UNIVERSAL ROTOR FOR ALL SYSTEMS USED TO SUBJECT FLUIDS TO CENTRIFUGAL ACCELERATIONS
20230285873 · 2023-09-14
Inventors
Cpc classification
B01D15/1892
PERFORMING OPERATIONS; TRANSPORTING
International classification
Abstract
A rotor for all systems used to circulate various single-phase or multiphase fluids, ranging from organic or non-organic solvents to CO.sub.2 in a liquid or supercritical phase in cells connected to each other by channels, the assembly being subjected to adjustable centrifugal acceleration and including precision temperature control for chemical or biochemical reactions and extractions, and purification and separation reactions and, for use in chemical and biochemical reactors. Such a rotor is formed of one or more discs stacked on top of each other, each being made up of circular sectors consisting of a circular half-sector and a circular half-sector, each being the mirror image of the other relative to the plane of the circular half-sector after they have been assembled opposite each other in a sealed manner. Their half-channels having respective links which form a link channel when the half-sectors are joined.
Claims
1. A universal rotor for operations requiring fluids to be subjected to centrifugal accelerations involving the circulation of single-phase or multiphase fluids, for treatments consisting of purifications, extractions, separations, centrifugal partition chromatography (CPC), liquid-liquid extractions, chemical and/or biochemical reactions, the rotor comprising: (a) one or more discs stacked one on top of the other, (b) each of said discs comprising a retainer in which a ring, including an assembly of one or more circular sectors, is inserted, (c) in a case of a single circular sector, a space being provided between two ends of the single circular sector, or in a case of several circular sectors, said space being arranged between ends of two contiguous circular sectors, (d) a linking connector is inserted into said space or spaces, (e) said linking connector including branching channels for a liquid phase entering through inlets into said linking connector to be guided to travel through a network of cells up to outlets of said linking connector, said outlets being in direct contact with inlets of a linking connector of a next disc and so on up to an outlet of a last disc which is connected to an outlet of said rotor.
2. The rotor according to claim 1, formed by a single circular sector comprising a network of successive cells and interconnected by said channels arranged in a plane approximately at a midpoint of its thickness, wherein there is at least one gap between its two ends for arranging in a sealed manner a linking connector, said linking connector comprising at least one inlet and at least one outlet configured to respectively allow entry of a liquid mixture into said network of cells and the exit of said mixture from said network of cells.
3. The rotor according to claim 1, wherein the sectors are formed from a first circular half-sector and a second circular half-sector, each of which is a mirror image of the other, all carrying at their mirror plane half-cells and and half-channels and, the two half-sectors being assembled in a sealed manner face-to-face, to become one circular sector.
4. The rotor according to claim 1, wherein each circular sector of a ring is formed by superposing elements each comprising half cells the sharp edges of which are replaced by chamfers forming rounded surfaces, one against the other.
5. The rotor according to claim 1, wherein the circular sectors are made in one piece, by additive construction.
6. The rotor according to claim 1, wherein a single circular sector comprises, in its thickness, one or more ducts having a generally rectangular cross-section each arranged in a circular pattern, typically three in number, delimited by concentric walls and arranged such that an average radius of each respective circular pattern of ducts substantially corresponds to a same mean radius as that of a corresponding circular pattern of a network of cells, for circulating a temperature control or thermostatting fluid in said ducts in an identical manner for each one of said networks of cells.
7. The rotor according to claim 1, the wherein said linking connector comprises said branches so that said temperature control or thermostatting fluid entering through an inlet passes through all of said ducts connected in series of each one of said circular sectors constituting said ring and then, guided by said linking connector, passes to a linking connector of a next adjacent disc of said stack and so forth up to an outlet of said rotor.
8. The rotor according to claim 1, wherein a linking connector comprises said branches so that said temperature control or thermostatting fluid entering through an inlet passes through all of said ducts connected in series of each one of a number of circular sectors constituting said ring and then, guided by said linking connector, passes to a linking connector of a next adjacent disc of the stack and so forth up to an outlet of said rotor.
9. The rotor according to claim 1, wherein said linking connector also includes an inlet and an outlet allowing entry and exit of a temperature control or thermostatting fluid in order for it to pass through said at least one temperature control or thermostatting fluid duct.
10. The rotor according to claim 1, wherein said cells have walls provided with fins.
11. The rotor according to claim 1, wherein said linking connector comprises at least one inlet and at least one outlet for respectively allowing entry of a liquid mixture into said networks of cells and an exit of said mixture from the networks of cells, such that between said outlet and said inlet, said liquid phase passes through all the cells and channels of a respective disc.
12. The rotor according to claim 1, wherein when said linking connector is a non-static connector, in this case a single or multi-way valve comprising “ON” and “BYPASS positions is added thereto, making it possible to select positions such that in the “ON” position of said valve a said liquid phase entering at said inlet is directed to an outlet of said valve to then enter said inlet of a contiguous circular sector in order to traverse said entire network of cells of said disc and arrive at said outlet of a last circular sector and then to said inlet) and then to said outlet of said linking connector, to enter a next contiguous of said disc at said inlet of said linking connector thereof but, if a ball of said valve is in said “BYPASS” position, said liquid phase entering at said inlet is directed directly to said outlet without traversing said cells of said disc concerned, the latter being short-circuited, allowing a user to adjust a number of said cells to each of its various applications in steps by said number of said cells contained in said disc.
13. The rotor according to claim 1, wherein, “n” first cells of said rotor have decreasing volumes according to a determinable function ranging from (V7) to (V) with (V7>V), V being a constant volume of most of said cells of said rotor, thereby increasing the productivity of said rotor, in CPC mode, in an ascending mode.
14. A method of using a universal rotor, in an apparatus, the method comprising: circulating one or more liquids submitted to stable and adjustable centrifugal accelerations, at high pressures and at temperatures able to be varied with short time constants, said apparatus being a chemical and/or biochemical reactors and/or for extractions, separations and purification in centrifugal partition chromatography (CPC), the fluids comprising organic or non-ionic liquids, ionic liquids, CO.sub.2 in liquid or supercritical phase, using said rotor of said apparatus, which includes one or more discs stacked one on top of the other, each of said discs including a retainer in which a ring is inserted into an assembly of one or more circular sectors, providing a space between ends of a single circular section for a single circular sector or arranging said space between said ends of said contiguous circular sectors for several circular sectors, and inserting a linking connector into said space or spaces, and directly contacting outlets of a linking connector with inlets of another linking connector of a next of said discs, said linking connectors having branching channels to cause a liquid phase entering through inlets to be guided to travel through a network of cells to outlets.
15. The method of using the universal rotor according to claim 14, in operations requiring fluids to be subjected to said centrifugal accelerations requiring said circulation of single-phase or multiphase fluids, for said purifications, extractions, separations, centrifugal partition chromatography (CPC), liquid-liquid extractions.
16. The method of using the universal rotor according to claim 14, in operations requiring fluids to be subjected to said centrifugal accelerations requiring said circulation of single-phase or multiphase fluids, for chemical and biochemical reactions.
Description
BRIEF DESCRIPTION OF THE DRAWINGS
[0029]
[0030]
[0031]
[0032]
[0033]
[0034]
[0035]
[0036]
[0037]
[0038]
DETAILED DESCRIPTION OF EMBODIMENTS
[0039]
[0040] The ring A1 shown in
[0041] In the case of several circular sectors 2 to 5, the two ends of the circular sectors 2 and 5 correspond to one end of a first circular sector 2 which is not connected to another circular sector, and to one end of a last circular sector 5 also not connected to another circular sector. In the case of a single circular sector, its two ends correspond to those of an assembly of several circular sectors.
[0042] A linking connector 6 is interposed in a sealed manner between the two ends of the assembly of the circular sectors 2 to 5. This linking connector makes it possible, in one embodiment of the invention, to allow the mobile phase and the sample to be injected to enter into the ring A1, and then after they have passed through all the cells, to direct them into a linking connector of an adjacent ring which in turn performs the same function, and so on up to the last ring of a rotor constituted by a stack of discs. The various components of the sample entrained by the mobile phase, in the case of a CPC separation application for example, are separated during the course of their path through the cells and channels, and then are 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. The linking connector may have other functions according to the invention which will be presented in the detailed description of
[0043]
[0044]
[0045] Their respective channels 18 and 19 linking the cells, see the section taken along line B-B of
[0046] According to the invention, rounded surfaces or chamfers 20 are made, shown in detail in the enlarged view of half-cell 27A, instead of cells having sharp corners, these latter considerably degrading hydrodynamic operation and consequently performance of the apparatus. This manner can be advantageously applied to all conceivable geometries of cells, whether they are symmetrical or dissymmetrical and whatever their various applications. The channels 18 and 19 linking the cells are advantageously circular in cross-cross-section, also for good hydrodynamic operation. However, in the case of conventional mechanical machining of said channels, it will be possible for reasons of ease of machining and/or state of their surface, to give them a polygonal cross-section, for example square, taking care to round all the angles in order to obtain a cross-section closest to a circular cross-section.
[0047]
[0048] To aid understanding, the linking connectors A6 and B6,
[0049] Said linking connector A6 or B6
[0050]
[0051] In the Bypass position, the mobile phase which had previously filled the cell network concerned is trapped therein. The mobile phase entering at ports 29 or 31 of the said linking connector is directed directly by the ball valve towards the outlet 34 or 36 of the linking connector adjacent to the next linking connector of the stack. This embodiment makes it possible for the user, by turning the ball valve 41 one quarter of a turn in one direction or the other by means of a screwdriver introduced into slot 43, to adjust the number of active cells of the rotor in steps corresponding to the number of cells contained in a disc. The operation of this major embodiment of the invention is shown more in detail in the following discussion of
[0052]
[0053] The linking connectors 6, whether they are of fixed configuration A6 of
[0054] Cross-section E1-E1 is an assembly view including the double-channel ball valves adapted to the two networks of cells of different volumes V and 8V of the present embodiment. For its use, the network corresponding to the volume of the selected cells is selected by connecting, for example, the arrival of the mobile phase in descending mode to the inlet 56, outlet 57 then being that of the rotor which will be connected to a detector and to a fraction collector, for example. It is recommended to connect a plug at ports 54 and 55, to prevent the phase in the corresponding cell network from escaping, so as not to risk a dynamic imbalance of the rotor when rotating. Cross-section E1-E1 also shows the inlet and outlet 58 and 59 intended for the circulation of a liquid for controlling temperature or a thermostatting fluid for the rotor.
[0055] Cross-section E2-E2 more precisely shows the hydraulic operation of the valves “RUN”-“BYPASS” showing, on a larger scale in
[0056] The cross-section E3-E3 shows the plane parallel to cross-section E2-E2 and passing through the axis of the connectors 58-59. The temperature control liquid or thermostatting fluid enters, for example by the connector 58, then arrives at the inlet 37 of the first linking connector A6 or B6. A diverter 60 directs it in the direction of the arrows towards the temperature control liquid or thermostatting control channel 12A of the contiguous circular sector. After the temperature control liquid or thermostatting fluid has passed through all the ducts 12A, 12B to 12C of the circular sectors of the disc, it arrives at duct 12C to be directed at port 38 of diverter 60 of the linking connector and directly passes from outlet 38 to the inlet 37 of the adjacent linking connector of the next disc until it arrives at the outlet 59 of the rotor.
[0057]
[0058] In this example, the mobile phase thus passes through 320 cells of the rotor that comprises 480. It is possible to produce rotors with many more cells to widen the field of applications. It can be seen, for example, that the number of cells used in such a rotor can be modified by a number of cells corresponding to the number of cells contained in each disc, by performing a quarter turn of the balls 41 of valves 42 and thus making it possible to operate with 80, 160, 240, 320 or 400 cells of such a rotor, depending on the requirements of the separations to be performed. If the light mobile phase is connected to inlet 57, the path in the networks of cells remains the same but in ascending mode.
[0059]
[0060] These rotary seals must be adapted to the pressures and speeds of rotation involved and must be of easy access in order to simplify maintenance, cleaning, changes in seals, after-sales servicing, etc. A nut 86 having a bore for receiving a spring 87 is threaded onto rotor shaft 85 so that the spring 87 provides sufficient permanent pressure to ensure sealing of all the seals of the discs of the stack constituting the rotor and so that the assembly is mechanically homogeneous and stable. The frame carrying this mechanical assembly is fixed to the apparatus by dampers 92 provided for this purpose, to which safety fasteners are added along with mechanical locking means for transport, complying with applicable standards.
[0061]
[0062] For the calculation and construction of a production apparatus intended to carry out a given application long term, calculations and experiments for scale change, derived from results of measurements performed on laboratory devices, preferably equipped with “RUN-BYPASS” valves on each disc according to the invention, should save on time and precision. However, measurements may be somewhat affected by error, an industrial rotor constructed on these bases may not be exactly at its optimum, a defect that can be easily corrected by the technological flexibility of the invention, because it is possible to add or remove one or more discs making it possible to optimize performance under actual conditions and by adjusting the number of cells necessary, this operation being simplified by the construction of the discs using assembly of circular sectors, said circular sectors being able to have more or fewer cells on demand.
[0063] View A of
[0064] This embodiment presented with a vertical axis does not exclude an assembly made with a horizontal or articulated axis of rotation allowing the portion supporting the rotor to be angularly displaced. A person skilled in the art will know the use of various means known in conventional mechanics in order to put such a mounting into practice.
[0065]
[0066] It is useful to employ discs equipped with a valve 42 according to the invention making it possible to connect or not, all or parts of the discs of the rotor comprising the networks of cells of different volumes in order to adjust the number as a function of the needs of each application. The rotor according to the invention is used in centrifugal partition chromatography CPC operations allowing the separation of a compound contained in a solution formed from several components. The separation of the sample is based on the partition coefficients specific to each of the components of the sample between the mobile and stationary phases. The partition coefficient determines the affinity of each molecule in the mobile and stationary phases and therefore the speed at which each molecule moves in the system. At the end of the purification process, automated fraction collectors retain all the selected fractions according to the parameters of the program.
[0067] The rotor according to the invention can be used not only in separation operations, but also for reaction operations between components, thus acting as an intensified chemical and/or biochemical reactor due to the excellent mixing occurring in each of the cells. The advantage of the system is that of obtaining a plug flow reactor-like behavior, which is recognized to give the best performance, considering said universal rotor as a succession of perfectly stirred reactors, consisting of the cells. The reactions can be carried out in single phase or be diphasic, which is most relevant when the reactants and the product are in different phases.
[0068] This invention makes a clean break with conventional batch processes: the double jacketed stirred tank, which is the most frequently used tool, with more than 50% of chemical production units in the world. The engineering of the reactors comprises two key elements: the kinetics of the reactions and the design of the reactors. The design of the reactors must be thought through so that the reaction proceeds at its intrinsic speed, that is to say if there is a perfect mixing and mass transfer in the reactor.
[0069] Often, in large, stirred tank reactors, the reaction does not take place at its intrinsic speed because it is limited by the mixing in the tank, that is, the reactants are not perfectly mixed. In this case, it is known that it is “limited by the mixing”. The role of an intensification of the process is to reduce or eliminate these limitations so that the reaction can reach its intrinsic rhythm. Thus, the purpose is to ensure that the mixing and heat/mass transfer rates will be relatively fast with respect to the fundamental kinetics of the process. A high acceleration can be obtained as long as is required by operating in such a rotary system. Transposing chemical syntheses in reactors in which the phases have a piston-like flow, then makes it possible to minimize reaction volumes (safety of installations and operators), to intensify the exchanges of material (mixing, reaction, separation), to regulate and control the temperature with good precision and to add alerting systems in the event of overshoot. Examples include the reduction of benzal-aldehyde to benzyl alcohol by homogeneous ruthenium catalysis, or the two-phase esterification reaction of oleic acid to ethyl oleate by a lipase (Candida Antarca).
[0070] Liquid/liquid extraction is a basic operation in the field of process engineering. It consists in passing a solute (the molecule of interest) from a so-called “feed” phase to a so-called “extract” phase. The two phases are immiscible or partially miscible. Many examples exist in the industry, for example the production of antibiotics with an acido-basic extraction cycle.