A comprehensive reaction device platform integrating flow reaction, fixed bed reaction and chromatography functions

Abstract

The invention relates to a comprehensive reaction device platform integrating the functions of circulation reaction, fixed bed reaction and chromatography. The platform comprises a touch liquid crystal screen connected to a PLC. The PLC is also respectively connected to a heating system, a refrigeration system, a delivery pump and an ultrasonic transducer. A plurality of delivery pumps are provided for delivering different reaction materials respectively. An intelligent control module, a pumping system, a temperature control and an oil bath system, and an ultrasonic module reaction flow channel are integrated into a set of instruments. Reaction flow channels of different materials and forms are configured. Ultrasonic waves are used to mix the reaction liquid in the flow channel. The functions of circulation reaction, fixed bed reaction, chromatography and the like are integrated together. With the support of an additional module, the functions of illumination reaction, microwave reaction and electrochemical reaction can be expanded. Function switching, reaction flow channel switching and flow channel extension are very easy and convenient to operate. The reaction flow channel has a simple structure and rich forms and materials to meet the requirements of different use environments.

Description

Technical Field

[0001] The present invention relates to the field of reaction devices, in particular to a comprehensive reaction device platform integrating flow reaction, fixed bed reaction and chromatography functions. Background Art

[0002] The heat transfer specific surface area of ​​a traditional reactor is 0.1 cm2 / ml to 0.05 cm2 / ml, and the heat transfer specific surface area of ​​a microchannel reaction is 100 cm2 / ml to 10 cm2 / ml, which differs by 3-4 orders of magnitude.

[0003] In recent years, microchannel continuous reaction has been increasingly valued in the fields of chemical industry, pharmaceutical industry, biology, etc., which depends on its unique structural advantages. The specific surface area of ​​microchannel reaction is thousands of times larger than that of traditional kettle reaction. The heat transfer specific surface area of ​​traditional reactor is 0.1cm2 / ml~0.05cm2 / ml, and the heat transfer specific surface area of ​​microchannel reaction is 100cm2 / ml~10cm2 / ml, which is 3-4 orders of magnitude different. The ability to control the thermal conditions of the reaction through the heat exchange medium is also thousands of times that of the traditional reactor. For thermally unstable substances or intermediate states, reactions need to be carried out at extremely low temperatures. The side reactions of unstable intermediate states are closely related to temperature and reaction time. The higher the temperature, the more significant the side reactions are, and the longer the time, the more obvious the side reactions are. Microchannel continuous reaction can solve these problems well. The large proportion of heat transfer area can maintain the rapid cooling of the reaction fluid to a temperature more suitable for the reaction. The heat released during the reaction process is instantly removed from the reaction system through heat exchange, ensuring the temperature stability of the reaction environment, thereby ensuring the stability of reaction conversion rate, yield, quality, impurities and other data.

[0004] When conducting dangerous chemical reactions, they are often accompanied by huge heat release. If the released heat cannot be removed from the reaction system in time, the heat generated will continue to increase the temperature of the reaction system. When the temperature reaches the boiling point of the solvent or the critical value of the secondary reaction, it will cause a serious safety accident. This is an important reason for many accidents in kettle reactions. Microchannel continuous production can solve this kind of problem very well. The huge heat transfer specific surface can control the temperature of the reaction fluid at a safe and optimal reaction temperature to ensure that the reaction is carried out within a safe range. The continuous reaction is carried out in the channel, and the volume of the reaction liquid in the channel is one thousandth to one ten-thousandth of that of the traditional reactor. Its risk factors will be greatly reduced, and the consequences of the impact can be greatly reduced.

[0005] Mass transfer conditions are important factors in chemical, biological and many physical processes. Traditional reactors will have spatial inhomogeneity during the stirring process. For example, when the specific gravity of the materials is different, the stirring process will be inhomogeneous in the depth direction. When a material is added dropwise or in batches to the reactor, it takes a period of time for the material to be mixed evenly with the reaction system under stirring. This period of time will gradually increase as the scale of the reaction is enlarged. Before the material is mixed evenly, it will be too concentrated locally. The longer this time is, the greater the degree of side reactions will be. In the process of dropping or adding materials in batches, there will be a huge difference in reaction time between the first batch of materials added and the last batch of materials added. This difference will gradually increase as the scale of the kettle reaction is enlarged. The products, intermediates and transition states produced by the reaction will have more significant side reactions as the time is longer. Continuous microchannel reaction is to mix the reaction materials instantly at appropriate temperature and pressure, the contact time between the materials is uniform, the retention time of the materials under the reaction conditions is consistent, and the occurrence of side reactions is effectively controlled, thereby improving the reaction conversion rate and yield, reducing the difficulty of reaction purification, and improving economic benefits.

[0006] Microchannel reactions are carried out continuously, and materials are transported by pumps, which is easy to automate, reduce labor intensity, and reduce the risk of occupational injuries. Continuous reactions are carried out in the channel, with fewer material exposure links, which reduces environmental pollution. Therefore, microchannel reactions have very obvious advantages in terms of safety, environmental protection, labor intensity, and economic benefits.

[0007] In recent years, the concept of microchannel reaction has been increasingly valued by manufacturers in various application fields, and microchannel reactors of different brands and forms have appeared on the market. Corning's heart-shaped flow channel reactor, Micro-Kai's tubular reactor, and Chemtrix's Z-shaped flow channel reactor have all been successfully applied in different fields. Some commercial products have also appeared in the domestic market.

[0008] However, all these products have the following problems: 1. Professionals are required to operate the equipment for use and installation, and the flexibility of the equipment is not high. Many reactors are designed as a whole, with fixed forms and flow channel lengths. They are installed once to form a set of equipment. Professionals are required to come to the site for adjustment, which greatly limits the freedom of research and development personnel or engineering and technical personnel. 2. Almost all microreactors focus on the reaction channel itself as the design and development focus, ignoring the coordination between the basic reaction parameters such as material preparation, transportation, and condition control, as well as these conditions. Simply put, the reaction channel is only a part of the continuous reaction. Only a balanced configuration from the material input to the output, including pumping, temperature control, software, etc., is an ideal reactor. 3. Different use environments have different requirements for the flow channel of the reaction. The commercial instruments currently on sale overemphasize the importance of the flow channel form. Some reactions have high requirements for heat transfer, some reactions have high requirements for mass transfer, and some reactions require the input or output of granular materials. It is not a flow channel that can be fully solved. A single flow channel design will affect the flexibility of use. 4. The price of the instrument is very high. In order to find a material that can fully solve the material environment, some extreme materials must be used in material selection. These materials are often expensive and the processing technology is also very complicated, so the price is very expensive, which leads to the high price of the instrument. 5. Due to the inflexible use and high price, the concept of microchannel reaction is difficult to popularize in the application field. For this reason, it is difficult to accumulate and inherit the experience of use in the application field, which further restricts the popularization of instruments and concepts. The development and use of instruments and equipment are far from entering an era of virtuous cycle. The microchannel continuous reaction instrument with such advantages has failed to play its due value in scientific research and production. The market is calling for a product that is low-priced, easy to use, flexible, rich in functions, and low in maintenance and use costs. There is an urgent need for such a product to fill the gap in the market. Summary of the invention

[0009] The technical problem to be solved by the present invention is to provide a comprehensive reaction device platform integrating flow reaction, fixed bed reaction and chromatography functions, so as to solve the defects existing in the prior art.

[0010] The technical solution of the present invention to solve the above technical problems is as follows:

[0011] A comprehensive reaction device platform integrating flow reaction, fixed bed reaction and chromatography functions, comprising a touch LCD screen connected to a PLC, the PLC is also connected to a heating system, a refrigeration system, a delivery pump and an ultrasonic transducer respectively, the delivery pump is provided with a plurality of them, respectively used to deliver different reaction materials, each of the delivery pumps is connected to the heating system and the refrigeration system through a separate pipeline, the heating system and the refrigeration system are respectively provided with ultrasonic transducers, the heating system and the refrigeration system are connected through a reaction channel connecting pipe; the heating system comprises an oil bath box filled with heat exchange bath liquid, a reaction plate is arranged in the oil bath box, the reaction plate comprises a plurality of plate reactor plates arranged side by side, and the plate reactor plates are connected through a reaction pipeline; the oil bath box of the heating system is connected to a heating rod; the refrigeration system comprises an oil bath box filled with heat exchange bath liquid, a reaction plate is arranged in the oil bath box The reaction plate comprises a plurality of plate reactor plates arranged side by side, the plate reactor plates are connected by reaction pipelines, and the reaction pipelines are fixed by pipeline brackets; the oil bath box of the heating system is connected to a refrigeration unit connected to a compressor through a cooling coil; the delivery pump also comprises two pump bodies connected to the chromatography column, the pump bodies enter the chromatography column after passing through a mixer, one of the pump bodies delivers solvent to wet the chromatography column filler and exhaust air, and the other pump body delivers the material or solution to be separated, and then selects different proportions of elution solvents through a touch LCD screen, and delivers them to the chromatography column under the control of a PLC; the whole device is powered by a low-voltage power supply; the PLC is also connected to an emergency stop button; the ultrasonic transducer can achieve the required irradiation power per unit volume of the reaction liquid by adjusting the circulation speed and ultrasonic power in the circulation reaction, and the air explosion effect of the ultrasonic wave can accelerate the progress of the chemical reaction;

[0012] Furthermore, the chromatography column can be arranged in multiple stages, with a relay pump arranged between every two chromatography columns; each chromatography column is fixed by a chromatography column bracket;

[0013] Furthermore, a stirring motor and a cross-flow agitator are provided in the oil bath boxes of the heating system and the refrigeration system, the stirring motor drives the stirring conveyor belt to rotate, and then drives the cross-flow agitator to stir, and the stirring motor is started and shut down by a motor controller controlled by a PLC;

[0014] Furthermore, a compressor and a cooling fan are provided below the heating system and the cooling system, and the compressor and the cooling fan are connected to the PLC. When the temperature reaches a set value, the PLC controls the compressor and the cooling fan to work to cool down the heating system and the cooling system.

[0015] Furthermore, the delivery pump is connected to the material delivery port through a pump head, and the delivery pump is powered by a motor;

[0016] Furthermore, the top of the reaction plate is provided with a reaction plate cover, and the top of the oil bath box is provided with a box cover to keep the device sealed;

[0017] The beneficial effects of the present invention are as follows: an intelligent control module, a pumping system, a temperature control and oil bath system, and an ultrasonic module reaction channel are integrated into a set of instruments; reaction channels of different materials and forms are configured; ultrasound is used to mix the reaction liquid in the channel; and functions such as flow reaction, fixed bed reaction, and chromatography are integrated together. With the support of additional modules, the functions of light reaction, microwave reaction, and electrochemical reaction can be expanded; function switching, reaction channel switching, and channel extension are very easy and convenient to operate; the reaction channel has a simple structure and rich forms and materials to meet the requirements of different usage environments. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] Figure 1 It is a front view structural schematic diagram of the present invention;

[0019] Figure 2 It is a schematic diagram of the top view structure of the present invention;

[0020] Figure 3 Schematic diagram of the installation of the reaction plate in the oil bath of the present invention Figure 1 ;

[0021] Figure 4 Schematic diagram of the pipeline reaction module of the present invention Figure 2 ;

[0022] Figure 5 It is a schematic diagram of a plate type reactor of the present invention;

[0023] Figure 6 It is a schematic diagram of the control system principle of the present invention;

[0024] Figure 7 It is a schematic diagram of the reaction principle of the present invention;

[0025] Figure 8 It is a schematic diagram of the chromatography function principle of the present invention;

[0026] The following are the descriptions of the reference numerals:

[0027] 1. Emergency stop button, 2. Touch LCD screen, 3. Pump head, 4. Stirring synchronous conveyor belt, 5. Stirring motor, 6. Cross-flow agitator, 7. Compressor, 8. Refrigeration unit, 9. Chromatography column bracket, 10. Chromatography column, 11. Reaction channel connecting pipe, 12. Oil bath box, 13. Reaction plate, 14. Heating rod, 15. Ultrasonic transducer, 16. Radiator, 17. Cooling fan, 18. PLC, 19. Low-voltage power supply, 20. Motor controller, 21. Motor, 22. Material conveying port, 23. Cooling coil, 24. Heat exchange bath liquid, 25. Reaction plate cover, 26. Reaction pipeline, 27. Pipeline bracket, 28. Plate reactor plate, 29. Box cover; DETAILED DESCRIPTION

[0028] The principles and features of the present invention are described below in conjunction with the accompanying drawings. The examples given are only used to explain the present invention and are not used to limit the scope of the present invention.

[0029] like Figure 1 As shown, a comprehensive reaction device platform integrating flow reaction, fixed bed reaction and chromatography functions includes a touch LCD screen 2 connected to a PLC 18, the PLC 18 is also connected to a heating system, a refrigeration system, a delivery pump and an ultrasonic transducer 15 respectively, the delivery pump is provided with a plurality of them, respectively used to deliver different reaction materials, each of the delivery pumps is connected to the heating system and the refrigeration system through a separate pipeline, the heating system and the refrigeration system are respectively provided with an ultrasonic transducer 15, and the heating system and the refrigeration system are connected through a reaction channel connecting pipe 11;

[0030] The heating system comprises an oil bath box 12 filled with a heat exchange bath liquid, a reaction plate 13 is arranged in the oil bath box 12, and the reaction plate 13 comprises a plurality of plate reactor plates 28 arranged side by side, and the plate reactor plates 28 are connected through a reaction pipeline 26; the oil bath box 12 of the heating system is connected to a heating rod 14;

[0031] The refrigeration system includes an oil bath box 12 filled with a heat exchange bath liquid, a reaction plate 13 is arranged in the oil bath box 12, and the reaction plate 13 includes a plurality of plate reactor plates 28 arranged side by side, and the plate reactor plates 28 are connected through a reaction pipeline 26, and the reaction pipeline 26 is fixed by a pipeline bracket 27; the oil bath box 12 of the heating system is connected to a refrigeration unit 8 connected to a compressor 7 through a cooling coil 23;

[0032] The delivery pump also includes two pump bodies connected to the chromatography column 10. The pump bodies enter the chromatography column 10 after passing through the mixer. One pump body delivers solvent to wet the chromatography column filler and exhaust air. The other pump body delivers the material or solution to be separated. Then, different proportions of elution solvents are selected through the touch LCD screen 2 and delivered to the chromatography column 10 under the control of PLC18.

[0033] The entire device is powered by a low voltage power supply 19; the PLC 18 is also connected to the emergency stop button 1;

[0034] More specifically, the chromatography column 10 can be arranged in multiple stages, with a relay pump arranged between every two chromatography columns; each chromatography column 10 is fixed by a chromatography column support 9;

[0035] More specifically, a stirring motor 5 and a cross-flow stirrer 6 are provided in the oil bath box 12 of the heating system and the refrigeration system. The stirring motor 5 drives the stirring conveyor belt 4 to rotate, and then drives the cross-flow stirrer 6 to stir. The stirring motor 5 is started and shut down by a motor controller 20 controlled by a PLC 18;

[0036] More specifically, a compressor 7, a radiator 16, and a cooling fan 17 are provided below the heating system and the cooling system. The compressor 7 and the cooling fan 17 are connected to the PLC 18. When the temperature reaches the set value, the PLC 18 controls the compressor 7 and the cooling fan 17 to work to cool down the heating system and the cooling system.

[0037] More specifically, the delivery pump is connected to the material delivery port 22 through the pump head 3, and the delivery pump is powered by the motor 21;

[0038] More specifically, the top of the reaction plate 13 has a reaction plate cover 25, and the top of the oil bath box 12 has a box cover 29 to keep the device sealed;

[0039] Specific working principle:

[0040] The instrument is equipped with two bath boxes, one of which is equipped with a heating device to provide reaction conditions above room temperature; the other is a refrigeration unit installed at the bottom of the instrument, which cools the coolant through the coil in the box to provide reaction conditions below room temperature. The reaction plate is immersed in the bath to achieve the best heat exchange conditions. The reaction plate can be selected from pipeline reactors and plate microchannel reactors, which have the same appearance and size and are easy to replace. The reaction plate can be made of PFA, polytetrafluoroethylene, stainless steel, Hastelloy, monel alloy and other inert metals.

[0041] Ultrasonic chemistry is an interdisciplinary subject that is seriously neglected in the application field. The strong shearing effect of ultrasound on liquid enables the mass transfer of materials to be carried out at the micrometer scale, which cannot be surpassed by any flow channel design and mechanical stirring. The air explosion effect produced by ultrasound inside the liquid produces ultra-high temperature and ultra-high pressure locally, which can accelerate many chemical reactions, even up to hundreds of times. During solid-liquid reactions, solid materials can be crushed and peeled off from the surface to increase the contact with fresh surfaces, especially reactions involving metals, such as Grignard reaction and zinc reagent reaction, breaking through the concept that batch reactions need to be triggered. At present, there are few devices that can be used for ultrasonic chemistry, and the use of ultrasound in microchannel reactions has not yet been seen. The use of ultrasound in kettle reactions has a significant amplification effect, because the distribution of ultrasound power will change significantly during the amplification process, while in circulation reactions, the irradiation power per unit volume of reaction liquid can be perfectly unified only by adjusting the circulation speed and ultrasound power.

[0042] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims

1. A comprehensive reaction device platform integrating flow reaction, fixed bed reaction and chromatography functions, characterized in that: It includes a touch LCD screen connected to a PLC, and the PLC is also connected to a heating system, a refrigeration system, a delivery pump and an ultrasonic transducer respectively. The delivery pumps are provided in plurality and are used to deliver different reaction materials respectively. Each of the delivery pumps is connected to a reaction plate controlled by a heating system and a refrigeration system through a separate pipeline. The heating system and the refrigeration system are respectively provided with ultrasonic transducers, and the heating system and the refrigeration system are connected through a reaction channel connecting pipe; the heating system includes an oil bath box filled with a heat exchange bath liquid, a reaction plate is provided in the oil bath box, and the reaction plate includes a plurality of plate reactor plates arranged side by side, and the plate reactor plates are connected through a reaction pipeline; the oil bath box of the heating system is connected to a heating rod; the refrigeration system includes an oil bath box filled with a heat exchange bath liquid, a reaction plate is provided in the oil bath box, and the reaction plate includes The invention comprises a plurality of plate reactor plates arranged side by side, wherein the plate reactor plates are connected to each other through reaction pipelines, and the reaction pipelines are fixed by pipeline brackets; the oil bath box of the heating system is connected to a refrigeration unit connected to a compressor through a cooling coil; the delivery pump also comprises two pump bodies connected to the chromatography column, and the pump bodies enter the chromatography column after passing through a mixer, wherein one pump body delivers a solvent for wetting the chromatography column filler and exhausting air, and the other pump body delivers a material or solution to be separated, and then selects elution solvents of different proportions through a touch LCD screen, and delivers them to the chromatography column under the control of a PLC; the whole device is powered by a low-voltage power supply, and the PLC is also connected to an emergency stop button, and the ultrasonic transducer can achieve the required irradiation power per unit volume of the reaction liquid by adjusting the circulation speed and ultrasonic power during the circulation reaction, and the air explosion effect of the ultrasonic wave can accelerate the progress of the chemical reaction.

2. A comprehensive reaction device platform integrating flow reaction, fixed bed reaction and chromatography functions according to claim 1, characterized in that: The chromatography columns are arranged in multiple stages, and a relay pump is arranged between every two chromatography columns; and each chromatography column is fixed by a chromatography column bracket.

3. A comprehensive reaction device platform integrating flow reaction, fixed bed reaction and chromatography functions according to claim 2, characterized in that: The oil bath boxes of the heating system and the refrigeration system are both provided with a stirring motor and a cross-flow agitator. The stirring motor drives the stirring conveyor belt to rotate, and then drives the cross-flow agitator to stir. The stirring motor is started and shut down by a motor controller controlled by a PLC.

4. The comprehensive reaction device platform integrating flow reaction, fixed bed reaction and chromatography functions according to claim 3, characterized in that: A compressor and a cooling fan are arranged below the heating system and the cooling system. The compressor and the cooling fan are connected to the PLC. When the temperature reaches a set value, the PLC controls the compressor and the cooling fan to work to cool down the heating system and the cooling system.

5. The comprehensive reaction device platform integrating flow reaction, fixed bed reaction and chromatography functions according to claim 4, characterized in that: The delivery pump is connected with the material delivery port through a pump head, and the delivery pump is powered by a motor.

6. The comprehensive reaction device platform integrating flow reaction, fixed bed reaction and chromatography functions according to claim 5, characterized in that: The top of the reaction plate is provided with a reaction plate cover, and the top of the oil bath box is provided with a box cover to keep the device sealed.

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