Liquid phase automated synthesis device
The liquid phase automated synthesizer addresses inefficiencies and safety concerns in current liquid phase experiments by automating sample loading, temperature control, light irradiation, and monitoring through a centralized computer system, thereby enhancing experimental accuracy and efficiency.
Patent Information
- Application Number
- JP2023535356
- Authority / Receiving Office
- JP · JP
- Patent Type
- Patents
- Current Assignee / Owner
- Priority Date
- 2020-12-19
- Filing Date
- 2021-12-18
- Publication Date
- 2025-04-10
- Estimated Expiration
- 2041-12-18
AI Technical Summary
Current liquid phase experiments require manual intervention for sample loading, stirring, temperature control, and light irradiation, leading to inefficiencies and safety concerns, such as the risk of fire from improper mercury lamp usage.
A liquid phase automated synthesizer is developed, incorporating an automatic sample loading system, a liquid phase synthesis auxiliary system for temperature and light control, and an online automatic monitoring system, all connected to a master computer for centralized control and data analysis.
The automated system significantly reduces manual effort and time, enhances experimental accuracy and safety, and improves the overall efficiency of liquid phase synthesis experiments by automating key processes.
Smart Images

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Abstract
Description
[Technical field]
[0001] The present invention relates to the technical field of laboratory equipment, in particular to automated liquid phase synthesis equipment. [Background technology]
[0002] Liquid phase experiments are an essential part of academic research. Current liquid phase experiments require quantitative addition of reactants and dissolutions, and the mixed solution is obtained by manually controlling the stirring reaction. During the process of detecting the mixed solution, the reactant needs to be manually added to the monitor, and the monitoring report created by the monitor needs to be manually sorted and checked, which makes the liquid phase experiment and monitoring process time-consuming and laborious.
[0003] Based on this, some automatic sample loading devices have been provided in the prior art, and their sample loading means mainly include the following two types: (1) Pipeline transfer sample loading: Currently, peptide solid-phase synthesizers, oligosaccharide solid-phase synthesizers, automatic solid-phase extractors, etc. are on the market. Its advantages are airtightness, safety, no external interference, and strong systematization, and its disadvantages are the long research and development cycle and the high design and development costs of a single finished product. It is designed in the following two ways: 1. The components are purchased and assembled, and can be flexibly adjusted and changed, making it easier to integrate programs (syringe pump units, multi-channel switching valves, light sources, low-temperature circulation, magnetic stirring, and other online monitoring), but there are many factors that affect the operation results after assembly, such as the need for redesign, the long cycle, and the need for talent in all aspects. 2. Conversion and upgrade from similar products on the market, that is, the appropriate modification of mature automation products has a short cycle, does not require much effort, and ensures normal operation. However, mature products have mature software control systems developed by independent patents, so the program integration is cumbersome, there is no source code, and the integrated circuit chip may need to be redesigned. (2) As for automatic pipetting and sample loading, there are many mature automatic liquid pipetting workstations on the market. There are several versions (priced between 100,000 and 400,000 yuan) that can be purchased directly and modified slightly. Its advantages are simple and fast, and can directly fix manual operations to the equipment. The disadvantages are that all operations need to be replaced by mechanical arms, which results in high failure rates, long-term prospects, and also mature products, and the integration of programs is inconvenient.
[0004] In addition, in the liquid phase experiment process, temperature control and light irradiation control are also important parts of the experiment. In the existing experimental liquid phase synthesis process, a common two-port quartz reactor is often used, and the experiment is carried out in a -80℃ low temperature bath with side irradiation. In the side irradiation process, a long-arc mercury lamp light source and a quartz cold trap are generally used as the light source device, and the light source device needs to be equipped with a low-temperature circulation device that is combined with the quartz cold trap so that the circulation temperature (-20℃, the mercury lamp cannot be started at a temperature that is too low) is higher than the temperature of the low temperature bath (-80℃), so it is difficult to accurately control the temperature of the low temperature bath. Furthermore, the low-temperature circulation device is set up separately and needs to be turned on just before the mercury lamp is turned on. If the mercury lamp is turned on while forgetting to turn on the low-temperature circulation device of the cold trap, the mercury lamp will be turned on and irradiated for a long time, which will cause a very high risk of fire.
[0005] In order to solve the above problems, the irradiation method uses a long-arc mercury lamp light source and a cold trap made of quartz material, but the cold trap is placed horizontally, the ultraviolet light is irradiated from top to bottom onto the reactor, and the reactor is placed in a low-temperature bath Dewar bottle of ethanol / dry ice. According to this method, the temperature is easy to control and stable, and the model reaction synthesis effect is consistent with the previous laboratory side illumination method and tends to be slightly better, but there is still a need to start an additional low-temperature circulation device for the cold trap while cooling it, the equipment is not easy to assemble, it is not safe, the utilization rate of ultraviolet light is very low, and an additional ultraviolet protection device is also required.
[0006] Therefore, providing a highly efficient and highly accurate automated liquid phase synthesis device that can realize the automation of liquid phase experiments is a technical challenge that must be solved as soon as possible in this field. Summary of the Invention [Problem to be solved by the invention]
[0007] An object of the present invention is to provide an automated liquid phase synthesis device for realizing automation of liquid phase synthesis experiments and further improving the efficiency and accuracy of high-speed liquid phase synthesis experiments. [Means for solving the problem]
[0008] In order to achieve the above object, the present invention provides the following aspects.
[0009] Automatic sample loading system, liquid phase synthesis auxiliary system, liquid phase synthesis online automatic monitoring system, and master computer and a reactor Including, The automatic sample loading system, the liquid phase synthesis auxiliary system, and the liquid phase synthesis online automatic monitoring system are all electrically connected to the master computer; The automatic sample loading system completes an automatic sample loading operation according to a sample loading command from the master computer. By this, the liquid-phase synthesized sample is sucked into the automatic monitoring system. The liquid phase synthesis auxiliary system is configured to control the temperature and light irradiation in accordance with a temperature control command and a light irradiation control command from the master computer. , Liquid phase synthesis The automatic monitoring system is for completing the temperature and light irradiation control of the reaction solution, The aspirated sample is used as a first reaction solution. and generating a monitoring report, and the master computer is for generating an experimental analysis result according to the monitoring report. the law of nature, The reactor includes a bottle mouth, a bottle body, a sample loading port, an exhaust port, a sampling port, a circulating liquid exhaust port, and a circulating liquid inlet, The centerline of the sampling port forms a set angle with respect to the longitudinal centerline of the bottle body. A liquid phase automated synthesis apparatus comprising:
[0010] Preferably ,before The reactor comprises: Each one is different The automatic sample loading system, the liquid phase synthesis auxiliary system, and the liquid phase synthesis online automatic monitoring system are each connected via a first pipeline.
[0011] Preferably ,beforeThe center line of the exhaust port is perpendicular to the center line of the bottle mouth, The bottle body includes a reaction liner from the inside to the outside. Low temperature circulating fluid a vacuum layer, and a bottom of the reaction liner is an arc-shaped structure; The sampling port is connected to the reaction liner, The circulating fluid outlet and the circulating fluid inlet are both Low temperature circulating fluid The circulating liquid outlet and the circulating liquid inlet are diagonally arranged. R .
[0012] Preferably, the automatic sample loading system includes an inert gas supply module, a sampling channel switching module, a quantification module, a treatment module, and a liquid storage module; The liquid storage module and the sampling channel switching module are both Second The quantitative module is connected to the inert gas supply module through a pipeline, and the quantitative module is Third The liquid storage module is connected to the sampling channel switching module and the treatment module via a pipeline, respectively. Fourth connected to the sampling channel switching module via a conduit; The inert gas supply module, the sampling channel switching module, and the quantitative measurement module are all electrically connected to the master computer; The inert gas supply module supplies the inert gas stored therein Second The liquid storage module and the sampling channel switching module are respectively supplied through a pipeline, the sampling channel switching module is for extracting the reaction waiting solution stored in the liquid storage module and switching the channel for extracting the reaction waiting solution, and the quantitative determination module is for determining the amount of the reaction waiting solution in the treatment module; The master computer is for controlling the on-off of the inert gas supply module and the quantitative measurement module, and for controlling the channel switching of the sampling channel switching module.
[0013] Preferably, the sampling channel switching module includes a first multi-channel switching valve and a second multi-channel switching valve; The first multichannel switching valve is configured to supply M Liquid Storage Bottle and the second multichannel switching valve is connected to NM liquid storage bottles through a sixth line, where M is the number of liquid storage bottles connected to the first multichannel switching valve, and N is the number of liquid storage bottles connected to the first multichannel switching valve. bottle NM is the difference between N and M liquid storage bottles, The metering module includes a syringe pump unit, a pressure sensor, a flow meter, and a second solenoid valve unit; The inlet of the syringe pump unit is connected to the sampling channel switching module via a seventh pipeline, the outlet of the syringe pump unit is connected to the flow meter via an eighth pipeline, and the flow meter is connected to the treatment module via a ninth pipeline, the second solenoid valve unit is installed in the eighth pipeline connecting the flow meter and the treatment module, the pressure sensor is installed in the pipeline connecting the syringe pump unit and the flow meter, and the second solenoid valve unit, the pressure sensor, and the flow meter are all electrically connected to the master computer; The treatment module includes a solution tube and a waste bottle; The sampling port of the reactor and the liquid inlet of the waste liquid bottle are both Each one is different a first solenoid valve unit connected to the second solenoid valve unit through a tenth line, and the solution tube connected to an exhaust port of the reactor through an eleventh line; The second solenoid valve unit is for closing a twelfth pipe connected between the flow meter and the reactor and opening a thirteenth pipe connected between the flow meter and the waste liquid bottle when the solution in the reactor reaches a certain amount.
[0014] Preferably, the syringe pump unit includes a first syringe pump and a second syringe pump, The first syringe pump is connected to one of the first multichannel switching valves via a fourteenth pipe. t The second syringe pump is connected to a channel of the second multichannel switching valve via a 15th conduit. t of the first syringe pump connected to the channel of flow rate of the second syringe pump flow rate will be smaller than
[0015] Preferably, the liquid phase synthesis auxiliary system includes a mixing device and a temperature control device; The above Reactor is installed in the mixing device, and the mixing device and the temperature control device are both electrically connected to the master computer.
[0016] Preferably, the temperature control device includes an ultraviolet light source and a low-temperature circulation device; The drain of the low-temperature circulation device is connected to a 16th pipe The reactor The circulating fluid inlet is connected to the circulating fluid inlet, and the inlet of the low-temperature circulating device is connected to the circulating fluid inlet through a seventeenth pipe. The reactor the ultraviolet light source is connected to the circulating liquid outlet and is for irradiating the reactor; The mixing device includes an automatic stirrer and a thermostatic plate; The automatic stirrer and the thermostatic plate are both electrically connected to the master computer, the automatic stirrer is for stirring the mixed liquid in the reactor in accordance with a stirring command from the master computer, the reactor is placed on the automatic stirrer, and the thermostatic plate is for maintaining the temperature of the reactor constant.
[0017] Preferably, the liquid phase synthesis online automatic monitoring system includes a sampling module, a power module, a monitoring and analysis module, and a cleaning module; The sampling module is connected to the power module via an eighteenth line, and the power module is connected to the monitoring and analysis module via a nineteenth line, and the sampling module, the power module, and the monitoring and analysis module are all electrically connected to the master computer; The sampling module is housed in the reactor. Ta The power module is for sucking a second reaction solution, the power module is for applying a suction force to the sampling module in accordance with a suction command from the master computer, and for injecting the second reaction solution sucked by the sampling module into the monitoring and analysis module to use it as a first reaction solution, the monitoring and analysis module is for generating a monitoring report using the first reaction solution and then transmitting the monitoring report to the master computer, and the master computer calculates an analysis result based on the monitoring report. Generate , The cleaning module is connected to the sampling module and the power module via a twentieth line.
[0018] Preferably, the sampling module includes a stainless steel needle, a slide rail, and a rotating plate; The stainless steel needle is connected to the power module via a first pipeline, the first pipeline is disposed on the slide rail, and the slide rail forms a set angle with respect to a horizontal line, the stainless steel needle is fixedly disposed on one end of the slide rail, and the other end of the slide rail is a free end, the slide rail is for driving and sliding the stainless steel needle, the stainless steel needle is for entering a reactor and sucking in a second reaction solution, and the slide rail is fixedly installed on the rotating plate, The rotating plate and the slide rail are both electrically connected to the master computer; the power module includes a power pump, the power pump being a syringe pump or a plunger pump; The power pump is connected to the sampling module and the monitoring and analysis module via a 21st line, the monitoring and analysis module is a high performance liquid chromatograph; the cleaning module includes a first liquid container, a second liquid container, and a solenoid valve; The stainless steel needle is for sucking the cleaning liquid in the first liquid container, and the second liquid container, the power module, and the monitoring and analysis module are all Each one is different It is connected to the solenoid valve via a 22nd pipe. Effect of the Invention
[0019] According to the specific embodiments provided by the present invention, the present invention discloses the following technical effects: The liquid phase automated synthesis apparatus provided by the present invention includes an automatic sample loading system, a liquid phase synthesis auxiliary system, and a liquid phase synthesis onlineAn automatic monitoring system and a master computer are installed, the automatic sample loading system completes the automatic sample loading operation in accordance with a sample loading command from the master computer, the liquid phase synthesis auxiliary system completes the temperature and light irradiation control of the solution waiting for reaction in accordance with a temperature control command and a light irradiation control command from the master computer, the automatic monitoring system monitors the reaction solution and creates a monitoring report, and the master computer generates experimental analysis results in accordance with the monitoring report, thereby completing the automation of the process from sample loading to report creation during the liquid phase experiment, further reducing the effort and cost of the experiment and improving the efficiency of the experiment.
[0020] In order to more clearly describe the embodiments of the present invention or the technical aspects in the prior art, the drawings necessary to be used in the embodiments are briefly described below. The drawings below are only some embodiments of the present invention, and it is obvious to those skilled in the art that other drawings can be obtained based on these drawings without paying creative labor. [Brief description of the drawings]
[0021] [Figure 1] FIG. 1 is a schematic diagram of the structure of an automated liquid phase synthesis apparatus provided by the present invention; [Diagram 2] FIG. 2 is a schematic diagram of the structure of the liquid phase automated synthesis apparatus provided by the present invention; [Diagram 3] FIG. 3 is a structural schematic diagram of a reactor provided in an embodiment of the present invention; [Figure 4] FIG. 4 is a structural schematic diagram of an automatic sample loading system provided in an embodiment of the present invention; [Diagram 5] FIG. 5 is a structural schematic diagram of a liquid phase synthesis auxiliary system provided in an embodiment of the present invention; [Figure 6] FIG. 6 is a structural schematic diagram of a liquid phase synthesis online automatic monitoring system provided in an embodiment of the present invention; [Figure 7] FIG. 7 is a diagram of an automated liquid phase synthesis apparatus provided in an embodiment of the present invention. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0022] The following will clearly and completely describe the technical aspects of the embodiments of the present invention in combination with the drawings in the embodiments of the present invention, and it will be clear that the above embodiments are only some of the embodiments of the present invention, but are not all of the embodiments. Any other embodiments obtained by those skilled in the art without creative labor based on the embodiments of the present invention will also fall within the protection scope of the present invention.
[0023] An object of the present invention is to provide an automated liquid phase synthesis device that realizes automation of liquid phase synthesis experiments and further improves the efficiency and accuracy of liquid phase synthesis experiments.
[0024] In order to make the above objects, features and advantages of the present invention more clearly comprehensible, the present invention will be further described in detail below in combination with drawings and specific implementation methods.
[0025] As shown in FIG. 1, the liquid phase automated synthesis apparatus provided by the present invention includes an automatic sample loading system 1, a liquid phase synthesis auxiliary system 2, and a liquid phase synthesis online An automatic monitoring system 3 and a master computer 5 . Automatic sample loading system 1, liquid phase synthesis auxiliary system 2, and liquid phase synthesis Online in Each of the automatic monitoring systems 3 is electrically connected to a master computer 5 .
[0026] The automatic sample loading system 1 is for completing an automatic sample loading operation according to a sample loading command from the master computer 5. The liquid phase synthesis auxiliary system 2 is for completing temperature and light irradiation control of a reaction waiting solution according to a temperature control command and a light irradiation control command from the master computer 5. The automatic monitoring system is for monitoring a reaction solution and creating a monitoring report. The master computer 5 generates an experiment analysis result based on the monitoring report.
[0027] Since the liquid phase automated synthesis apparatus is used during the liquid phase experiment, the equipment needs to stir the solution in the reactor, but the existing reactor is very prone to splashing during the stirring process, and when low temperature experiments are performed, the outer wall of the existing reactor is very prone to generating water vapor, making it impossible to directly observe the reaction solution in the reactor. Therefore, according to the liquid phase automated synthesis apparatus provided by the present invention, the present invention provides a reactor that is compatible with the entire liquid phase automated synthesis apparatus. Reactor 1-41 are provided accordingly. Reactor Of course, 1-41 can also be used in other laboratory equipment, since it has advantages that other existing reactors cannot match.
[0028] The present invention provides Reactor 1-41 is an automatic sample loading system 1, a liquid phase synthesis auxiliary system 2, and a liquid phase synthesis online Each is connected to a pipeline of the automatic monitoring system 3.
[0029] As shown in FIG. Reactor 1-41 includes a bottle mouth 1-411, a sampling port 1-412, an exhaust port 1-413, a sampling port 1-414, a bottle body 1-415, and a circulating fluid exhaust port 1-416.
[0030] The sampling port 1-412 forms a set angle (preferably 60°) with respect to the bottle body 1-415. The exhaust port 1-413 and the sampling port 1-412 are arranged symmetrically around the center line of the bottle mouth 1-411. The center line of the sampling port 1-414 has a spatial angle of 60° with respect to the center line of the exhaust port 1-413, and the setting of this particular angle is to avoid the reaction liquid from splashing out of the reactor during the stirring process.
[0031] The bottle body 1-415 includes, from the inside to the outside, a reaction liner 1-4151, a temperature circulation layer 1-4152, and a vacuum layer 1-4153 in that order. The bottom of the reaction liner 1-4151 has an arc-shaped structure.
[0032] The sampling port 1-414 is connected to a reaction liner 1-4151. The circulating fluid outlet 1-416 and the circulating fluid inlet are both connected to the temperature circulation layer 1-4152, and are disposed diagonally opposite to the circulating fluid outlet 1-416 and the circulating fluid inlet.
[0033] In addition, the bottle mouth 1-411 is provided with a top lid 1-417 or the bottle mouth 1-411 has a sealed structure. The top lid 1-417 provided is preferably a high light transmittance quartz sheet. When the bottle mouth 1-411 is provided with a top lid 1-417, the top lid 1-417 is provided to improve the sealing property. Reactor It is preferable that the bottle 1-41 further includes a sealing clip. The sealing clip is for clamping the bottle mouth 1-411 and the top lid 1-417. The sealing clip has a double jacketed eggplant-shaped structure, specifically, two flange clamps are used, and the shape formed between the two flange clamps is changed from U-shaped to eggplant-shaped.
[0034] As shown in FIG. 4, the automatic sample loading system 1 provided in the present invention includes an inert gas supply module 1-1, a sampling channel switching module 1-2, a quantitative module 1-3, a treatment module 1-4, and a liquid storage module 1-5.
[0035] The liquid storage module 1-5 and the sampling channel switching module 1-2 are both connected to the inert gas supply module 1-1 via pipelines. The quantification module 1-3 is connected to the sampling channel switching module 1-2 and the treatment module 1-4 via pipelines. The liquid storage module 1-5 is connected to the sampling channel switching module 1-2 via pipelines.
[0036] The inert gas supply module 1 - 1 , the sampling channel switching module 1 - 2 , and the quantitative measurement module 1 - 3 are all electrically connected to a master computer 5 .
[0037] The inert gas supply module 1-1 is for supplying the inert gas stored therein to the liquid storage module 1-5 and the sampling channel switching module 1-2 through a pipeline. The sampling channel switching module 1-2 is for extracting the reaction-awaiting solution stored in the liquid storage module 1-5 and for switching the channel for extracting the reaction-awaiting solution. The quantitative measurement module 1-3 is for determining the amount of reaction-awaiting solution to be injected into the treatment module 1-4.
[0038] The master computer 5 is for controlling the on / off of the inert gas supply module 1-1 and the quantitative measurement module 1-3, and for controlling the channel switching of the sampling channel switching module 1-2. Other external devices control the program by controlling a Programmable Logic Controller (PLC) through the master computer 5 via a communication protocol to ensure the normal operation of the automation program.
[0039] Among others, the inert gas supply module 1-1 includes an inert gas reservoir 1-11, a pressure regulating filter 1-12, and a first solenoid valve unit 1-13.
[0040] The inert gas reservoir 1-11 is connected to the liquid storage module 1-5 and the sampling channel switching module 1-2 via pipelines. The pressure adjustment filter 1-12 and the first solenoid valve unit 1-13 are installed in the pipeline connecting the inert gas reservoir 1-11 and the liquid storage module 1-5, or in the pipeline connecting the inert gas reservoir 1-11 and the sampling channel switching module 1-2.
[0041] Among them, the first solenoid valve unit 1-13 includes a first two-way solenoid valve 1-131, a second two-way solenoid valve 1-132, and a three-way solenoid valve 1-133.
[0042] The first two-way solenoid valve 1-131 and the three-way solenoid valve 1-133 are installed in a pipeline connecting the inert gas reservoir 1-11 and the sampling channel switching module 1-2. The second two-way solenoid valve 1-132 is installed in a pipeline connecting the inert gas reservoir 1-11 and the liquid storage module 1-5.
[0043] Preferably, the number of pressure-regulating filters 1-12 is two, and the two pressure-regulating filters 1-12 are installed in the pipeline connecting the inert gas reservoir 1-11 and the sampling channel switching module 1-2, and in the pipeline connecting the inert gas reservoir 1-11 and the liquid storage module 1-5, respectively.
[0044] The liquid storage module 1-5 includes N liquid storage bottles 1-51.
[0045] Each of the liquid storage bottles 1-51 is connected to the inert gas supply module 1-1 via a pipe. The bottom of the liquid storage bottle 1-51 is conical or arc-shaped.
[0046] Each of the liquid storage bottles 1-51 has a first channel port, a second channel port, a third channel port, and a bottle lid.
[0047] The first channel port is for connection to the sampling channel switching module 1-2 via a conduit. The second channel port is for connection to the inert gas supply module 1-1 via a conduit. The third channel port is for discharging the gas or liquid in the liquid storage bottle 1-51.
[0048] The bottle cap and the bottle mouth 1-411 of the liquid storage bottle 1-51 are connected by screwing.
[0049] Since each liquid storage bottle 1-51 is filled with inert gas at a slight positive pressure, negative pressure due to loss of liquid in the sealed liquid storage bottle 1-51 will not occur, and furthermore, the accuracy of sampling will not be affected.
[0050] The liquid storage bottle 1-51 provided in the present invention preferably has four kinds, namely, a 10mL pointed-bottom liquid storage bottle, a 20mL pointed-bottom liquid storage bottle, a 500mL round-bottom liquid storage bottle, and a 125mL two-mouth liquid storage bottle. The 10mL and 20mL pointed-bottom liquid storage bottles are mainly used for storing building block samples and reagent catalysts, and the purpose of the pointed-bottom design is to make the pipes enter the bottle bottom 1-512 to avoid loss and waste of storage liquid, and the female thread design is easy to match with customized polytetrafluoroethylene bottle caps. The 500mL round-bottom liquid storage bottle is mainly used for storing ultra-dry organic solutions, and the 125mL two-mouth bottle is mainly used for storing organic solutions that dilute reaction solutions and thus waste liquids. The side sample loading port 1-412 is mainly used for inserting and removing sampling needles during online monitoring. All liquid storage bottles 1-51 are made of transparent sealed tubular glass material, have pressure resistance, and do not use brown or black colors. The main purpose is to allow users to easily check the remaining amount of stored liquid. As can be seen from the overall structure of the automatic sampling, in the process of research and development of the synthesis equipment, in addition to the most important reactor, light source, automatic sampling and the close integration of the master computer 5 software, there are also customized accessories designed that play auxiliary and fundamental roles, mainly various liquid storage bottles 1-51 and corresponding bottle covers.
[0051] The design of the customized bottle lid matching the customized liquid storage bottle 1-51 has been repeatedly researched, verified and modified. The bottle lid has three channels, which are for ventilation, liquid flow and air release, respectively. In order to ensure the stability of the concentration of the storage liquid and the accuracy of automatic sample loading, the bottle lid needs to be tightly sealed, easy to open and close, corrosion resistance and durability are required. The length of the PTFE bottle lid is increased, an on / off switch is embedded inside the bottle lid, the bottom of the bottle lid is thinned and connected with an inverted cone, which is compacted and sealed without a sealing ring and is firmly connected, and the upper part of the bottle lid is connected with an inverted cone in a triangular arrangement, ensuring the sealing of the connecting pipe line to obtain the first customized bottle lid. After repeated testing, it was found that the on / off switch embedded inside the first bottle lid above had liquid leakage, so a normal elastic seal gasket was also added to the on / off switch location, which is on the outside of the bottle lid and does not need corrosion resistance, that is, a PTFE three-channel compact bottle lid is obtained.
[0052] The sampling channel switching module 1-2 includes a first multi-channel switching valve 1-21 and a second multi-channel switching valve 1-22.
[0053] The first multichannel switching valve 1-21 is connected to M liquid storage bottles 1-51 via pipes, and the second multichannel switching valve 1-22 is connected to NM liquid storage bottles 1-51 via pipes.
[0054] The two 10-channel switching valves can connect liquid storage bottles 1-51 with different specifications in parallel or cross-connection. For ease of use, the 10th channel of the two switching valves is always connected to inert gas, the 9th channel is connected to normal ultra-dry solution (e.g. dichloromethane), the 8th channel is connected to second-choice ultra-dry solution (e.g. acetonitrile, toluene, etc.), and each of the other channels is connected to different or the same storage liquid independently or cross-connected, so that no cross-contamination occurs.
[0055] Generally, according to the needs of the experiment, when the sample loading amount is less than or close to 1 mL, it is connected to the first multi-channel switching valve 1-21, and when it is more than or close to 1 mL, it is connected to the second multi-channel switching valve 1-22, and each channel number of the multi-channel switching valve should correspond one-to-one with the substance in each liquid storage bottle 1-51. The inert gas reservoir 1-11 is sequentially depressurized and filtered through the pressure reducing valve and pressure regulating filter 1-12 for use, which serves the functions of providing positive pressure and cleaning the pipeline.
[0056] The quantitative module 1-3 includes a syringe pump unit 1-31, a pressure sensor 1-32, a flow meter 1-33, and a second solenoid valve unit 1-34.
[0057] The inlet of the syringe pump unit 1-31 is connected to the sampling channel switching module 1-2 via a pipeline. The outlet of the syringe pump unit 1-31 is connected to the flow meter 1-33 via a pipeline. The flow meter 1-33 is connected to the treatment module 1-4 via a pipeline. The second solenoid valve unit 1-34 is installed in the pipeline connecting the flow meter 1-33 and the treatment module 1-4. The pressure sensor 1-32 is installed in the pipeline connecting the syringe pump unit 1-31 and the flow meter 1-33. The second solenoid valve unit 1-34, the pressure sensor 1-32, and the flow meter 1-33 are all electrically connected to the master computer 5.
[0058] The syringe pump unit 1-31 includes a first syringe pump 1-311 and a second syringe pump 1-312.
[0059] The first syringe pump 1-311 is connected to one channel of the first multichannel switching valve 1-21 via a conduit. The second syringe pump 1-312 is connected to one channel of the second multichannel switching valve 1-22 via a conduit. The range of the first syringe pump 1-311 is smaller than the range of the second syringe pump 1-312.
[0060] In order to ensure the accuracy of sample loading, when the sample loading amount of the entire sample loading system provided by the present invention is less than or close to 1 mL, it is injected from the line connected to the syringe pump with a smaller range (i.e., the first syringe pump 1-311). When the sample loading amount is higher than or close to 1 mL, it is injected from the line connected to the syringe pump with a larger range (i.e., the second syringe pump 1-312), and both lines run in parallel at first, and then are integrally connected to enter the reactor. The syringe in the syringe pump is replaceable, with a minimum of 500 μL and a maximum of 25 mL, and can be expanded by increasing the number of switching valves and syringe pumps as modules. Each line is provided with sample loading power by a syringe pump. Each pipeline is synergistically combined and dual-controlled by an independent syringe pump and the subsequent high-precision flowmeter 1-33 to ensure the accuracy of sample loading, and the measurement amount of the flowmeter 1-33 between the syringe pump and the flowmeter 1-33 is the final sample loading amount. The reason for this setting is that, on the one hand, the accuracy of the syringe pump itself (1%) is lower than the accuracy of the flowmeter 1-33 itself (2‰). On the other hand, the syringe pump cannot distinguish the presence or absence of bubbles or liquid, and the measurement difference between gas and liquid of the flowmeter 1-33 is relatively large, and the measurement fluctuation is large when gas passes through, which can be fed back to the dual self-correction of the flowmeter 1-33 and the syringe pump.
[0061] The above-mentioned processing modules 1-4 are: Reactor 1-41, a solution tube 1-42, and a waste bottle 1-43.
[0062] Reactor The sample loading port 1-412 of the sample loading port 1-41 and the liquid inlet of the waste liquid bottle are both connected to the second solenoid valve unit 1-34 via a pipeline. Reactor It is connected to the exhaust port 1-413 of 1-41.
[0063] The second solenoid valve unit 1-34 is used Reactor When the solution in 1-41 reaches a certain amount, the flow meter 1-33 and Reactor The pipe connecting the flow meter 1-33 and the waste liquid bottle 1-43 is closed, and the pipe connecting the flow meter 1-33 and the waste liquid bottle 1-43 is opened.
[0064] After the high-precision flowmeter 1-33 controls the required sample loading amount, the solenoid valve adjacent to the flowmeter 1-33 immediately switches the excess reaction waiting solution to the waste bottle 1-43. Reactor This ensures the accuracy of the amount of sample loaded into the waste bottle 1-41. After each sample loading, if necessary, a command as to whether or not to perform pipe cleaning can be written in the master computer 5, and the waste liquid from the pipe cleaning is also put into the waste liquid bottle 1-43. Reactor A mineral oil bubbler capable of preventing suck-back is connected to the inlet of 1-41. The purpose of this is to Reactor The air pressure in 1-41 is normalized, and external gas or water vapor is prevented from entering the reactor, and the sealing requirement of the entire automatic sample loading system 1 can be met. As shown in FIG. 5, the liquid phase synthesis auxiliary system 2 includes a temperature control device 2-1 and a mixer 2-2.
[0065] The master computer 5 incorporates the software programs used to control the specific workflow of the mixing device 2-2 and the temperature control device 2-1. Reactor 1-41 is provided in the mixer 2-2, and both the mixer 2-2 and the temperature controller 2-1 are electrically connected to the master computer 5.
[0066] The temperature control device 2-1 includes an ultraviolet light source 2-11 and a low-temperature circulation device 2-12.
[0067] The drain of the low-temperature circulation device 2-12 is connected to the pipeline of the circulating fluid inlet 1-416. The inlet of the low-temperature circulation device 2-12 is connected to the pipeline of the circulating fluid outlet.
[0068] The ultraviolet light source 2-11 is Reactor In the present invention, the ultraviolet light source 2-11 is preferably a mercury lamp light source with a model number of CEL-M series.
[0069] The mixing device 2-2 includes an automatic stirrer 2-21 and a thermostatic plate 2-22.
[0070] The automatic mixer 2-21 and the thermostatic plate 2-22 are both electrically connected to the master computer 5. The automatic mixer 2-21 operates in accordance with a mixing command from the master computer 5. Reactor It is used to stir the mixture in 1-41. Reactor 1-41 is installed in the automatic mixer 2-21. The automatic mixer 2-21 is installed on a thermostatic plate 2-22. The automatic mixer 2-21 rotates Reactor The constant temperature plate 2-22 drives the rotation of the 1-41 and realizes the mixing function by the action of centrifugal force. Reactor It is used to maintain the temperature of 1-41 constant.
[0071] Furthermore, the automatic stirrer 2-21 in the present invention may be a stirring rod, and is used to stir the mixed liquid in the reactor to uniformly mix the solution. Reactor It is located above 1-41.
[0072] Figure 6: Liquid phase synthesis online The automatic monitoring system 3 includes a sampling module 3-1, a power module 3-2, and a monitoring and analysis module 3-3.
[0073] The sampling module 3-1 is connected to the pipeline of the power module 3-2. The power module 3-2 is connected to the pipeline of the monitoring and analysis module 3-3. The sampling module 3-1, the power module 3-2, and the monitoring and analysis module 3-3 are all electrically connected to the master computer 5.
[0074] Sampling module 3-1 is Reactor The power module 3-2 is for applying suction force to the sampling module 3-1 in accordance with a suction command from the master computer 5, and for injecting the suctioned reaction solution into the monitoring and analysis module 3-3. The monitoring and analysis module 3-3 is for generating a monitoring report based on the reaction solution, and then transmitting the monitoring report to the master computer 5. The master computer 5 produces an analysis result based on the monitoring report.
[0075] The specific structures of each of the above modules provided in the present invention will now be described.
[0076] The sampling module 3-1 includes a stainless steel needle, a slide rail, and a rotating plate.
[0077] The stainless steel needle is connected to the power module 3-2 via a first pipeline. The first pipeline is installed on a slide rail, and the slide rail forms a set angle (preferably 60°) with respect to the horizontal line. The stainless steel needle is fixedly installed at one end of the slide rail, and the other end of the slide rail is a free end. The slide rail is for driving and sliding the stainless steel needle, and the stainless steel needle is Reactor 1-41 to suck up the reaction solution. The slide rail is fixed to the turntable. Both the turntable and the slide rail are electrically connected to the master computer 5.
[0078] Among other things, the slide rail includes a slide plate and a support frame. The slide plate moves downward along the support frame, and the stainless steel needle ReactorThe support frame is fixed to the rotating plate, and the rotating plate can drive and rotate the entire slide rail, so it is easy to suck the liquid in the container, even though the stainless steel needle is different. The slide rail can be adjusted up and down. Reactor The first pipe line is fixed in position 1-41. To fix the first pipe line more firmly, the slide rail may be provided with a slideway to facilitate fixing the first pipe line. The rotating plate (machining module group) drives and supports the slide rail, and rotates and stays at various positions at set angles toward different directions.
[0079] In the present invention, the stainless steel needle is preferably a 9# needle. At the connection position between the stainless steel needle and the first pipeline, a pierceable airtight rubber gasket and an organic filter head are also provided. Here, the selection specifications of the organic filter head include 0.22 μm, 0.45 μm, and 0.8 μm. When used, the front end of the organic filter head is lightly plugged with absorbent cotton, which corresponds to the molecular sieve that first filters the reaction solution, and then filtered through the filtration membrane of the organic filter head to meet the requirements for the liquid phase and realize double filtration, thereby effectively avoiding clogging of the organic filter head.
[0080] The power module 3-2 includes a power pump. The power pump is a syringe pump or a plunger pump. The power pump selected in the present invention has a strong suction force and also has a reverse suction function. The provision of the reverse suction function is effective in the liquid phase synthesis. online This is because the pipelines of the entire automatic monitoring system 3 can be easily cleaned.
[0081] The power pump is connected to the pipelines of the sampling module 3-1 and the monitoring and analysis module 3-3.
[0082] The monitoring and analysis module 3-3 is preferably a high performance liquid chromatography (HPLC). In the present invention, in order to facilitate the realization of the automatic monitoring function, the liquid chromatography is improved by removing and adjusting the sample loading part, connecting it to the online sample loading 6-way valve through a loop, receiving the master computer 5 to control the trigger operation, determining and selecting the operation method, and performing automatic flush cleaning after the operation is completed. The high performance liquid chromatography provides a report in TXT format based on the extracted reaction solution sample, and supplies it to the master computer 5 to extract the data and generate an analysis report.
[0083] In order to facilitate cleaning of the entire system, the liquid phase synthesis method provided by the present invention is O Online The automated monitoring system 3 further includes a cleaning module 3-4.
[0084] The cleaning module 3-4 is connected to the pipelines of the sampling module 3-1 and the power module 3-2.
[0085] The cleaning module 3-4 includes a first liquid container 3-41, a second liquid container 3-42, and a solenoid valve 3-43.
[0086] By driving the rotating disk, the stainless steel needle can suck up the cleaning liquid in the first liquid container 3-41. The second liquid container 3-42, the power module 3-2, and the monitoring and analysis module 3-3 are all connected to the solenoid valve 3-43 pipeline. The power module 3-2 may use a reverse suction function to suck up the cleaning liquid in the second liquid container 3-42 into the power pump, and then inject it into the monitoring and analysis module 3-3 to facilitate cleaning. The cleaning liquid used in the present invention is preferably an organic solution.
[0087] Among them, the solenoid valve 3-43 is preferably an online sample loading 6-way valve (high pressure flow path switching valve). It corresponds to the sample loading 6-way valve of the sample loader in high performance liquid chromatography, and connects the HPLC loop to the waste liquid. It is different from the 6-way valve in the HPLC, and is independently online and controlled by the master computer 5 or the HPLC.
[0088] The sliding and rotation of the slide rail and the rotating platen realized in the present invention are both performed using servo motors, which are existing prior art, so no detailed explanation will be given here.
[0089] Solution Phase Synthesis Provided by the Invention online During the process of automatic sampling, monitoring, and report analysis of the reaction solution using the automatic monitoring system 3, it is necessary to rely on a software program. online The specific advantages of the automatic monitoring system 3 will be explained in detail in conjunction with the software program embedded in the master computer 5. Since the focus of the present invention is on protecting the hardware structure, only a conceptual level explanation of the software control will be given.
[0090] This invention uses Shimadzu's DB version (database version) to analyze the liquid phase, prepares a short circuit joint for trigger control in advance, combines a short circuit signal from the master computer 5 to the PLC to control the liquid phase, operates automatically as necessary, and automatically generates a PDF version report and a TXT report in ASCII code of the original data after the operation is completed, and extracts the TXT report by the master computer 5.
[0091] The master computer 5 sets up an interface called "online monitoring" to continuously extract newly generated TXT reports. According to the liquid naming method, the newly generated TXT report is named after the previous TXT report to facilitate the extraction of the master computer 5, and the master computer 5 can compare, judge and analyze the new TXT report according to the logic relationship embedded inside after extracting it.
[0092] Taking the "pre-activation" one-pot reaction principle as an example, whether it is a general activation method or a light-induced activation method, after donor activation, "sampling monitoring" is required to monitor whether the donor is fully activated, that is, activation monitoring, giving feedback on the activation result, if the activation is not complete, continue to activate, or activate repeatedly, or continue to activate with light irradiation, if it is fully activated, enter the "reaction time", and after a certain time and temperature, "sampling monitoring" is performed to see whether the receptor has completely disappeared, and at the same time, whether a new compound has been generated, that is, reaction monitoring, and then giving feedback on the reaction result. Whether the receptor remains is the key to determining whether to continue the reaction of the next cycle, if the receptor remains, the reaction time is extended or the reaction temperature is increased to continue the reaction, if the receptor disappears or falls below a certain limit, the next cycle may be continued by default, or the activation reaction may be continued to be monitored. If the receptor continues to exist beyond a certain limit, it is considered to terminate the automated synthesis.
[0093] Based on the above, each system provided by the present invention is organically integrated, and the actual liquid phase automated synthesis apparatus obtained is as shown in Figure 7, and the length, width and height of the liquid phase automated synthesis apparatus in this combination mode are 870cm, 730cm and 600cm, respectively. This combination mode is not the only assembly method of the liquid phase automated synthesis apparatus provided by the present invention, and all combination methods that can be obtained by those skilled in the art in combination with the above content of the present invention fall within the protection scope of the present invention.
[0094] Here, in the liquid phase automated synthesis apparatus, a power distribution cabinet is installed to supply electric energy to the entire liquid phase automated synthesis apparatus. Moreover, in order to save layout space, the inside of the liquid phase automated synthesis apparatus provided by the present invention has a multi-layer structure, and each layer structure is provided with a door, and the door is provided with a stainless steel handle. The material of the door is mainly brown organic glass, so that the operator can easily block light and heat while observing the internal experimental process. Among them, the door is divided into a lower door, a side door, and an upper door, and the side door includes a left side door and a right side door. Each door is provided with a door stopper and a door hole to ensure the sealing of the entire liquid phase automated synthesis apparatus.
[0095] In addition, to facilitate sample collection, a linear slide rail is installed below the liquid storage module 1-5, which is fixed to the bottom plate. A side baffle separates the liquid storage module 1-5 from the mixer 2-2. Each embodiment in this specification has been described using an incremental approach, with the emphasis being on how each embodiment differs from other embodiments, and similar parts between the embodiments may be referenced interchangeably.
[0096] In this document, the principle and embodiment of the present invention are described using specific examples, but the description of the above examples is only used to assist in understanding the method of the present invention and its core idea. At the same time, those skilled in the art may make changes in the specific embodiments and application scope based on the idea of the present invention. As described above, the contents of this specification should not be understood as limitations on the present invention. [Explanation of symbols]
[0097] 1 Automatic sample loading system, 1-1 Inert gas supply module, 1-11 Inert gas reservoir, 1-12 Pressure regulating filter, 1-13 First solenoid valve unit, 1-131 First two-way solenoid valve, 1-132 Second two-way solenoid valve, 1-133 Three-way solenoid valve, 1-2 Sampling channel switching module, 1-21 First multi-channel switching valve, 1-22 Second multi-channel switching valve, 1-3 Quantitative module, 1-31 Syringe pump unit, 1-311 First syringe pump, 1-312 Second syringe pump, 1-32 Pressure sensor, 1-33 Flow meter, 1-34 Second solenoid valve unit, 1-4 Treatment module, 1-41 Reactor , 1-42 solution tube, 1-43 waste bottle, 1-5 liquid storage module, 1-51 liquid storage bottle, 2- liquid phase synthesis auxiliary system, 2-1 temperature control device, 2-11 ultraviolet light source, 2-12 low temperature circulation device, 2-2 mixing device, 2-21 automatic stirrer, 2-22 thermostatic plate, 3- liquid phase synthesis online Automatic monitoring system, 3-1 sampling module, 3-2 power module, 3-3 monitoring and analysis module, 3-4 cleaning module, 3-41 first liquid container, 3-42 second liquid container, 3-43 solenoid valve, 1-411 bottle mouth, 1-412 sampling port, 1-413 exhaust port, 1-414 sampling port, 1-415 bottle body, 1-4151 reaction liner, 1-4152 Temperature circulation layer, 1-4153 Vacuum layer, 1-416 Circulating fluid outlet, 1-417 Top cover, 5 Master computer
Claims
1. Including an automatic sample loading system, a liquid phase synthesis auxiliary system, a liquid phase synthesis online automatic monitoring system, a master computer and a reactor, The automatic sample loading system, the liquid phase synthesis auxiliary system, and the liquid phase synthesis online automatic monitoring system are all electrically connected to the master computer; the automatic sample loading system is for aspirating a liquid-phase synthesized sample into the automatic monitoring system by completing an automatic sample loading operation in accordance with a sample loading command from the master computer; the liquid-phase synthesis auxiliary system is for completing temperature and light irradiation control of a solution waiting for reaction in liquid-phase synthesis in accordance with a temperature control command and a light irradiation control command from the master computer; the automatic monitoring system is for monitoring the aspirated sample as a first reaction solution and creating a monitoring report; and the master computer is for generating an experimental analysis result in accordance with the monitoring report; The reactor includes a bottle mouth, a bottle body, a sample loading port, an exhaust port, a sampling port, a circulating liquid exhaust port, and a circulating liquid inlet, The centerline of the sampling port forms a set angle with respect to the longitudinal centerline of the bottle body; The reactor is connected to the automatic sample loading system, the liquid phase synthesis auxiliary system, and the liquid phase synthesis online automatic monitoring system through different first lines, respectively; The automatic sample loading system includes an inert gas supply module, a sampling channel switching module, a quantification module, a treatment module, and a liquid storage module; The liquid storage module and the sampling channel switching module are both connected to the inert gas supply module via a second pipeline, the quantitative module is connected to the sampling channel switching module and the treatment module respectively via a third pipeline, and the liquid storage module is connected to the sampling channel switching module via a fourth pipeline; The inert gas supply module, the sampling channel switching module, and the quantitative measurement module are all electrically connected to the master computer; The inert gas supply module is for supplying the inert gas stored therein to the liquid storage module and the sampling channel switching module through a second pipeline, the sampling channel switching module is for extracting the reaction waiting solution stored in the liquid storage module and switching the channel for extracting the reaction waiting solution, and the quantitative determination module is for determining the amount of the reaction waiting solution in the treatment module; The master computer is for controlling the on / off of the inert gas supply module and the quantitative measurement module, and for controlling the channel switching of the sampling channel switching module; The metering module includes a flow meter and a second solenoid valve unit; The treatment module includes a solution tube and a waste bottle; The sampling port of the reactor and the inlet of the waste liquid bottle are each connected to the second solenoid valve unit via a different tenth pipeline, and the solution tube is connected to an exhaust port of the reactor via an eleventh pipeline; the second solenoid valve unit is for closing a twelfth pipe connected between the flow meter and the reactor, and for opening a thirteenth pipe connected between the flow meter and the waste liquid bottle, when the solution in the reactor reaches a certain amount.
2. 2. The automated liquid phase synthesis apparatus according to claim 1, wherein the set angle is 60 degrees.
3. The center line of the exhaust port is perpendicular to the center line of the bottle mouth, The bottle body includes a reaction liner, a low-temperature circulating liquid layer, and a vacuum layer in this order from the inside to the outside, and in a cross-sectional view of the bottle body, the bottom of the reaction liner has an arc-shaped structure; The sampling port is connected to the reaction liner, 2. The automated liquid phase synthesis apparatus according to claim 1, wherein the circulating liquid outlet and the circulating liquid inlet are both connected to the low-temperature circulating liquid layer, and the circulating liquid outlet and the circulating liquid inlet are diagonally arranged.
4. The sampling channel switching module includes a first multi-channel switching valve and a second multi-channel switching valve; The first multi-channel switching valve is connected to M liquid storage bottles through a fifth pipe, and the second multi-channel switching valve is connected to N-M liquid storage bottles through a sixth pipe, where M is the number of liquid storage bottles connected to the first multi-channel switching valve, N is the total number of liquid storage bottles, and N-M is the difference between the N liquid storage bottles and the M liquid storage bottles; The metering module further includes a syringe pump unit and a pressure sensor; 2. The automated liquid phase synthesis apparatus according to claim 1, wherein an inlet of the syringe pump unit is connected to the sampling channel switching module via a seventh pipeline, an outlet of the syringe pump unit is connected to the flow meter via an eighth pipeline, and the flow meter is connected to the treatment module via a ninth pipeline, the second solenoid valve unit is installed in the eighth pipeline connecting the flow meter and the treatment module, the pressure sensor is installed in the pipeline connecting the syringe pump unit and the flow meter, and the second solenoid valve unit, the pressure sensor, and the flow meter are all electrically connected to the master computer.
5. The syringe pump unit includes a first syringe pump and a second syringe pump, 5. The automated liquid phase synthesis apparatus according to claim 4, wherein the first syringe pump is connected to one channel in the first multichannel switching valve via a fourteenth pipe, the second syringe pump is connected to one channel in the second multichannel switching valve via a fifteenth pipe, and a flow rate of the first syringe pump is smaller than a flow rate of the second syringe pump.
6. The liquid phase synthesis auxiliary system includes a mixing device and a temperature control device, 2. The liquid phase automated synthesis apparatus according to claim 1, wherein the reactor is installed in the mixing device, and the mixing device and the temperature control device are both electrically connected to the master computer.
7. The temperature control device includes an ultraviolet light source and a low-temperature circulation device, the drain of the low-temperature circulation device is connected to the circulating liquid inlet of the reactor via a sixteenth pipeline, the inlet of the low-temperature circulation device is connected to the circulating liquid outlet of the reactor via a seventeenth pipeline, and the ultraviolet light source is for irradiating the reactor; The mixing device includes an automatic stirrer and a thermostatic plate; 7. The liquid phase automated synthesis apparatus according to claim 6, wherein the automatic stirrer and the thermostatic plate are both electrically connected to the master computer, the automatic stirrer is for stirring the mixed liquid in the reactor according to a stirring command from the master computer, the reactor is placed on the automatic stirrer, and the thermostatic plate is for maintaining the temperature of the reactor constant.
8. The liquid phase synthesis online automatic monitoring system includes a sampling module, a power module, a monitoring and analysis module, and a cleaning module, The sampling module is connected to the power module via an eighteenth line, and the power module is connected to the monitoring and analysis module via a nineteenth line, and the sampling module, the power module, and the monitoring and analysis module are all electrically connected to the master computer; The sampling module is for sucking the second reaction solution contained in the reactor, the power module is for applying suction force to the sampling module in accordance with a suction command from the master computer, and for injecting the second reaction solution sucked by the sampling module into the monitoring and analysis module to use it as a first reaction solution, the monitoring and analysis module is for generating a monitoring report using the first reaction solution and then transmitting the monitoring report to the master computer, and the master computer generates an analysis result based on the monitoring report, 2. The automated liquid phase synthesis apparatus according to claim 1, wherein the cleaning module is connected to the sampling module and the power module via a twentieth pipe, respectively.
9. The sampling module includes a stainless steel needle, a slide rail, and a rotating plate; the stainless steel needle is connected to the power module through a first pipeline, the first pipeline is disposed on the slide rail, and the slide rail forms a set angle with respect to a horizontal line, the stainless steel needle is fixedly disposed on one end of the slide rail, and the other end of the slide rail is a free end, the slide rail is for driving and sliding the stainless steel needle, and the stainless steel needle is for entering a reactor to suck up a second reaction solution, the slide rail is fixedly installed on the turntable, and both the turntable and the slide rail are electrically connected to the master computer, the power module includes a power pump, the power pump being a syringe pump or a plunger pump; the power pump is connected to the sampling module and the monitoring and analysis module via a twenty-first line; the monitoring and analysis module is a high performance liquid chromatograph; the cleaning module includes a first liquid container, a second liquid container, and a solenoid valve; The liquid phase automated synthesis apparatus according to claim 8, characterized in that the stainless steel needle is for sucking up the cleaning liquid in the first liquid container, and the second liquid container, the power module, and the monitoring and analysis module are all connected to the solenoid valve via different 22nd pipelines.
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