A modular continuous liquid phase synthesis mixing system

Abstract

The application provides a modular continuous liquid-phase synthesis mixing system, and relates to the technical field of chemical equipment, comprising an emulsifying device, a pump and at least one peristaltic mixing device; the emulsifying device, the pump and a plurality of peristaltic mixing devices are sequentially connected through pipelines; the emulsifying device can stir initial reaction raw materials, the pump is used for pumping the initial reaction raw materials into the peristaltic mixing device, an intermediate raw material adding port is arranged on a connecting pipeline between the peristaltic mixing device and the pump, and all the reaction raw materials are continuously peristaltically extruded to simulate stirring to realize continuous stirring and mixing reaction of the system. The scheme provided by the application can ensure the expansion of the reaction system, and the mixing system can realize a reaction process similar to the laboratory reaction condition, so as to meet the pilot scale-up demand of the present innovation achievements.

Description

Technical Field

[0001] This invention relates to the field of chemical equipment technology, and in particular to a modular continuous liquid phase synthesis and mixing system. Background Technology

[0002] The purpose of chemical reaction scale-up is to successfully replicate optimal small-scale chemical processes from the laboratory on large-scale commercial facilities. This ensures similar conversion rates, similar selectivity, and safety and reliability.

[0003] Generally, the stability of laboratory-scale reactions (such as those synthesizing less than 10g per batch) is related to the system size and is affected by factors such as molecular thermal motion and reactant concentration uniformity during the reaction. Therefore, laboratory reactions often experience reduced yields, increased byproducts, or even reaction failure during pilot-scale expansion. In nanoparticle preparation, reactions based on co-precipitation or in-situ solution preparation methods also encounter similar problems during scale-up. Specifically, fluctuations in raw material concentration, uneven stirring, and changes in reactant addition time can lead to uneven particle size, decreased dispersibility, and reduced product quality stability. Consequently, the quality of industrially produced nanoparticles is often inferior to that obtained from small-scale laboratory reactions, which can fatally impact the performance stability and advantages of nanoparticle applications. This limits the application of nanoscience in the market, preventing new high-quality nanoparticles from entering the market, and also lowers market evaluation of nanoscience achievements, further hindering their market entry.

[0004] The current pilot-scale process for chemical reactions often involves first scaling up the reaction at a constant scale in a reactor to observe its stability. Then, specific parameters such as stirring rate, feed ratio, feeding time, and reaction temperature are adjusted to bring the reaction yield close to the laboratory reaction efficiency. This also considers the reactor's stirring method, shape, and fluid dynamics parameters during the feeding process to achieve a stirring efficiency similar to that in the laboratory reaction, ultimately achieving pilot-scale scale-up. For example, the utility model patent with authorization publication number CN214636163U describes a reaction conducted in a mixing vessel. This same process is repeated when the reaction system is further scaled up. This process is clearly inefficient, difficult, time-consuming, labor-intensive, risky, and has a low return on investment. Sometimes it even involves the redevelopment and optimization of reaction equipment, thus severely hindering industry's willingness to invest in new scientific research achievements. Another way to rapidly scale up reactions for nanoparticle preparation is through microfluidics. This involves constructing reaction channels and microreactors on a substrate using photolithography, followed by pumps and control panels to regulate the flow of liquid within the channels at a specific rate, enabling continuous reaction. However, this method suffers from several drawbacks. First, the design and volume of the mixing chamber are highly dependent on its size, making it difficult to scale up the designed channels directly. Second, the channels are prone to blockage when applied to nanomaterials, potentially leading to equipment failure. Therefore, currently, there is no mixing system that can rapidly scale up the reaction while maintaining reaction conditions similar to laboratory conditions to meet the requirements for pilot-scale production of current innovative technologies. Summary of the Invention

[0005] The purpose of this invention is to provide a modular continuous liquid phase synthesis mixing system to solve the problems existing in the prior art. This mixing system can quickly scale up the reaction system while maintaining reaction conditions similar to those in the laboratory to meet the needs of pilot-scale amplification of current innovative achievements.

[0006] To achieve the above objectives, the present invention provides the following solution:

[0007] This invention provides a modular continuous liquid-phase synthesis and homogenization system, including an emulsification device, a pump, and at least one peristaltic mixing device; the emulsification device, the pump, and several peristaltic mixing devices are sequentially connected by pipelines; the emulsification device can stir the initial reaction raw materials, the pump is used to pump the initial reaction raw materials into the peristaltic mixing devices, and an intermediate raw material addition port is provided on the connecting pipeline between the peristaltic mixing devices and the pump; all reaction raw materials undergo continuous peristaltic extrusion and simulated stirring in the peristaltic mixing devices to achieve continuous stirring and mixing reaction of the system.

[0008] Preferably, it also includes a mixer, with one mixer provided before each of the peristaltic mixing devices. The newly added reaction raw materials and the original reaction raw materials or intermediate products are stirred and mixed in the mixer before being introduced into the peristaltic mixing device.

[0009] Preferably, the flow rate of the pump is controllable.

[0010] Preferably, a set of pumps connected in series and several peristaltic mixing devices are referred to as a reaction string group, and a reaction system may include one emulsifying device and multiple reaction string groups.

[0011] Preferably, the peristaltic mixing device includes a roller assembly, a housing, and a peristaltic pipe. The peristaltic pipe is spiral-shaped and covers the inner wall of the housing. The roller assembly includes multiple rollers arranged around a circumference. The multiple rollers are disposed inside the housing, and when the rollers rotate around the circumference, they can continuously squeeze the peristaltic pipe to achieve the peristaltic movement of the material inside the peristaltic pipe towards the outlet of the peristaltic pipe.

[0012] Preferably, the roller assembly includes a plurality of rollers, a central column, and a motor. At least a portion of the central column is inserted into the housing. The rollers are disposed around the periphery of the central column. The motor drives the central column to rotate and causes the rollers to rotate around the axis of the central column.

[0013] Preferably, the inlet of the peristaltic pipe is located at the bottom, and the outlet is located at the top.

[0014] The present invention achieves the following technical effects compared to the prior art:

[0015] The modular continuous liquid-phase synthesis mixing system provided by this invention employs a peristaltic mixing method to continuously stir and mix the reactants, simulating stirring. By reacting continuously in a small-diameter tube, a large amount of raw material is continuously fed into a controllable small-volume reaction tube (peristaltic pipe), resulting in continuous product output after the raw material reacts through the mixing system. This ensures controlled reaction efficiency during large-scale product production in the laboratory, assisting in rapidly increasing production capacity and bringing innovative laboratory results to market. Furthermore, this mixing system can quickly scale up the reaction system while maintaining reaction conditions similar to those in the laboratory, meeting the current requirements for pilot-scale amplification of innovative achievements. Attached Figure Description

[0016] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0017] Figure 1 A schematic diagram of the modular continuous liquid phase synthesis and homogenization system provided by the present invention;

[0018] Figure 2 This is a schematic diagram of the peristaltic mixing device;

[0019] Figure 3 This is a schematic diagram of the structure of the central column and rollers;

[0020] Figure 4 This is a schematic diagram of the outer shell structure;

[0021] In the diagram: 1-Emulsifying device; 2-Pump; 3-Mixer; 4-Peristaltic mixing device; 5-T-joint; 6-Flow meter; 7-Booster pump; 41-Outer shell; 42-Adjusting plate; 43-Center column; 44-Roller; 45-Base; 46-Inlet of peristaltic mixing device; 47-Concave groove. Detailed Implementation

[0022] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0023] The purpose of this invention is to provide a modular continuous liquid phase synthesis mixing system to solve the problems existing in the prior art. This mixing system can quickly scale up the reaction system while maintaining reaction conditions similar to those in the laboratory to meet the needs of pilot-scale amplification of current innovative achievements.

[0024] To make the above-mentioned objects, features and advantages of the present invention more apparent and understandable, the present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments.

[0025] This invention provides a modular continuous liquid-phase synthesis and homogenization system suitable for scale-up of chemical reactions, especially for scale-up of nanoparticle preparation processes, such as... Figure 1As shown, the system includes an emulsifying device 1, a pump 2, and at least one peristaltic mixing device 4. The emulsifying device 1, pump 2, and several peristaltic mixing devices 4 are sequentially connected via pipelines. The emulsifying device 1 stirs the initial reaction materials, and the pump 2 pumps the initial reaction materials to the peristaltic mixing devices 4. An intermediate material addition port is provided on the connecting pipeline between the peristaltic mixing devices 4 and the pump 2. All reaction materials undergo continuous peristaltic extrusion and mixing within the peristaltic mixing devices 4 to achieve continuous mixing and reaction of the system. Specifically, a T-joint 5 can be installed on the connecting pipeline, with one port serving as the intermediate material addition port. Alternatively, other methods can be used, such as directly creating an opening on the connecting pipeline.

[0026] Among them, the diameter of the peristaltic pipe in the peristaltic mixing device 4 is much smaller than the size of the reaction chamber in the existing scaled-up reaction, which is similar to the laboratory reaction conditions. Moreover, the length of the peristaltic pipe is relatively long, which can realize continuous feeding and continuous reaction.

[0027] The modular continuous liquid-phase synthesis mixing system provided by this invention employs a peristaltic mixing method to continuously stir and mix the reactants, simulating stirring. By reacting continuously in a small-diameter tube, a large amount of raw material is continuously fed into a controllable small-volume reaction tube (peristaltic pipe), resulting in continuous product output after the raw material reacts through the mixing system. This ensures controlled reaction efficiency during large-scale product production in the laboratory, assisting in rapidly increasing production capacity and bringing innovative laboratory results to market. Furthermore, this mixing system can quickly scale up the reaction system while maintaining reaction conditions similar to those in the laboratory, meeting the current requirements for pilot-scale amplification of innovative achievements.

[0028] In some embodiments, the modular continuous liquid phase synthesis and homogenization system provided in this embodiment also includes a homogenizer 3. A homogenizer 3 is provided before each peristaltic homogenizing device 4. The newly added reaction raw materials and the original reaction raw materials or intermediate products are stirred and mixed in the homogenizer 3 before being passed to the peristaltic homogenizing device 4.

[0029] The peristaltic mixing in the above embodiments is only to simulate the stirring in the reaction process, and its mixing effect is poor. Therefore, the mixer 3 in this embodiment can pre-stir and mix the newly added reaction raw materials with the original reaction raw materials or intermediate products, and then discharge them into the peristaltic mixing device 4 for continuous peristaltic mixing reaction after thorough mixing.

[0030] In some embodiments, the pump 2 in the solution provided in this embodiment is a metering pump with controllable flow rate, so as to adjust the reaction time according to the reaction raw materials. When the flow rate of pump 2 is high, the time of the raw materials in the peristaltic pipe is short, and the reaction time is correspondingly shortened. Conversely, when the flow rate of pump 2 is low, the time of the raw materials in the peristaltic pipe is long, and the reaction time is correspondingly extended.

[0031] In some embodiments, a booster pump 7 is provided between the mixer 3 and the peristaltic mixing device 4, a flow meter 6 is provided at the outlet of the pump 2, and a flow meter 6 is also provided at the intermediate raw material addition port of the tee head.

[0032] In some embodiments, a set of pumps 2 connected in series and several peristaltic mixing devices 4 are referred to as a reaction string group, and a reaction system may include an emulsifying device 1 and multiple reaction string groups.

[0033] This embodiment achieves an increase in the production rate of reaction products under the premise of unchanged reaction conditions by using parallel equipment. The more reaction series groups are set, the greater the scale-up will be.

[0034] In addition, when only one reaction string group is set up, and the reaction string group includes multiple peristaltic mixing devices 4, a one-pot multi-step reaction can be realized.

[0035] In some embodiments, such as Figures 2-4 As shown, the peristaltic mixing device 4 includes a roller assembly, a housing 41, and a peristaltic conduit. The peristaltic conduit is spiral-shaped and covers the inner wall of the housing 41. The roller assembly includes multiple rollers 44 arranged in a circle within the housing 41. As the rollers 44 rotate around the circumference, they continuously compress the peristaltic conduit, causing the material inside to move towards the outlet of the peristaltic conduit. The inner diameter of the peristaltic conduit is 8mm-10mm, and it is a flexible tube, preferably a silicone tube. The inner wall of the housing 41 has concave grooves 47 for coiling and fixing the peristaltic conduit, and the housing 41 itself can achieve temperature control through an internal temperature control structure.

[0036] The roller assembly includes multiple rollers 44, a central column 43, and a motor. At least a portion of the central column 43 is inserted into the housing 41. The rollers 44 are arranged around the central column 43. The motor drives the central column 43 to rotate and causes the rollers 44 to rotate around the axis of the central column 43. The motor is connected to the upper part of the central column 43 through a coupling.

[0037] The inlet of the peristaltic tube is located at the bottom, and the outlet is located at the top.

[0038] In order to enable the central column 43 to drive the roller 44 to rotate, an adjusting plate 42 is fixedly installed on both the upper and lower parts of the central column 43. The roller 44 is located between the two adjusting plates 42, and both ends of the roller 44 are connected to the adjusting plates 42. The central column 43 drives the adjusting plates 42 to rotate, and the adjusting plates 42 drive the roller 44 to rotate. In addition, a base 45 is also provided. The central column 43 is connected to the base 45 through a plane bearing. The base 45 is fixedly installed at the lower end of the outer shell 41.

[0039] In some embodiments, the adjusting plate 42 is provided with multiple holes, and the distance between the multiple holes and the center line of the adjusting plate 42 is not completely consistent. The roller 44 is detachably connected to the holes, and the degree of compression on the peristaltic tube can be adjusted by adjusting the position of the roller 44 on the adjusting plate 42.

[0040] In some embodiments, a roller is rotatably fitted around the roller 44, and the roller 44 is rotatably connected to the roller 44 via a bearing. In use, the outer wall of the roller squeezes the peristaltic channel, and the roller can rotate, thereby improving the peristaltic squeezing effect.

[0041] Based on the above structure, the solution flows counterclockwise (top view) inside the silicone tube within the outer shell 41 from bottom to top. When the stepper motor is energized, the motor drives the coupling, which in turn drives the adjusting plate 42 and the roller 44 to rotate clockwise (top view). The compression of the silicone tube by the roller 44 does not seal off the internal space of the silicone tube. Therefore, when the solution continues to flow inside the silicone tube, the flow rate increases when it encounters the compression point of the roller 44, and decreases after passing through it, thus achieving stirring. By controlling the flow rate and the stepper motor speed, the time and number of mixing cycles (or rate) of the liquid in the silicone tube passing through the mixer 3 can be adjusted. At the same time, changing the position of the roller 44 on the adjusting plate 42 can control the mixing force.

[0042] This invention addresses the problems of increased byproducts, reduced yield, and decreased product quality caused by scale-up in existing one-pot reactions and nanomaterial preparation reactions. While the system provided by this invention can continuously react large quantities of raw materials, the volume of the reaction system remains unchanged during the actual reaction (the reaction takes place in a peristaltic tube of 8mm-10mm). Therefore, it avoids the decrease in reaction efficiency or quality caused by stirring, molecular thermal motion, and system temperature instability during volume scaling. Furthermore, reaction parameters can be easily controlled through simple equipment adjustments, offering significant advantages over existing reactors in terms of reaction parameter control and reaction system management. Secondly, particularly for nanoparticle preparation, this system can achieve nanoparticle surface modification and functionalization, core-shell structured nanoparticle preparation, and other methods based on nanoparticle formation through simple system cascading, without requiring the replacement of the reactor throughout the reaction process. Because the entire mixing process is continuous, each reaction step in the system is independent, and multi-step reactions can be implemented through system cascading. At the same time, this continuous flow reaction avoids the fact that the total realization time of each batch of reaction in the existing industrial molecular synthesis process is directly related to the reaction steps, but only to the volume of the reaction system.

[0043] This system is suitable for reaction systems of different volumes and can easily increase production capacity through parallel connection without further equipment debugging, avoiding equipment-related problems encountered during laboratory reaction scale-up. It is simple and easy to operate.

[0044] The peristaltic mixer 3 involved in this system provides more precise control of reaction parameters than similar reaction vessels, especially the control of parameters such as mixing speed and system temperature. Thanks to the small inner diameter of the silicone tube, this mixer 3 can achieve more uniform and rapid system temperature control. There is no need to consider the risk of reaction failure due to unstable temperature control or long temperature change time during reaction scale-up. In addition, the equipment is easy to start and stop, consumes little energy, and is particularly suitable for laboratory or laboratory capacity scale-up experiments and mass production of related products.

[0045] Specific examples have been used to illustrate the principles and implementation methods of this invention. The descriptions of the above embodiments are only for the purpose of helping to understand the method and core ideas of this invention. Furthermore, those skilled in the art will recognize that, based on the ideas of this invention, there will be changes in the specific implementation methods and application scope. Therefore, the content of this specification should not be construed as a limitation of this invention.

Claims

1. A modular continuous liquid-phase synthesis and homogenization system, characterized in that: The system includes an emulsifying device, a pump, and at least one peristaltic mixing device; the emulsifying device, the pump, and several peristaltic mixing devices are sequentially connected by pipelines; the emulsifying device can stir the initial reaction raw materials, the pump is used to pump the initial reaction raw materials into the peristaltic mixing devices, and an intermediate raw material addition port is provided on the connecting pipeline between the peristaltic mixing devices and the pump; all reaction raw materials undergo continuous peristaltic extrusion and simulated stirring in the peristaltic mixing devices to achieve continuous stirring and mixing reaction of the system; The peristaltic mixing device includes a roller assembly, a housing, and a peristaltic conduit. The peristaltic conduit is spiral-shaped and covers the inner wall of the housing. The roller assembly includes multiple rollers arranged in a circle within the housing. As the rollers rotate around the circumference, they continuously compress the peristaltic conduit to move the material inside the conduit towards its outlet. The roller assembly includes multiple rollers, a central column, and a motor. At least a portion of the central column is inserted into the housing. The rollers are positioned around the periphery of the central column. The motor drives the central column to rotate and causes the rollers to rotate around the axis of the central column.

2. The modular continuous liquid phase synthesis and homogenization system according to claim 1, characterized in that: It also includes a mixer, with one mixer provided before each of the peristaltic mixing devices. The newly added reaction raw materials and the original reaction raw materials or intermediate products are stirred and mixed in the mixer before being introduced into the peristaltic mixing device.

3. The modular continuous liquid phase synthesis and mixing system according to claim 1, characterized in that: The flow rate of the pump is controllable.

4. The modular continuous liquid phase synthesis and mixing system according to claim 1, characterized in that: A set of pumps connected in series and several peristaltic mixing devices are referred to as a reaction string group, and a reaction system includes one emulsifying device and multiple reaction string groups.

5. The modular continuous liquid phase synthesis and mixing system according to claim 1, characterized in that: The inlet of the peristaltic tube is located at the bottom, and the outlet is located at the top.

6. The modular continuous liquid phase synthesis and homogenization system according to claim 1, characterized in that: The inner wall of the outer shell has concave grooves for coiling and fixing the peristaltic tubes, and the outer shell itself achieves temperature control through an internal temperature control structure.

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