Method of fluid circulation and interaction in a setup for implementing a multi-step chemical process
20240382870 ยท 2024-11-21
Inventors
Cpc classification
B01D17/12
PERFORMING OPERATIONS; TRANSPORTING
B01D17/0214
PERFORMING OPERATIONS; TRANSPORTING
B01J2204/002
PERFORMING OPERATIONS; TRANSPORTING
B01J19/0046
PERFORMING OPERATIONS; TRANSPORTING
International classification
B01D17/02
PERFORMING OPERATIONS; TRANSPORTING
B01D17/12
PERFORMING OPERATIONS; TRANSPORTING
Abstract
The invention relates to a method of fluid circulation in a setup for implementing a multi-step chemical process, comprising: supplying (102), through a first fluidic circulation system (10a) of the setup and a second fluidic circulation system (10b) of the setup (5) configured in a first supply setting, reagents (R1; R2) for performing a first step of the multi-step chemical process, to a fluidic interaction structure (25; 30) of the setup, collecting (104), in an intermediate product container (37a, 37b) of the setup, a product (R4) obtained from the interaction between the reagents within the fluidic interaction structure (25, 30) during the first step of the multi-step chemical process, and supplying (106), through the first fluidic circulation system (10a) and the second fluidic circulation system (10b) configured in a second supply setting different from the first supply setting, reagents for performing a second step of the multi-step chemical process, to the fluidic interaction structure (25; 30), and
wherein the reagents for performing the second step include the product from the first step collected in the intermediate product container (37a, 37b) or a product obtained from the interaction between said collected product and another reagent within another fluidic interaction structure (30).
Claims
1. A method of fluid circulation in a setup for implementing a multi-step chemical process, comprising: supplying, through a first fluidic circulation system of the setup and a second fluidic circulation system of the setup (5) configured in a first supply setting, reagents for performing a first step of the multi-step chemical process, to a fluidic interaction structure of the setup, collecting, in an intermediate product container of the setup, a product obtained from the interaction between the reagents within the fluidic interaction structure during the first step of the multi-step chemical process, and supplying, through the first fluidic circulation system and the second fluidic circulation system configured in a second supply setting different from the first supply setting, reagents for performing a second step of the multi-step chemical process, to the fluidic interaction structure, and wherein the reagents for performing the second step include the product from the first step collected in the intermediate product container or a product obtained from the interaction between said collected product and another reagent within another fluidic interaction structure.
2. The method according to claim 1, wherein the first and second fluidic circulation systems each comprises a multi-way distribution valve configured to selectively connect fluidically two ways together, and wherein the method further comprises switching from the first supply setting to the second supply setting by connecting different ways of the multi-way distribution valve of at least one of the first and second fluidic circulation systems than the ways connected in the first supply setting.
3. The method according to claim 2, comprising receiving commands for connecting fluidically together two ways of each multi-way distribution valves.
4. The method according to claim 2, wherein the first and the second fluidic circulation systems each comprises a pump configured to control the circulation of reagents in the multi-way distribution valve, and wherein the method further comprises receiving commands for activating and or deactivating either synchronously, asynchronously with a controlled delay, or independently the pumps, and or for adjusting the flowrate, the volume of reagents supplied and/or the duration of supply by the pumps of the first and the second fluidic circulation systems.
5. The method according to claim 1, comprising supplying, through the first fluidic circulation system and the second fluidic circulation system configured in another supply setting different from the first supply setting, reagents for performing another step of the multi-step chemical process, to the other fluidic interaction structure of the setup, the reagents for performing this other step comprising the product from the first step collected in the intermediate product container.
6. The method according to claim 1, comprising controlling the temperature within the fluidic interaction structure.
7. The method of claim 5, comprising receiving a receiving commands, for controlling the temperature within the fluidic interaction structure.
8. The method according to claim 1, comprising receiving commands and operating the fluidic interaction structure.
9. The method according to claim 1, wherein the fluidic interaction structures are chosen among a reaction structure, a phase separation structure, or a physico-chemical characterization structure.
10. The method according to claim 1, comprising redirecting a fluid obtained at an outlet of the fluidic interaction structure towards the intermediate product container or towards another container of the setup.
11. A computer implemented method of controlling fluid circulation in a setup for implementing a multi-step chemical process, comprising steps according to claim 1.
12. The computer implemented method according to claim 11, wherein controlling comprises sending commands to the first and second fluidic circulation systems or to the fluidic interaction structure.
13. The computer implemented method according to claim 12, wherein said commands comprise commands for activating and/or deactivating pumps of the first and second fluidic circulation systems either synchronously, asynchronously with a controlled delay, or independently.
14. The computer implemented method according to claim 13, wherein said commands comprise commands for adjusting the flowrate of pumps of the first and second fluidic circulation systems.
15. A computer program product comprising computer readable instructions that, when executed by a processor arrangement, causes the processor arrangement to perform the computer implemented method of claim 12.
Description
BRIEF DESCRIPTION OF THE DRAWINGS
[0062] The invention may be better understood from reading the following detailed description of non-limiting implementation examples thereof and from examining the appended drawing, in which:
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DETAILED DESCRIPTION
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[0075] The setup 5 comprises a first and a second fluidic circulation system 10.sub.a and 10.sub.b, a fluidic interaction structure 25 and an intermediate product container 37.sub.a.
[0076] The fluidic interaction structure 25 comprises inlets configured to be fluidically connected to both the first and second fluidic distribution systems 10a, 10b. The first and second fluidic circulation systems 10a, 10b are configured to be in a first setting to supply the fluidic interaction structure 25 with reagents for performing a first step of the multi-step chemical process, and in a second setting, different from the first setting, to supply the fluidic interaction structure 25 with reagents for performing a second step of the multi-step chemical process.
[0077] The intermediate product container is configured to be fluidically connected to the outlet of the fluidic interaction structure 25 and to one of the fluidic circulation systems 10a, 10b. The intermediate product container 37a is configured to collect a product obtained from the interaction between the reagents within the fluidic interaction structure 25 during the first step.
[0078] In the present example, at least one of the fluidic circulation systems 10a, 10b is configured to supply the product collected in the intermediate product container 37a to the fluidic interaction structure 25 as a reagent for performing the second step.
[0079] In other embodiments described below with reference to
[0080] According to embodiments, the first and a second fluidic circulation systems 10.sub.a and 10.sub.b each comprises a pump 15.sub.a and 15.sub.b and a multi-way distribution valve 20.sub.a and 20.sub.b. The multi-way distribution valve 20.sub.a and 20.sub.b are configured to selectively connect fluidically two ways together, and the pumps 15.sub.a and 15.sub.b are configured to control the circulation of reagents in the multi-way distribution valves 20a, 20b. The connected ways of at least one of the multi-way distribution valves 20a, 20b are different in the first setting are different from the connected ways and in the second setting.
[0081] The fluidic interaction structure 25 is a reaction structure, a phase separation structure, or a physico-chemical characterization structure. The reaction structure is for instance a thermally controlled reactor, a plasma reactor, an electrochemical reactor, a photochemical reactor, or a cartridge containing solid-phase reagents or catalysts. The phase separation structure is for instance a liquid-liquid and/or gas-liquid separation structure. The physico-chemical characterization structure is for instance a high-performance liquid chromatography structure, a gas chromatography structure, a mass spectrometry structure or a combined high performance liquid chromatography-mass spectrometry structure or a combined gas chromatography-mass spectrometry structure, or a nuclear magnetic resonance structure or an ultraviolet/visible spectrometer structure or an infrared spectrometer structure.
[0082] In the illustrated example of
[0083] The fluidic interaction structure 25 comprises two inlets 27.sub.a and 27.sub.b that are connected respectively to ways 28.sub.a and 29.sub.a of the respective multi-way distribution valves 20.sub.a and 20.sub.b and an outlet connected to the intermediate product container 37.sub.a.
[0084] The intermediate product container 37.sub.a is further connected to a way 28.sub.b of the multi-way distribution valve 20.sub.a of the first fluidic circulation systems 10.sub.a.
[0085] Some ways of the respective multi-way distribution valves 20.sub.a and 20.sub.b are connected to reagent reservoirs (not illustrated).
[0086]
[0087] At a first step 102, a fluidic interaction structure 25 of the setup 5 is supplied with reagents for performing a first step of a multi-step chemical process. The supply is done through a first and a second fluidic circulation system 10a and 10b of the setup 5 that are configured in a first supply setting.
[0088] According to embodiments, the first and second fluidic circulation systems 10a, 10b each comprises a multi-way distribution valve 20a, 20b configured to selectively connect fluidically two ways together. As will be done in a later step (see step 106 below), one can switch from the first supply setting to another supply setting by connecting different ways of the multi-way distribution valves 20a and 20b than the ways connected in the first supply setting.
[0089] In some embodiments, step 102 includes receiving commands from an electronic device 500. In those embodiments, the multi-way distribution valves 20.sub.a and 20.sub.b may receive commands to fluidically connect the ways 28.sub.a and 29.sub.a to other ways connected to reservoirs comprising some reagents to be supplied for the first step of a multi-step chemical process. Upon activation of the pumps 15.sub.a and 15.sub.b of the respective multi-way distribution valves 20.sub.a and 20.sub.b, the reagents contained in the connected reservoirs are supplied to the fluidic interaction structure 25 for performing said first step. In practice, the pumps 15.sub.a and 15.sub.b may receive commands for activating either synchronously, asynchronously with a controlled delay, or independently. Optionally, the pumps 15.sub.a and 15.sub.b may also receive commands for adjusting some parameters such as their flowrate, the volume of reagents supplied and/or the duration of supply, as well as commands for deactivating. In embodiments where the setup comprises a temperature controller, it receives, at step 102, commands to set the temperature of the fluidic interaction structure 25.
[0090] At a step 104, the product obtained from the interaction between the reagents during the first step of the multi-step chemical process within the fluidic interaction structure 25 is collected in the product intermediate reservoir 37.sub.a.
[0091] At a step 106, the fluidic interaction structure 25 is supplied with reagents for performing a second step of the multi-step chemical process. The supply is done through the first and the second fluidic circulation system 10a and 10b that are configured in a second supply setting different from the first supply setting. The ways that are connected fluidically together in at least one of the multi-way distribution valves 20.sub.a and 20.sub.b are switched to be in the second setting and allow to perform the second step. At least one of the ways connected in at least one of the multi-way distribution valves 20.sub.a and 20.sub.b is different in the second setting from the ways that are connected in the first setting.
[0092] In embodiments, the ways that are connected fluidically together in both multi-way distribution valves 20.sub.a and 20b are switched to be in the second setting and allow to perform the second step. At least one of the ways connected in each of the multi-way distribution valves 20.sub.a and 20b is different in the second setting from the ways that are connected in the first setting.
[0093] According to embodiments, the method further comprises switching from the first supply setting to the second supply setting by connecting different ways of the multi-way distribution valve than the ways connected in the first supply setting.
[0094] According to a first example, the collected product can be provided as such to the same fluidic interaction structure 25 for performance of the second step of the multi-step chemical process. Alternatively, according to a second example, the product collected in the product intermediate reservoir 37.sub.a is not provided as such to the fluidic interaction structure 25 but is further transformed during an intermediary step occurring in another fluidic interaction structure 30. In this second example, the further transformed product is supplied to the fluidic interaction structure 25 as a reagent of the second step of the multi-step chemical process.
[0095] In some embodiments, step 106 includes receiving commands, in particular from an electronic device 500, as described below. The multi-way distribution valves 20.sub.a and 20.sub.b may receive commands to fluidically connect the ways of the multi-way distribution valve 20.sub.a to a reagent reservoir comprising some reagents to be supplied for the second step of the multi-step chemical process and to the reagent of product intermediate reservoir 37.sub.a comprising the collected product from the first step (in the first example) or to another product intermediate reservoir comprising the further transformed product (in the second example). Similarly to step 104, upon activation of the pumps 15.sub.a and 15.sub.b of the respective multi-way distribution valves 20.sub.a and 20.sub.b, the reagents contained in the connected reservoirs are supplied to the fluidic interaction structure 25 for performing said second step. Here again the pumps and eventually the temperature controller may receive commands to adjust some parameters.
[0096] In embodiments, the product obtained from the interaction between the reagents during the second step of the multi-step chemical process within the fluidic interaction structure 25 may be collected in the product intermediate reservoir 37.sub.a (or another connected reservoir) for further use in another step of the multi-step chemical process. Advantageously, the method and the setup according to the invention are particularly useful for chemical processes comprising lots of steps.
[0097] Advantageously, the setup 5 allows cleaning of the fluidic interaction structure between two steps of the multi-step chemical process, especially without manual operation. Advantageously, cross-contamination can be avoided, and the quantity of intermediate product collected can be maximized.
[0098] For example, the first and/or second fluidic circulation systems may receive commands for supplying a fluid (in particular an inert gas) to the fluidic interaction structure to flush the fluid initially contained in the said fluidic interaction system. In another example, the first and/or second fluidic circulation systems may receive commands for supplying a fluid (in particular a liquid solvent) to the fluidic interaction structure to dilute and flush residual species, hence cleaning internal parts of said fluidic interaction structure.
[0099] Embodiments are not limited to the description above.
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[0101] In second and third embodiments illustrated on
[0102] In a fourth embodiment illustrated on
[0103] In a fifth embodiment illustrated on
[0104] The sixth embodiment illustrated on
[0105] Complex multi-step chemical processes can be performed using the set-up by taking advantage of the intermediate product containers 37a-d and of the multiplicity of ways on the multi-way distribution valves 20a and 20b. The following example is an illustration of a possible multi-step chemical process that can be performed within the setup.
Examples
[0106] An example is presented below. The multi-step process is performed with the setup of
[0107] The setup is connected to a computer. The computer is configured to execute computer readable instructions generated by a computer program to command the different elements of the setup as described previously to perform a method for fluid circulation and interaction. An example of method is illustrated on
[0108] The first step consists in the liquid-liquid extraction of the amine using 1 mL of an acidic aqueous step (HCl 1 M). By separating the organic and the aqueous steps, the alkene is recovered as is, while the amine is in protonated form in the aqueous step. The ammonium ion is deprotonated using 1 mL of an alkaline brine (NaOH 2 M+NaCl 120 g/L). The amine is recovered by liquid-liquid extraction using 2 mL of an organic solvent (e.g., ethyl acetate) followed by step separation.
[0109] The method performed with the setup 5 can be summarised by the following sequence: [0110] 1. Pump 15a picks up the model mixture at way 2 of valve 20a and dispenses it to the separation structure 30 through way 12 of valve 20a while Pump 15b does the same with HCl 1 M from way 2 to way 12 of valve 20b. The organic phase resulting from the phase separation is collected in a vial through valve 40a. The aqueous phase ?.sub.aq,1 resulting from the phase separation is collected in the intermediate product container 37b through valve 40b. [0111] 2. Pump 15a picks up ?.sub.aq,1 in the intermediate product container 37b and dispenses it through the ways 3 and 11 of the valve 20a to the heated reactor 25 while Pump 15b does the same with NaOH 2 M+NaCl 120 g/L from way 3 to way 11 of valve 20b. The resulting aqueous phase ?.sub.aq,1 outputted by the heating reactor is directed to an intermediate product container 37a. [0112] 3. Pump 15a picks up ?.sub.aq,1 from the intermediate product container 37a and dispenses it through the ways 4 and 12 of the valve 20a to the extraction/separation module 30 while Pump 15b does the same from way 4 to way 12 of valve 20b with extraction solvent EtOAc. The organic phase resulting from the phase separation is collected in a vial through valve 40a. The aqueous phase resulting from the phase separation is directed to the waste through valve 40b.
[0113] Between these main events, a certain number of actions have been undertaken. The internal volumes of the tubes and of the phase separator were flushed or washed after each step by deionised water, extraction solvent and/or air to recover a maximum of the material. These intermediate operations also require movements of the pump valves and of the rotary valves.
[0114] The invention is not limited to the exemplary embodiments which have just been described. For example, the fluidic interaction structure can be different than a heated reactor or than a liquid-liquid separator and may be as mentioned above. Additional fluidic interaction structure, redirection means, container and/or intermediate reservoir container may be added.
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[0116] The electronic device 500 comprises one or more processors 502. The one or more processors control operation of other components of the electronic device 500. The one or more processors 502 may, for example, comprise a general-purpose processor. The one or more processors 502 may be a single core device or a multiple core device. The one or more processors 502 may comprise a central processing unit (CPU) and/or a graphical processing unit (GPU). Alternatively, the one or more processors 502 may comprise specialized processing hardware, for instance a RISC processor or programmable hardware with embedded firmware. Multiple processors may be included.
[0117] The electronic device comprises a working or volatile memory 504. The one or more processors may access the volatile memory 504 to process data and may control the storage of data in memory. The volatile memory 504 may comprise RAM of any type, for example Static RAM (SRAM), Dynamic RAM (DRAM), or it may comprise Flash memory, such as an SD-Card.
[0118] The electronic device comprises a non-volatile memory 506. The non-volatile memory 506 stores a set of operation instructions 508 for controlling the operation of the processors 502 in the form of computer readable instructions. The non-volatile memory 506 may be a memory of any kind such as a Read Only Memory (ROM), a Flash memory or a magnetic drive memory.
[0119] The one or more processors 502 are configured to execute operating instructions 508 to cause the setup to perform the method of fluid circulation and interaction 100. The operating instructions 508 may comprise code (i.e. drivers) relating to the hardware components of the system/apparatus 500, as well as code relating to the basic operation of the system/apparatus 500. Generally speaking, the one or more processors 502 execute one or more instructions of the operating instructions 508, which are stored permanently or semi-permanently in the non-volatile memory 506, using the volatile memory 504 to temporarily store data generated during execution of said operating instructions 508.
[0120] Implementations of the methods described below may be realized as in digital electronic circuitry, integrated circuitry, specially designed ASICs (application specific integrated circuits), computer hardware, firmware, software, and/or combinations thereof. These may include computer program products (such as software stored on e.g. magnetic discs, optical disks, memory, Programmable Logic Devices) comprising computer readable instructions that, when executed by a computer, such as that described in relation to
[0121] Systems according to the invention may include a setup as shown in any of
[0122] Those of skill in the art will understand that modifications (additions and/or removals) of various components of the methods, setups, systems and embodiments described herein may be made without departing from the full scope and spirit of the present invention, which encompasses such modifications and any and all equivalents thereof.