DESC:FORM 2
THE PATENTS ACT, 1970
(39 of 1970)
&
THE PATENT RULES, 2003
COMPLETE SPECIFICATION
(See Section 10 and Rule 13)
Title of invention:
A CONTINUOUS MICROREACTOR SYSTEM
APPLICANT:
PIDILITE INDUSTRIES LTD
Address:
An Indian entity having address as
Regent Chambers, 7th floor, Jamnalal Bajaj Marg, 208, Nariman point, Mumbai 400021, Maharashtra, India

The following specification particularly describes the invention and the manner in which it is to be performed.

CROSS-REFERENCE TO RELATED APPLICATIONS AND PRIORITY
The present application claims priority from the Indian provisional patent application, having application number 202421045865, filed on 13th June 2024, incorporated herein by a reference.

TECHNICAL FIELD
The present disclosure relates to a continuous reactor system. More particularly the present disclosure relates to a continuous microreactor system for polymerization based on flow chemistry.
BACKGROUND
Currently, many scale-up chemical reactions are carried out in batch manner and are responsible for large number of material manufacture and synthesis worldwide. The industrial chemical reactions encompass a wide range of processes used in various industries to produce chemicals, materials, products, cosmetics, pharmaceutical products, etc.
In present state of the art, the types of industrial chemical processes include organic, inorganic, or hybrid reactions such as paint manufacturing, adhesive manufacturing, polymer synthesis, pharmaceutical synthesis, fertilizer production, water treatment, effluent treatment, emulsification, emulsion synthesis, nitration, esterification, etc.
In present state of the art, the industrial chemical processes are employed for several end-use applications, such as nanocomponent manufacturing, rubber, polyurethane articles, construction materials, adhesives, paints and coatings, paper and paperboard coating, carpet backing, and textiles.
In many industrial processes, the multiphase reactions may be carried out such as dispersion in solvent or water, catalysis, solid-liquid process, purification, gas-gas, gas-liquid, particle dispersion, which are essential for various applications across industries and cannot be carried out via simple reactors for flow reactions, tubular reaction, batch synthesis, or multi-step batch synthesis.
In some cases, such as reactions related to obtaining the reaction intermediates are carried out in a single reactor where reactants are first dispersed in aqueous phase and catalysts/initiators/chain extender are introduced or generated in an aqueous phase are very difficult to isolate and control at the same stage.
Commercial products that are made using a semi-continuous or a simple batch process are inexpedient because the heat evolved in a simple batch process such as nitration would be uncontrollable in a large reaction vessel and usually tend to produce undesired impurities and side products.
In the semi-continuous batch process, like polymerization monomers and initiators are added in proportions and at a controlled rate so that rapid polymerization occurs. In this method, the monomer concentration is low, also called under-starved monomer conditions, to facilitate temperature control.
Recently, chemical processes using flow reactor have received significant interest because they are expected to make an innovative and revolutionary change for chemical synthesis by virtue of their advantages over conventional macroscale batch reactors, such as effective mass transfer and heat transfer, extremely fast mixing, and precise residence time control.
Flow chemistry is an immerging advance technology to convert conventional industrial plants into compact, safe, and more energy efficient continuous processes.
In the state of the art, fine products such as paints and adhesives are produced by semi-batch system. The semi-batch system enables addition of a part of total charge of reactants in a reactor followed by adding secondary reactants such as catalysts, extenders, other additives, and also a part of primary component in continuous manner. After achieving the property at that stage, the reactor mass is transferred to holding tank for the next batch and prior to that the reactor is flushed and made ready.
In state of the art, to carry out continuous reactions loop type continuous stirred tank reactors (CSTR) or pulsed packed column were investigated. The transfer of a semi-batch processes to continuous fashion needs to be investigated for the viability of a tubular micro reactor for the chemical industrial processes.
In view of the above, there is a long-felt need for providing a reactor system for users that works in an efficient manner. Also, there is a long felt need to overcome the drawbacks related to reactor setup and operational conditions necessary to reach a very stable operation and to achieve improved kinetics, time and properties indicating uniform reaction, reduced side products, selectivity and maximum conversion of reactants.
SUMMARY
The present disclosure overcomes one or more shortcomings of the prior art and provides additional advantages discussed throughout the present disclosure. Additional features and advantages are realized through the techniques of the present disclosure. Other embodiments and aspects of the disclosure are described in detail herein and are considered a part of the claimed disclosure. The present disclosure has been made in order to solve the above problems, and it is the object of the present disclosure to provide a continuous microreactor system based on flow chemistry to carry out multi-component reactions.

In one embodiment, a continuous microreactor system is disclosed. The continuous microreactor system may comprise at least one of a microreactor segment for a continuous reaction. The microreactor segment may comprise a first mixing device for mixing of at least one of a primary reactant and a secondary reactant. The microreactor segment may comprise a first micro-reactor coil, a second micro-reactor coil, and a back pressure control valve. The back pressure control valve may be enabled to control and alternating flow of at least one of the primary reactant and the secondary reactant from the first mixing device to at least one of the first micro-reactor coil or the second micro-reactor coil. The continuous microreactor system may comprise a second mixing device configured for mixing of primary reactant received from a back pressure control valve with a secondary reactant. The continuous microreactor system may comprise a controller unit in communication with the at least one microreactor segment.
BRIEF DESCRIPTION OF DRAWINGS
The detailed description is described with reference to the accompanying Figures. In the Figures, the left-most digit(s) of a reference number identifies the Figure in which the reference number first appears. The same numbers are used throughout the drawings to refer like features and components.
Figure 1 illustrates a continuous microreactor system (100) is a system enabled for integrated continuous online monitoring, control, synthesis of polymers and formulations, in accordance with an embodiment of the present subject matter.
Figure 2 illustrates a continuous microreactor system (200) comprising a continuous microreactor segment/apparatus (104), for continuous reaction of a primary reaction component and secondary reactants based on flow chemistry, in accordance with an embodiment of the present subject matter.
List of Abbreviations and Reference numerals
100- continuous microreactor system for continuous reaction
101- controller unit, 102- cloud network, 103- a server,
104- continuous microreactor segment/apparatus
201, 202, 208, 209- one or more feed transfer units
203- first mixing device, 210- second mixing device
204 - one or more micro reactors
204(a), 204(b)- one or more micro reactor coils
206, 211- one or more temperature-controlled baths
207- a back pressure controlling valve
212- a product storage vessel
213- a cleaning fluid input tank
DETAILED DESCRIPTION
Reference throughout the specification to “various embodiments,” “some embodiments,” “one embodiment,” or “an embodiment” means that a particular feature, structure, or characteristic described in connection with the embodiment is included in at least one embodiment. Thus, appearances of the phrases “in various embodiments,” “in some embodiments,” “in one embodiment,” or “in an embodiment” in places throughout the specification are not necessarily all referring to the same embodiment. Furthermore, the particular features, structures or characteristics may be combined in any suitable manner in one or more embodiments.
Disclosed is a compact, scalable, continuous reaction apparatus. The present disclosure may be utilized as an alternative to existing batch/semi batch processes for chemical reactions comprising multicomponent and multiphase combinations.
In a non-limiting embodiment, a continuous microreactor system may comprise a controller unit, a cloud network, a server, and a continuous reaction apparatus. In a non-limiting embodiment of the present disclosure, continuous microreactor apparatus may comprise at least one of a feed transfer unit, one or more mixing devices, one or more micro-reactors, one or more temperature-controlled baths, at least one of a back pressure controlling valve, and a product storage vessel.
In one embodiment of the present disclosure, the system for continuous reaction may comprise a micro-controller unit enabling smooth and efficient functioning of the system and achieving complete conversion of the reactant. In one embodiment, the system is a compact microreactor based system facilitating point of sell (POS) use. The advantages of the system are instant, and just in time manufacturing of products such as emulsions, polymer emulsion, paints, coatings, and adhesives. In a related embodiment, said system is a scalable setup.
In one embodiment, the system for continuous mode reactions is disclosed herein. The disclosed system explores feasibility of incorporating a micro reactor setup to perform various chemical industrial processes, such as a monomer polymerization and as a multi-component, and multi-utility system.
The continuous microreactor system may comprise at least one micro-reactor segment for a continuous reaction. The micro-reactor segment of the system is a modular combination which is configured for scale-up with addition of at least one feed transfer unit which is enabled for feeding reactants modules and at least one mixing unit integrated with one or more micro-reactor units. The system may be skid mounted in an enclosure which may also include raw material handling/preparation, synthesis, formulation, and packing.
The system in accordance with present disclosure presents an efficient mass transfer, even at laminar flow regime, due to the short diffusion path length since there is a quadratic decrease of diffusion time with a downscaling of the linear dimension of a system by smaller reactor path internal diameter.
Further, the heat removal capacity of said system is huge because of the high surface to volume ratio of 800 to 2000, and this allows performing very fast and exothermic reactions isothermally. Furthermore, flow reactors facilitate easier scale-up by numbering up of reactors and they provide easier portability because of the smaller size of a system.
Additionally, the flow rate of reactants, total mass flow rate in a coiled reactor, temperature, and residence time may also be optimized to obtain better conversion of reactants up to 99.9%, comparative reaction and product quality, lower residual impurities, and side products. The present system converts one or more primary and secondary reactants to applicable product by continuous formulation within short duration reaction cycle. In an embodiment, the system is configured for auto-control of reaction temperature, pressure, flow, and transfer sequence by implementing a control unit in the system.
Referring to Figure 1 and 2, a continuous microreactor system (100) (maybe interchangibly referred to as (200), for continuous mode reaction comprises a controller unit (101), a cloud network (102), a server (103), and a continuous microreactor segment (104). Hereinafter, the continuous microreactor system (100) may be interchangeably referred to as a ‘system’, a ‘system (100)’, or a ‘microreactor system’.
In one embodiment, the system (100) for continuous mode reaction is a smart and compact system enabled for online integrated reaction monitoring and control in reactions such as polymer synthesis, emulsion polymerizations and formulations.
In one embodiment, the controller unit (101), a server (103), at least one continuous microreactor segment (104) may be interoperated via the cloud network (102) in a wired or wireless network control configuration.
It is preferable that each of the components mentioned above with reference to Figure 1 and Figure 2 be operatively connected to a controller unit (101) described below so as to enable the control means to control their operations.
Examples of the controller unit (101) may comprise control means provided with CPU, ROM, RAM and similar components. The ROM of the control means is a device for storing a program which controls the one or more feed transfer unit and mixing devices. The RAM of the controller unit (101) is a device for temporary storing data of the temperatures, mass flow, pressure, in cleaning mechanism in one or more microreactors segments of the microreactor system (100) to execute the instructions of via the processor. The CPU of the control means executes the program stored in the ROM based on reaction data. An example of the control by the control means (controller unit) of the continuous microreactor system (100) will be described below.
Further, in the embodiment shown in Figure 1, the controller unit (101) and server (103) may be integrated as a single unit or positioned separately at different locations. The controller unit (101) may comprise a microcontroller enabled for compact operation and for sending and receiving input from the server (103) or an input module (not shown) via a cloud network (102) and accordingly managing operation of the continuous microreactor system. In another embodiment, a controller unit (101) comprising microcontroller is enabled to monitor and receive input from the components and send the data to server (101) for analysis via cloud (102) network.
In another embodiment, the continuous microreactor system (100) is an edge control system enabled for the local and automated control of parameters such as reactor temperature, pressure, flow rate of reactants, control of one or more valves, and one or more feed transfer unit units through a controller unit (101) connected to a cloud (102) network for data storage and analysis, remote monitoring and control, and alerting over one more communication modes.
In one embodiment, the total mass flow rate maintained by the system (100) is in the range of 1 to 100 gm/min and preferably 2 to 40 gm/min. The temperature of the system may be between 20°C to 110°C, and preferably 50°C to 90°C. A reaction residence time of the system (100) is in a range of 1 to 75 min, and preferably 5 to 45 min.
Referring to Figure 1 and 2, the continuous microreactor system (200) may comprise the continuous microreactor segment (104). The continuous microreactor segment (104) may comprise at least one microreactor unit (204, 205), wherein each microreactor unit (204) may comprise at least one micro-reactor coil 204(a) or a second micro-reactor coil 204(b). The continuous microreactor segment (104) may comprise at least one of a feed transfer unit. The feed transfer unit may be one or more pumps P1 (201), P2 (202), P3 (208), and P4 (209). The continuous microreactor segment (104) may comprise one or more microreactor units (204, 205) each comprising a first micro-reactor coil 204(a) or a second micro-reactor coil 204(b). The continuous microreactor system (200) may comprise further a first mixing device (203) in the continuous microreactor segment (104), and a second mixing device (210).
The continuous microreactor system (100) is configured to carry out reactions comprising a primary reactant fed via at least one feed transfer unit P1 (201), and secondary reactants fed via at least one feed transfer unit P2 (202) to at least one of the first mixing device (203) or at least one of the second mixing device (210).
The continuous micro-reactor system comprises a first feed transfer unit (P1) for charging at least one primary reactant to at least one of the first micro-reactor coil 204(a) or the second microreactor coil 204(b) via the first mixing device (203).
The continuous microreactor system comprises a second feed transfer unit (P2) for simultaneous charging of at least one secondary reactant to at least one of the first micro-reactor coil 204(a) or the second microreactor coil 204 (b) via the first mixing device (203).
The term ‘primary reactant(s)’ as used herein is part of a major stream of main reactants such as but not limited to starting material, reaction intermediate, active ingredients, monomer, seed monomer, or base reactants. The term ‘secondary reactant(s) as used herein are part of a second optional stream of reactants comprising one or more secondary reactants such as but not limited to chain extender, extenders, intermediates, solvents, reagents, additives, initiator, emulsifiers, coagulants, and catalyst mixture.
In a related embodiment, the at least one microreactor unit (204), (205) may comprise a set of one or more micro-reactor coils (204 (a), 204 (b)) integrated with the controller unit (101).
The continuous microreactor segment (104) may comprise at least one of the first mixing device (203) connected to at least one of a first micro-reactor coil (204(a)), or a second micro-reactor coil (204(b). The micro-reactor coil (204(a)), and the second micro-reactor coil (204(b)), are connected to the at least one of the second mixing device (210) in a continuous manner via a back-pressure control valve (207).
In another embodiment, the micro-reactor coil (204(a), 204(b)) is a helically coiled tube of length ranging from 2 meter to 16 meter. In an embodiment, an internal diameter of the micro-reactor coil (204(a), 204(b)) is ranging from 2mm to 6mm. The external diameter of the micro-reactor coil (204(a), 204(b)) ranging from 3mm to 10mm.
In one embodiment, the micro-reactor coil is made of material selected from perfluoroalkoxy alkanes (PFA), fluorinated ethylene propylene (FEP) or polytetrafluoroethylene (PTFE). In another embodiment, the micro-reactor coil (204(a), 204(b)) is selected as but not limited to the PTFE coil.
In one embodiment, the first mixing device (203) and second mixing device (210) may be a static or dynamic mixer. Preferably, the first mixing device (210) is a static mixer enabled to mix at least two immiscible flows of synthetic product and mixture of formulating ingredients wherein temperature is atmospheric. In one embodiment, the static mixer may be any of but not limited to laminar flow regime static mixer, turbulent flow regime static mixer, plug flow reactor, disc static mixer, inclined plate static mixer, helical static mixer, non-clogging static mixer, and heat exchanger static mixer. In one embodiment, the one or more mixing devices (203, 210) are manufactured by 3D printing technology. Preferably, the static mixer is selected from at least one of a helical mixer, SMX mixer, or zig-zag mixer.
In a related embodiment, the first mixing device (203) or the second mixing device (210) is a static mixer enabled to mix at least two miscible or immiscible flows of the primary reactants or secondary reactants.
In one embodiment, the controller unit (101) is configured to adjust a temperature, mixing speed, residence time, and transfer action of the reactants in the mixing device (203, 210) as per the reaction requirements to avoid formation of any undesired side products. In one embodiment, the first mixing device (203) or the second mixing device (210), is configured to keep a temperature of the one or more reactants or materials below the primary reaction temperature of a reaction carried out in the continuous microreactor system (100). The maintenance of lower temperature in a range of 30°C to 50°C in the mixing devices enable elimination of radicals or side products formation in the reaction.
In a related embodiment, the first mixing device (203) may be a single piece mixing section length of 1cm to 15cm length, and an internal diameter ranging from 3mm to 15mm, and preferably 3mm to 6mm. In another embodiment, the first mixing device (203) is a static mixer made of a single piece mixing section of 1mm to 120mm, and preferably 10mm to 100mm, and more preferably 30mm to 80mm. The internal diameter of a static mixing device may range from 5cm to 50cm, and preferably 7cm to 40cm.
In a related embodiment, the second mixing device (210) may be a single piece mixing section length of 1cm to 15cm length, and an internal diameter ranging from 3mm to 15mm, and preferably 3mm to 6mm. In another embodiment, the second mixing device (210) is a static mixer made of a single piece mixing section of 1mm to 120mm, and preferably 10mm to 100mm, and more preferably 30mm to 80mm. The internal diameter of a static mixing device may range from 5cm to 50cm, and preferably 7cm to 40cm.
In one embodiment, the at least one continuous microreactor segment (104) may comprise a first feed transfer unit (P1) (201), configured for charging a first stream of a primary reactants to a first micro-reactor coil (204 (a)) or a second micro-reactor coil (204(b)) via the first mixing device (203). The second feed transfer unit (P2) (202) may be configured for simultaneous charging of secondary reactants to a first micro reactor coil 204(a) or second microreactor coil 204(b) via the first mixing device (203).
In one embodiment, the one or more feed transfer units (P1, P2, P3…, Pn) may be any of but not limited to a conveyor unit, pneumatic conveyors, rotary feeder, diaphragm pump, syringe pump, peristaltic pump, HPLC pump, micro pump, a micro syringe pump, or a combination thereof. Each of these feed transfer units serves different purposes of feed transfer depending on phase (solid, liquid, gas) and properties of the feed.
In one embodiment, the term ‘feed’ as used herein can be referred to any of the primary reactants or the secondary reactants.
In one embodiment, the micro-reactor unit (204) is configured for online receiving of one or more secondary reactants such as chaser catalyst, retardants, initiators, in the continuous flow of the micro-reactor coil in a first mixing device (203) via at least one of the feed transfer unit P1 (201), and P2 (202).
Further, the continuous microreactor system (100) is configured for series or parallel arrangement of the at least two microreactor segments (104) as per the reaction scale requirements. The continuous microreactor segment (104) ccomprising one or more micro-reactor units (204), (205) may include at least one microreactor coil (204 (a), 204 (b)). Each of the microreactor coils (204 (a), 204 (b)) of the single microreactor unit (204) are connected in series.
In one embodiment, the continuous microreactor segment (104) may comprise a plurality of micro reactor units (204), (205) …, n, each comprising one or more micro-reactor coils (a) and/or (b) enabling continuous polymerization reaction.
In one embodiment, one or more microreactor coil (204 (a), 204 (b)) may be at least one of helical coil, spiral coil, zig-zag coil, serpentine coil, T-type coil, Y-type coil, coriolis coil, multi-channel coil, 3D printed microreactor coil, capillary coil, and combination thereof.
The one or more microreactor coil (204 (a), 204 (b)) in combination with at least one feed transfer unit (P) may be enabled to induce any one of but not limited to turbulent flow, transitional flow, pulsatile flow, slug flow, plug flow, oscillatory flow, chaotic flow, laminar flow and a combination to facilitate an efficient reaction of a primary reactants and secondary reactants.
In one embodiment, the system (100) may comprise at least one temperature control bath (206, 211) to maintain a distinct temperature zone within each of the microreactor segment (104), the first mixing device (203), and the second mixing device (210).
The temperature-controlled bath (206) maintains and regulates temperature of the one or more microreactor segments (104) comprising at least one microreactor coil (204(a), 204(b)). The plurality of temperature control baths, each configured to maintain a distinct temperature zone within the microreactor system. The temperature control bath may include an integrated heating element and a cooling system to achieve precise temperature regulation.
In one embodiment, the micro reactor unit (204) is immersed in a first temperature control bath (206). The continuous micro-reactor system (100) may further comprise at least one temperature controlled bath (211) to maintain and regulate a temperature of at least one mixing device (210).
In one embodiment, the one or more temperature control baths (206, 211) may be selected from a module integrated with the controller unit (101) enabled for optimizing/adjusting temperature as per specific primary reactant and is electronically connected to an online smart control system configured to maintain a constant temperature.
The micro-reactor unit (204) kept in bath selected from a temperature-controlled bath (205, 211) is enabled for optimizing temperature as per specific primary reaction component and is electronically connected to the controller unit (101) such as online smart control system (101) configured to maintain a constant temperature. For the temperature control bath (206, 211) selected as water bath, the online smart control system (101) enables temperature between 50°C to 90°C.
In one embodiment, the first and second temperature control baths (206, 211) are selected from but not limited to sensor-based temperature control bath, temperature control bath comprising a fluid medium, a peltier module bath, cryogenic bath, thermoelectric bath or a combination thereof. In one embodiment, the fluid medium temperature-controlled baths (206), (211) may be selected from water, glycol-water mixture, oil, alcohol, liquid nitrogen, refrigerant, salt solutions, silicone fluids, thermal fluids, or antifreeze solutions. Said temperature control bath is configured to maintain a temperature gradient along the length of the microreactor coil, enabling multiple temperature-dependent reactions.
Referring to Figure 2, the continuous microreactor system (200) comprising continuous microreactor segment (104). The continuous microreactor segment (104) may comprise a back pressure controlling valve (207), and a product storage vessel (212). In one embodiment, the back pressure controlling valve (207) is configured to control the alternating flow of reactants from first micro-reactor coil 204(a) and/or a second micro-reactor coil 204(b) based on an input received from the controller unit (101).
Maintenance of a back-pressure is a very critical and important feature of the system (100) for maximum conversion and obtaining a high-quality end product. The back pressure control valve (207) may further comprise a pinch operated valve for the control of backpressure at required set-point.
The pinch operated valve may comprise an on-off flap maintains the back-pressure in a range of 0 to 6 bar and residence time in a range of 5 to 45 minutes of the reactant in the one or more micro-reactor coils (204(a), 204(b)) of the microreactor segment (104), and also avoids chocking of the reactants in the valve (207). Optionally, the on-off flap of the pinch valve is controlled by an overhead motor (not shown in figure) monitored and controlled by a microcontroller (101).
The continuous microreactor system (100) may comprise a microreactor segment (100) for a continuous reaction such as continuous polymerization reaction or continuous emulsion polymerization reaction. The microreactor segment (104) may comprise the first mixing device (203) for mixing of at least one of a primary reactant such as monomer and a secondary reactant additive.
The microreactor segment (104) may comprise a first micro-reactor coil 204(a), a second micro-reactor coil 204(b) and a back pressure control valve (207). The back pressure control valve (207) may be enabled to control and alternating flow of the primary reactant and the secondary reactant from the from the first mixing device (203) to at least one of the first micro-reactor coil 204(a) or the second micro-reactor coil 204(b).
The second mixing device (210) in line with the back-pressure control valve (208) of the continuous microreactor segment (104) is configured for mixing of primary reactant i.e. a reaction intermediate received from a back pressure control valve (207) with a secondary reactant auxiliary additive.
The microreactor system (100) is further configured for a cleaning in process mechanism operated via a controller unit (101). The cleaning in progress mechanism is configured to avoid chocking of unreacted primary and secondary reactants in a canal of the micro-reactor coil.
The continuous microreactor segment (104) further may comprise a cleaning fluid input tank (213) controlled via an isolation valve control alternate cleaning of the micro-reactor coils (204(a), and 204(b)). The isolation vale is configured to control ON/OFF mechanism of the cleaning flow and direction. The isolation valve enables in-process alternate cleaning of the micro-reactor coils (204(a), and 204(b)).

The cleaning fluid may be any one of a detergent, passivation material, water, thinner, solvent, or a reaction medium.
In a related embodiment, the micro reactor unit (204) may be further configured for cleaning in process (CIP). In one embodiment, a second micro-reactor coil (204 (b)) is also immersed in the temperature-controlled bath (206) enabled to operate whilst a first micro-reactor coil (204(a)) is not active or under maintenance. The in-process cleaning mechanism can be carried out while continuous reaction is taking place in an another microreactor coil simultaneously.
In a related embodiment, referring to Figure 1 and 2, the plurality of isolation valves are controlled by the controller unit (101). Further, the plurality of isolation valves selected as ON/OFF valves enable in-process cleaning of either first micro-reactor coil (204(a)) or a second microreactor coil (204(b)) of the microreactor segment (204), while the other micro-reactor coil not in cleaning can be incorporated in the continuous reaction. The implementation of the in-process cleaning mechanism avoids choking and production loss in the microreactor segment (204).
In one embodiment, each of the microreactor unit (204) may be further configured to time-based cleaning in process (CIP) by adjusting opening and closing of the back pressure controlling valve (207) between each of the first micro-reactor coil (204(a)) and/or a second micro-reactor coil (204(b)) of the micro-reactor segment (204).
The clean in process (CIP) mechanism is configured for longer, continuous and sustainable operation of the continuous reaction. The back pressure controlling valve (207) is for maintaining system pressure and controlling the primary and secondary reactant flow of an intermediate reaction product formed to the second mixing device (210).
The combination of cleaning-in-progress mechanism and the back pressure controlling valve (207) enables without interruption smooth operation of the system (100). The cleaning-in-progress mechanism and the back pressure controlling valve (207) reduces overall time cycle of the continuous microreactor system (100, 200) to 0.5 Hr to 4 Hr.
In one embodiment, the wherein at least one micro-reactor coil 204(a) of the continuous microreactor segment (104) is configured to stay in cleaning process and transfer the cleaning waste to a separate collector tank (not shown in figure), while at least another micro-reactor coil (204(b)) is configured for processing of the reaction and transferring the reaction mixture to the second mixing device (210) via a back-pressure control valve (207).
Further, the back-pressure control valve (207) transfers the reaction mixture to a second mixing device (210) immersed in a second temperature control bath (211) to obtain a reaction intermediate product.
The second mixing device (210) is further configured for receiving a reaction mixture from the microreactor unit (204) of the microreactor segment (104) via the back-pressure control valve (207). The reaction intermediate product may either be received through a feed transfer unit P3 (208) or directly from in-flow conduit line of the back-pressure control valve (207) into the at least one second mixing device (210).
Optionally, the at least one second mixing device (210) is configured to receive one or more formulation additives obtained from a feed transfer unit P4(209) to prepare a formulation from the intermediate product ready for packaging. An outlet of the one second mixing device (210) may further be connected to an auxiliary mixing device (now shown in figure), or to an another microreactor segment (104).
In one embodiment, the controller unit (101) is configured to send an alert to a user for error detection, cleaning notifications, reaction completion notification.
The one or more formulation additives may be any one of but not limited to a copolymer, a secondary reactant, auxiliary agents such as but not limited to chain extender, extenders, intermediates, solvents, reagents, additives, initiator, emulsifiers, coagulants, catalyst mixtures, accelerators, retardants, promoters, solvents, cleaning agents, or chelates.

In another embodiment, the micro-reactor unit (204) may be selected as a continuous flow reactor with a heat control technology. The micro-reactor unit (204) may comprise a thermoelectric cooling system for heat control.
In one embodiment, the continuous micro reactor system is configured to carry out one or more types of organic, inorganic, or hybrid reactions. The micro-reactor unit (204) is configured for controlled, accurate, and continuous conversion of the primary reactants and other secondary reactants or reagents.
In one embodiment, the one or more reaction carried out in the disclosed continuous microreactor system may be any of but not limited to nanocomponent manufacturing, rubber, polyurethane articles, construction materials, adhesives, paints and coatings, paper and paperboard coating, carpet backing, and textiles.
Moreover, the continuous microreactor system may also be implemented in the multiphase reactions such as dispersion in solvent or water, catalysis, solid-liquid process, purification, gas-gas, gas-liquid, and particle dispersion.
In some embodiment, the continuous microreactor system may be implemented for polymerization reactions such as copolymerization, dimerization, emulsion polymerization, bulk polymerization, solution polymerization, suspension polymerization, radical polymerization, anionic polymerization, cationic polymerization, ring opening polymerization, and step growth polymerization.
In a related embodiment, the polymerization may be carried out for polymerization of one or more monomer or comonomers selected from but not limited to group of vinyl monomers, acrylic monomer, such as but not limited to alkene monomers, acrylate methacrylate monomers, vinyl monomers, styrene monomers, epoxy monomers, monomers with various functional groups, lactone monomers, biomolecular monomers, and amino acids.
In one embodiment, the monomers may be any of but not limited to functional groups as acids, esters, urethanes and such as vinyl acetate, vinyl chloride, vinyl alcohol, and group of acrylics such as acrylamide, acrylic acid, butadiene, styrene, acrylonitrile, acrylate ester and methacrylate ester monomers.
In one embodiment, the mixture of formulation ingredients may comprise secondary reactants such as but not limited to one or more additives, surfactants, buffers, catalysts, dyes, stabilizers, plasticizers, lubricants and flame retardants.

In another embodiment, the discloses system is configured for various polymerization products such as adhesives, paints, decorators, varnishes, construction chemicals, plasticizers, epoxy putty, resins, etc.

The system for continuous mode reaction, in an embodiment is a portable, compact, and inexpensive unit configured for a point of sell (POS), point of service, end use location for instant or express manufacturing of the fresh lot of the end-use product. The system may be mounted on a small vehicle or a benchtop and can be converted to a compact mobile manufacturing facility to operate just in time, or just in schedule model.

The system (100) may additionally comprise an external power back-up unit configured to connect over an enclosure of the system. The external power back-up unit may be any one of a generator unit, rechargeable battery, or photovoltaic/solar cell-based power supply thereby enabling green and portable manufacturing of the product through the continuous reaction.

In accordance with embodiment of the present disclosure, the system (100) of continuous reaction described above have following advantages including but not limited to: compact, portable, inexpensive low volume reaction, thereby minimizing contamination of content of residual monomer in reacted mass, efficient mixing of reactants and maximum conversion, reduction in overall reaction time, and exclusion of the choking problem in the system.

The small scale of the disclosed apparatus enables control, and safety is thereby reduces safety cost, and reduction in waste generation. The continuous reactor and system maintained constant reactant ratio unlike as the batch reaction where reactant ratio keeps changing with progress of reaction.
The embodiments, examples and alternatives of the preceding paragraphs, the description, including any of their various aspects or respective individual features, may be taken independently or in any combination. Features described in connection with one embodiment are applicable to all embodiments, unless such features are incompatible.
,CLAIMS:WE CLAIM:
1. A continuous microreactor system (100), comprising:
at least one of a micro-reactor segment (104) for a continuous reaction, comprising:
a first mixing device (203) for mixing of at least one of a primary reactant and a secondary reactant, a first micro-reactor coil 204(a), a second micro-reactor coil 204(b), and a back pressure control valve (207),
wherein the back pressure control valve (207) controls an alternating flow of at least one of the primary reactant and the secondary reactant from the first mixing device (203) to at least one of the first micro-reactor coil 204(a), or the second micro-reactor coil 204(b);
a second mixing device (210) connected to the first micro reactor segment (104) configured for mixing of the primary reactant received from a back pressure control valve (207) with the secondary reactant; and
a controller unit (101) in communication with the at least one micro-reactor segment (104).
2. The system (100) as claimed in claim 1, comprising at least one of a feed transfer unit P1(201), P2(202), P3(208), or P4(209) to transfer at least one of the primary reactant or the secondary reactant to one or more mixing devices (203, 210) or to one or more microreactor segments (104).
3. The system (100) as claimed in claim 1, wherein the first mixing device (203) is connected to the first microreactor coil (204(a)), and at least one second microreactor coil (204(b)).
4. The system (100) as claimed in claim 1, wherein the first micro-reactor coil (204(a)), and the second micro-reactor coil (204(b)), are connected to at least one of the second mixing device (210) via the back-pressure control valve (207).
5. The system (100) as claimed in claim 4, wherein the back pressure control valve (207) comprises a pinch operated valve to control backpressure at a required set-point.
6. The system (100) as claimed in claim 5, wherein the pinch operated valve comprises an on-off flap to maintain a back-pressure and residence time of the reactant in the at least one micro-reactor (204(a), 204(b)).
7. The system (100) as claimed in claim 1, wherein the micro-reactor segment (104) comprises a cleaning fluid input tank (213) controlled via at least one isolation valve to control in-process alternate cleaning of the micro-reactor coils (204(a), and 204(b)).
8. The system (100) as claimed in claim 7, wherein the isolation valve is configured to keep the at least one micro-reactor coil (204(a) to stay in cleaning processes and transfer the cleaning waste to a separate collector tank, and at least another micro-reactor coil (204(b) for continuous reaction.
9. The system (100) as claimed in claim 1, wherein the at least one microreactor is at least one of a helical coil, spiral coil, zig-zag coil, serpentine coil, T-type coil, Y-type coil, coriolis coil, multi-channel coil, 3D printed microreactor coil, and capillary coil.
10. The system (100) as claimed in claim 1, wherein at least one of the micro-reactor coil (204(a), 204(b)) is selected from at least one of a polytetrafluoroethylene (PTFE) coil and per-fluoro alkoxy (PFA) alkane coil, and fluorinated ethylene propylene (FEP) coil.
11. The system (100) as claimed in claim 1, wherein the one or more mixing devices (203, 211) are a static mixer enabled to mix at least two immiscible flows of at least one of the primary reactant and the secondary reactant.
12. The system (100) as claimed in claim 1, wherein a surface to volume ratio of the microreactor segment (104) is 800 to 2000.
13. The system (100) as claimed in claim 1, wherein a total mass flow rate of the primary and secondary reactants in the microreactor segment (104) is 2 to 40 gm/min.
14. The system (100) as claimed in claim 1, wherein a residence time of reactant in the microreactor segment (104) is 5 to 45 min.
15. The system (100) as claimed in claim 1, wherein a duration of a single cycle of the continuous reaction is between 0.5 to 4 hrs.
16. The system (100) as claimed in claim 1, wherein the system (100) comprises at least one of a temperature control bath (206, 211) to maintain a distinct temperature zone within each of the microreactor segment (104), the first mixing device (203), and the second mixing device (210).
17. The system (100) as claimed in claim 1, comprises an external power back-up unit.
18. The system (100) as claimed in claim 1, wherein the controller unit (101) is configured to send an alert to a user for error detection, cleaning notifications, reaction completion notification.