but in the ascending mode.

[0080] Figure 7An embodiment of the invention is shown in which the rotor is formed by a stack 95 of discs A2 and in which the rotor shaft 85 is held upright at one of its ends by a suitable assembly arranged in a cylindrical piece 89. A motor 90 provided with a toothed pulley drives the rotor in rotation, the axis of which is also provided with a toothed pulley, the two toothed pulleys being mechanically coupled by a toothed belt 94, which is kept taut by an eccentric tensioner 97. Each end of the shaft 85 is equipped with a hydraulic rotary seal 88, which makes it possible for the mobile phase and temperature control fluid or thermostatic fluid to enter and exit the rotor without some being retained.

[0081] These rotary seals must be adapted to the associated pressures and rotational speeds and must be easily accessible to simplify maintenance, cleaning, replacement of the seals, after-sales service, etc.

[0082] A nut 86 with holes for receiving springs 87 is screwed onto the rotor shaft 85, so that the springs 87 provide sufficient permanent pressure to ensure the sealing of all the seals of the discs constituting the stack of the rotor and so that the assembly is mechanically uniform and stable. The frame carrying this mechanical assembly is fixed to the equipment by dampers 92 provided for this purpose, safety fastenings are added to the equipment for transport, together with mechanical locking means, in compliance with the applicable standards.

[0083] Figure 8 An example of a non-limiting embodiment according to the invention of a rotor resulting from production is shown in detail, for example, comprising a stack or superposition of 12 discs A2, it being specified that the number of discs of the rotor can easily be modified by this example and that this example has proved to be particularly suitable for production equipment. Since production equipment is operated long and frequently on the same application, these production equipment do not necessarily need to be optimized frequently. However, if the equipment considered aims at performing various operations as a function of needs in synthesis, purification, extraction, etc., the embodiment of the invention comprising a "pass-by" valve installed on each disc of the rotor can prove to be very effective. The user can use the valve 42 to quickly optimize the equipment to the closest to the optimum state for each of its various applications.

[0084] For the calculation and construction of production equipment intended for long-term application, the calculation and experimentation of proportional changes derived from measurements performed on a laboratory apparatus should be time-saving and accurate. According to the invention, the laboratory apparatus is preferably equipped with a "pass-through" valve on each disc. However, measurements may be affected to some extent by errors, and industrial rotors constructed on these basis may not be exactly at their optimal state. This deficiency can be easily corrected by the technical flexibility of the invention, as one or more discs can be added or removed, allowing performance to be optimized under actual conditions and by adjusting the necessary number of units. This operation is simplified by constructing the discs using components of circular sectors, which can have more or fewer units as needed.

[0085] Figure 8 View A shows a rotor A5 comprising twelve discs according to the invention, all of which have been pre-balanced and independently. Assuming that one or more discs need to be removed for any reason, let's assume six discs. For this purpose, the upper rotary seal 88 is removed, and the nut 86 and connecting pipe 91 are unscrewed, and the spring 87 is removed. From... Figure 8 A and Figure 8 B shows that flange 93 can be removed, and then the six disks are removed one after another, see Figure 8 B, to reach Figure 8 C, in Figure 8 In C, the rotor containing flange 93 is placed on a stack now consisting of six disks, and then spacers 98 slide on the shaft. The length of spacers 98 will preferably be a binary series in order to limit their number. The height of the minimum spacer is equal to the thickness of the disk. Then nuts 86 are placed and then rotary seals 88 are placed.

[0086] This embodiment, which presents a vertical axis, does not preclude components made of horizontal or hinged axes of rotation, which allow the portion supporting the rotor to be displaced at an angle. Those skilled in the art will understand the use of various devices known in conventional mechanics to put this installation into practice.

[0087] Figure 9 A non-limiting example of another embodiment of the invention is shown, which makes it possible to increase the injectable amount of a sample processed by a rotor in a CPC operation, the rotor comprising a set of identical units of the same volume V.

[0088] Before the rotor inlet, when it is desired to operate in ascending mode (ASC), a cell network with asymptotically increasing volumes is added, and for simplicity, the volume of the first V7 is n times larger than the volume V of the rotor's cells. Between V7 and the first cell V of the same cell network, multiple cells V6, V5, ... V1 are interleaved according to a volume variation pattern to be determined.Figure 9 In particular, for simplicity, this variation is presented in a non-limiting manner according to a linear function. The same applies to the following descending mode DSC operation, in which the same value of the volume of the cells is indicated by way of example.

[0089] According to the present application, it is useful to adopt a disc equipped with valves 42, so that it is possible to connect or not connect all or part of the discs in the rotor of the network of cells comprising different volumes, to regulate the number according to the needs of each application.

[0090] The rotor according to the present application is used in centrifugal partition chromatography CPC operations, thus allowing the separation of the compounds contained in a solution formed by several components. The separation of the sample is based on the distribution coefficient specific to each of the components of the sample between the mobile phase and the stationary phase. This distribution coefficient determines the affinity of each molecule in the mobile phase and in the stationary phase, and therefore also the speed of movement of each molecule in the system. At the end of the purification process, the automatic fraction collector retains all the selected fractions according to the parameters of the program.

[0091] The rotor according to the present application can be used not only in separation operations, but also in reaction operations between components, so that the rotor acts as an enhanced chemical and / or biochemical reactor due to the good mixing that occurs in each of the cells of the cells. The advantage of this system is that a plug flow reactor-like behaviour is obtained, considering that the said general rotor is a series of ideal stirred reactors comprising cells, which is considered to provide the best performance. The reaction can be carried out in a single phase or be biphasic, most relevant when the reactants and products are in different phases.

[0092] The present application breaks radically with the conventional batch process: the double-jacketed stirred tank is the most frequently used tool in more than 50% of the chemical production units in the world. The engineering of the reactor includes two key elements: the kinetics of the reaction and the design of the reactor. The design of the reactor must be carefully considered so that the reaction takes place at its inherent speed, that is to say, whether there is perfect mixing and mass transfer in the reactor.

[0093] Generally, in large stirred tank reactors, the reaction does not proceed at its inherent speed because the reaction is limited by the mixing in the tank, i.e. the reactants are not mixed completely. In this case, the reaction is known to be "limited by mixing". The role of intensification is to reduce or eliminate these limitations so that the reaction can reach its inherent pace. The goal is therefore to ensure that the mixing and heat / mass transfer rates will be relatively fast with respect to the basic kinetics of the process. High accelerations can be obtained as long as the operation in this rotary system requires it. The transfer of chemical syntheses in reactors with plug flow in each phase is then made possible, which makes it possible to minimize the reaction volume (safety of the installation and the operator), to enhance the exchange of materials (mixing, reaction, separation), to regulate and control the temperature with good precision and to add an alarm system in case of over-regulation. Examples include the reduction of benzaldehyde to benzyl alcohol by homogeneous ruthenium catalysis or the reduction of the two-phase esterification of oleic acid to ethyl oleate by lipase (Candida Antarca).

[0094] Liquid / liquid extraction is a fundamental operation in the field of process engineering. Liquid / liquid extraction consists in transferring a solute (molecule of interest) from a so-called "feed" phase to a so-called "extract" phase. These two phases are immiscible or partially miscible. There are many examples in industry, for example with acid-base extraction cycles to produce antibiotics.

Claims

1. A general purpose rotor for use in operations requiring a fluid to be subjected to centrifugal acceleration involving the circulation of a single-phase fluid or a multiphase fluid, for treatments including separation and / or chemical reactions, wherein, The separation comprises purification, extraction, and centrifugal partition chromatography (CPC), the extraction comprises liquid-liquid extraction, the chemical reaction comprises a biochemical reaction, characterized in that: - the rotor is formed by a plurality of discs stacked one on top of the other, - each of the discs comprises a holder (7) in which a ring (A1) consisting of an assembly of one or more circular sectors (A3) is inserted, each of the one or more circular sectors being formed with a network of cells (26, 27), - in the case of a single circular sector (A3), a space is provided between the two ends of the single circular sector, in the case of several circular sectors, a space is arranged between the ends of two adjacent circular sectors, - in one or more of the spaces, a junction connector is inserted, - the junction connector has branching means consisting of the channels required by the liquid phase, which enters the junction connector through a liquid phase inlet of the junction connector to be guided to travel through the network of cells up to a liquid phase outlet of the junction connector, which is in direct contact with the inlet of the junction connector of the next disc, and so on up to the outlet of the last disc, which is connected to the liquid phase outlet (55, 57) of the rotor.

2. The rotor according to claim 1, formed by a single circular sector, comprising a continuous network of cells and interconnected by channels (18, 19), said continuous network of cells and said channels being arranged in a plane approximately at the midpoint of the thickness of the single circular sector, characterized in that, Between the two ends of the single circular sector, there is at least one gap for arranging a junction connector in a sealed manner, the junction connector comprising at least one liquid phase inlet and at least one liquid phase outlet intended to allow the liquid phase to enter and exit the network of cells, respectively.

3. A rotor according to claim 1 or 2, characterised in that The circular sector is formed by a first circular half-sector (10) and a second circular half-sector (11), the first circular half-sector being a mirror image of the second circular half-sector, the first and second circular half-sectors each carrying a half-cell at their mirror plane, the first and second circular half-sectors being assembled face to face in a sealed manner to become a circular sector (A3).

4. The rotor of claim 1 or 2, wherein, Each circular sector (A3) of the ring (A1) is formed by two circular half-sectors superimposed face to face or by a stack of such superimpositions, each of the circular half-sectors comprising a half-cell (27A, 27B) whose sharp edge (20) is replaced by a chamfer forming a rounded surface, abutting against each other.

5. The rotor of claim 1 or 2, wherein The circular sector is made in one piece by additive construction.

6. The rotor of claim 1, each circular sector (A3) comprising in its thickness one or more ducts having a substantially rectangular cross section, each duct being arranged in a circular pattern, delimited by concentric walls, and arranged so that the average radius of each respective circular pattern of ducts substantially corresponds to an average radius identical to the average radius of the corresponding circular pattern of cells for each cell network for circulating the temperature control fluid in said ducts in as identical a manner as possible.

7. The rotor of claim 6, wherein, Each circular sector (A3) comprises three said ducts.

8. The rotor of claim 6, wherein, Said temperature control fluid comprises a thermostatic fluid.

9. The rotor of claim 6, wherein Said junction connector comprises the necessary branches so that the temperature control fluid that enters through the temperature control fluid inlet (37) of said junction connector passes through all the ducts in the single circular sector that makes up said ring and then, guided by said junction connector, is passed to the junction connector of the next adjacent disc of the stack and so on until the temperature control fluid outlet (59) of said rotor.

10. The rotor of claim 6, wherein Said junction connector comprises the necessary branches so that the temperature control fluid that enters through the temperature control fluid inlet (37) of said junction connector passes through all the ducts in series connection of each of the circular sectors that make up said ring and then, guided by said junction connector, is passed to the junction connector of the next adjacent disc of the stack and so on until the temperature control fluid outlet of said rotor.

11. The rotor of claim 1 or 2, wherein, Said junction connector further comprises a temperature control fluid inlet (37) that allows the entry of temperature control fluid and a temperature control fluid outlet (38) that allows the exit of temperature control fluid for passing said temperature control fluid through at least one temperature control fluid duct.

12. The rotor of claim 1 or 2, wherein Said cells (26, 27) have walls provided with fins.

13. The rotor of claim 1, wherein, Said junction connector comprises at least one liquid phase inlet and at least one liquid phase outlet intended to allow the entry of said liquid phase into said cell network and the exit of said liquid phase from said cell network, respectively, so that between said liquid phase outlet and said liquid phase inlet of said junction connector, said liquid phase passes through all said cells and said channels of the respective disc.

14. The rotor of claim 1, wherein When the junction connector is a non-static connector, in this case a single or multiple way valve (42) comprising an "open" position and a "bypass" position is added to the junction connector, so that a position can be selected so that in the "open" position of the valve (42) the liquid phase entering at the first liquid phase inlet (31) of the junction connector is directed by the valve to the first liquid phase outlet (32) of the junction connector, then to the cell network inlet of the adjacent circular sector, to cross the entire cell network of the disc and to reach the cell network outlet of the last circular sector, and then to the second liquid phase inlet (35) of the junction connector, and then to the second liquid phase outlet (36) of the junction connector, to enter at the first liquid phase inlet (31) of the junction connector of the next adjacent disc, but if the ball of the valve (42) is in the "bypass" position, the liquid phase entering at the first liquid phase inlet (31) of the junction connector is directed directly to the second liquid phase outlet (36) of the junction connector, without crossing the cells of the relevant disc, the latter being short-circuited, allowing the user to gradually adjust the number of cells for each of the various applications among those contained in the disc.

15. The rotor of claim 1 or 2, wherein The "n" first cells of the rotor have a volume that decreases according to a determinable function ranging from V7 to V, with V7 > V, V being the constant volume of the majority of the cells of the rotor, thus increasing the productivity of the rotor in the CPC mode in the ascending mode.

16. Use of a general rotor according to any one of claims 1 to 15 in an apparatus for circulating one or more liquids that need to be subjected to a stable and adjustable centrifugal acceleration at high pressure and at temperatures that can be varied at shorter time constants, which apparatus can be used as a chemical reactor and / or for separation in centrifugal partition chromatography (CPC), wherein, The chemical reactor comprises a bio-chemical reactor and the separation comprises extraction and purification.

17. Use of a generic rotor according to any one of claims 1 to 15 in an operation where a single-phase fluid or a multiphase fluid is to be circulated, in an operation where the fluid is to be subjected to centrifugal acceleration, for separation, wherein, The separation comprises purification, extraction and centrifugal partition chromatography (CPC), the extraction comprising liquid-liquid extraction.

18. Use of a generic rotor according to any one of claims 1 to 15 in an operation where a single-phase fluid or a multiphase fluid is to be circulated, in an operation where the fluid is to be subjected to centrifugal acceleration, for chemical reactions, wherein, The chemical reaction comprises a bio-chemical reaction.

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