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CN-121978027-A - Microreactor based on quartz capillary and application method thereof

CN121978027ACN 121978027 ACN121978027 ACN 121978027ACN-121978027-A

Abstract

The invention relates to the technical field of microreactors and discloses a microreactor based on a quartz capillary and a use method thereof, the microreactor comprises a device body with mounting frames arranged at two sides, quartz capillaries are arranged in through holes uniformly arranged in the device body, each quartz capillary comprises a reaction section and a separation section, a first microinjection pump and a second microinjection pump are respectively arranged at two sides of the device body, and the output ends of the first microinjection pump and the second microinjection pump are respectively connected with a first liquid feeding pipe and a second liquid feeding pipe. The invention utilizes excellent light transmittance of the quartz capillary, directly integrates a micro spectrum detection window in a reaction section, can track the change of absorbance, fluorescence and the like of a substance in the reaction process in real time, solves the problems of difficult observation and data lag of the reaction in the traditional microreactor, ensures more accurate capture of reaction dynamics data, and provides reliable data support for optimization of the reaction process.

Inventors

  • YANG JINGHUA
  • GU YUXIANG

Assignees

  • 南京鑫恩基因科技有限公司

Dates

Publication Date
20260505
Application Date
20251211

Claims (10)

  1. 1. A micro-reactor based on quartz capillaries and a use method thereof comprise a reactor body (1) with mounting frames (20) arranged at two sides, and are characterized in that quartz capillaries (12) are arranged in through holes (5) uniformly arranged in the reactor body (1), each quartz capillary (12) comprises a reaction section (30) and a separation section (31), slotted holes (10) are uniformly arranged in the reactor body (1) between adjacent quartz capillaries (12), a supporting plate (6) and a packaging top plate (4) are sequentially arranged at the top of the reactor body (1), a bearing frame (18) extending to the inside of the slotted holes (10) is uniformly arranged at the bottom of the supporting plate (6), and UV (ultraviolet) lamps (29) are arranged in the bearing frame (18); The two sides of the device body (1) are respectively provided with a first micro injection pump (2) and a second micro injection pump (9), the output ends of the first micro injection pump (2) and the second micro injection pump (9) are respectively connected with a first liquid delivery pipe (3) and a second liquid delivery pipe (7), the inner sides of the first liquid delivery pipe (3) and the second liquid delivery pipe (7) are respectively provided with a first shunt pipe (26) and a second shunt pipe (24) in parallel, and the first shunt pipe (26) and the second shunt pipe (24) are respectively provided with a first branch pipe (27) and a second branch pipe (23) corresponding to each quartz capillary (12); The bottom of the device body (1) is provided with a discharging pipe (15) through a collecting cover (13), and a spiral discharging slurry (14) is arranged in the discharging pipe (15).
  2. 2. A microreactor based on quartz capillary and its application method as claimed in claim 1, characterized in that the slot (10) and the through hole (5) are connected through a communication port (43), and a spectrum detector (8) is arranged in the communication port (43).
  3. 3. The quartz capillary-based microreactor and the use method thereof as claimed in claim 1, wherein spiral micro-grooves (34) are formed in the inner wall of the reaction section (30) of the quartz capillary (12), and array micro-protrusions (33) are uniformly formed in the inner wall of the reaction section (30) between two adjacent spiral micro-grooves (34).
  4. 4. The quartz capillary-based microreactor and a use method thereof according to claim 1, wherein a separation hole (32) is formed in the side wall of a separation section (31) of the quartz capillary tube (12), a permeable membrane (37) is arranged outside the separation hole (32), cavities (16) are formed in the outer side of the permeable membrane (37) and in the inner side of a reactor body (1), and each cavity (16) is connected with a negative pressure main pipe (21) arranged on the outer wall of the reactor body (1) through an exhaust pipe (36).
  5. 5. The quartz capillary-based microreactor and a use method thereof as claimed in claim 1 or 4, wherein the two sides of the reactor body (1) are provided with a negative pressure box (11) consisting of an upper shell (38), a lower shell (39) and an air suction fan (35), the air suction fan (35) is arranged on the inner side of the upper shell (38), the input end of the upper shell (38) is connected with the output end of a negative pressure main pipe (21), and the bottom of the lower shell (39) is provided with an output pipe connected with external equipment.
  6. 6. The quartz capillary based microreactor and the use method thereof according to claim 1, wherein round holes (17) for the top ends of the quartz capillaries (12) to pass through are uniformly distributed on the supporting plate (6), the packaging top plate (4) is provided with packaging end covers (25) at positions corresponding to the openings of the quartz capillaries (12), and the branch pipes (27) and the branch pipes (23) penetrate through the packaging end covers (25) in pairs and extend into the quartz capillaries (12).
  7. 7. A microreactor based on quartz capillary tubes and a use method thereof as claimed in claim 1, wherein the surface of the carrier (18) is uniformly distributed with light transmission openings (28), and a protective net (19) is arranged in each light transmission opening (28).
  8. 8. The quartz capillary-based microreactor and a use method thereof as claimed in claim 1, wherein one end of the discharge pipe (15) is provided with a servo motor (22), the output end of the servo motor (22) is connected with a spiral discharge slurry (14), and the other end of the discharge pipe (15) is provided with a discharge hole.
  9. 9. A micro-reactor based on quartz capillary and its application method as set forth in claim 1, wherein the first and second shunt tubes (26, 24) and the first and second liquid feeding tubes (3, 7) between the first and second micro-injection pumps (2, 9) are respectively provided with a first precise flow valve (40) and a second precise flow valve (41).
  10. 10. A quartz capillary based microreactor and method of use according to claim 1, characterized in that the method comprises the steps of: s1, injecting raw materials through a first liquid feeding pipe (3) and a second liquid feeding pipe (7) of a first micro injection pump (2) and a second micro injection pump (9), and matching set flow rates by adjusting a first precise flow valve (40) and a second precise flow valve (41); S2, enabling raw materials to generate local vortex by means of spiral micro grooves (34) and array type micro protrusions (33) on the inner wall of a quartz capillary tube (12) through a reaction section (30) of the quartz capillary tube, breaking a laminar boundary layer, and realizing rapid mixing and starting reaction; S3, enabling the reaction liquid to enter a separation section (31) of a quartz capillary tube (12), opening a vacuum extraction opening at the outer side of the separation section, and enabling small molecule byproducts generated by the reaction to be extracted through a permeable membrane so as to push the reaction to proceed forward; s4, enabling the reacted material to enter a discharge pipe (15) through a collecting cover (13), driving a spiral discharge slurry (14) through a servo motor (22), and guiding and collecting the product from a discharge hole.

Description

Microreactor based on quartz capillary and application method thereof Technical Field The invention relates to the technical field of microreactors, in particular to a microreactor based on a quartz capillary tube and a use method thereof. Background The microreactor is used as a novel reaction device, and has been widely applied to the fields of organic synthesis, drug research and development, environmental management and the like by virtue of the advantages of high mass transfer and heat transfer efficiency, small reagent consumption, easy control of reaction conditions and the like. Along with the continuous improvement of the precision of the reaction process, the purity of the product and the integration requirement of the process in the fine chemical industry and the biological medicine industry, the traditional microreactor gradually exposes a plurality of technical limitations, and is difficult to meet the application requirements of high efficiency and multifunction. The existing microreactors generally have the problem of lag in monitoring the reaction process. Most microreactors rely on offline sampling analysis to obtain reaction data, and the concentration change of substances in a reaction system cannot be tracked in real time, so that the reaction kinetic parameters are inaccurate to capture, the reaction conditions are difficult to adjust in time, and the fluctuation of the yield of a target product or the increase of byproducts are easily caused. Even if part of the microreactors try to integrate the monitoring function, the spectral signal attenuation is serious due to poor light transmittance of the materials of the reaction channels or unreasonable design of the monitoring window, so that the monitoring precision is difficult to guarantee. In terms of mass transfer efficiency and reaction-separation integration, conventional microreactors also have significantly shorter plates. On one hand, the inner wall of the reaction channel of the existing microreactor is mostly of a smooth structure, the reaction fluid is easy to form stable laminar flow in the channel, the laminar boundary layer is thick, the mass transfer resistance between liquid-liquid and gas-liquid is large, the reaction rate is obviously limited, the expected conversion rate can be achieved only by prolonging the reaction time especially for mass transfer control type reaction, on the other hand, the existing microreactor is mostly provided with a single reaction function, byproducts generated by the reaction are required to be removed by depending on subsequent independent separation equipment, the equipment investment and the operation complexity are increased, the product loss is possibly caused by the intermediate transfer process, and the overall process efficiency is reduced. In addition, the micro-reactor related to the photocatalytic reaction also faces the problem of insufficient uniformity of illumination. Most of light sources of the existing photocatalysis microreactors are external or locally fixed, illumination is difficult to uniformly cover the whole reaction area, partial area reaction in a reaction channel is incomplete, reaction dead angles appear, and the reaction efficiency and the product uniformity are further affected. Meanwhile, the feeding system of the existing microreactor also has the problem of insufficient flow control precision, and the material proportion deviation is easily caused by flow fluctuation when a plurality of reaction raw materials are fed, so that the reaction stability is damaged, and the repeatability of an experiment result is reduced. In a multi-channel parallel reaction scene, the structural design of the traditional microreactor also has the defect of poor consistency among channels. When the multi-channel layout is adopted, the material distribution of each reaction channel is uneven, the temperature/illumination condition difference is large, the reaction processes of different channels are easy to be asynchronous, the large-scale and standardized reaction operation is difficult to realize, and the application of the microreactor in a batch synthesis scene is limited. In summary, the technical limitations of the current microreactor in the aspects of real-time monitoring, mass transfer efficiency, reaction-separation integration, illumination uniformity, flow control precision and the like have become key bottlenecks for restricting the development of the microreactor to high efficiency, multifunction and integration. Therefore, developing a microreactor with real-time accurate monitoring, efficient mass transfer, reaction-separation integration, uniform illumination and accurate flow control becomes a technical problem to be solved in the field. Disclosure of Invention This section is intended to outline some aspects of embodiments of the application and to briefly introduce some preferred embodiments. Some simplifications or omissions may be made in this section as wel