Full-automatic intrinsic safety experiment robot platform based on microfluidic technology

Abstract

The invention discloses a full-automatic intrinsic safety experiment robot platform based on a microfluidic technology. The full-automatic intrinsic safety experiment robot platform comprises an automatic pumping sample injection system, a microchip reactor, an automatic sample receiving system, an automatic cleaning system, an accurate control system, a multifunctional online detection system and intelligent control software. According to the platform, through a silicon carbide ceramic micro-channel and a machine learning optimization model, full-closed automatic operation of high-temperature and high-pressure synthesis 200 DEG C / 20 MPa and dangerous experiments is realized, the reagent dosage is reduced to micro-upgrade, the reaction time is shortened by 90%, and the accident risk is zero; according to the invention, the data fusion analysis error of multiple sensors such as Raman spectrum, fluorescence, DLS and the like is less than or equal to 1%, LIMS system interconnection and ISO / IEC compliance report generation are supported, the method is suitable for high-risk experiments in the fields of pharmacy, nuclear chemistry, nano materials and the like, and laboratory automation and intrinsic safety upgrading are promoted.

Description

Technical Field

[0001] The present invention relates to the technical field of laboratory automation, and in particular to a fully automatic intrinsically safe experimental robot platform based on microfluidic technology. Background Art

[0002] In fields such as chemistry, biology, and materials science, many experiments require exposure to hazardous conditions, including high temperatures, high pressures, toxic and hazardous materials, and radioactive materials. These pose a serious threat to the safety of researchers and limit their repeatability and efficiency. Traditional solutions employ closed reactors, fume hoods, and protective clothing, but these methods fail to completely eliminate safety hazards and are complex and inefficient.

[0003] With the development of microfluidics and automation technology, microchip experimental platforms have gradually become a hot topic in laboratory research. Microchip platforms have the advantages of low sample consumption, fast reaction speed, and easy control.

[0004] However, the existing microchip experimental platform still has deficiencies in terms of automation, safety, and detection methods, and cannot meet the needs of high-risk experiments.

[0005] Therefore, there is an urgent need to provide an intrinsically safe and highly automated microchip experimental platform that can achieve efficient, accurate and repeatable operations of dangerous experiments while ensuring the safety of experimenters. Summary of the Invention

[0006] In view of this, the present invention provides a fully automatic intrinsically safe experimental robot platform based on microfluidic technology. The platform realizes rapid chemical reactions and accurately controls parameters such as reaction temperature, pressure, and residence time through an automatic pumping sampling system, an automatic sample receiving system, and an automatic cleaning system. The reaction system is encapsulated in a protective box, combined with microscope detection, online pH value, potential, fluorescence, laser Raman and other detection systems, and parameter optimization and intelligent control of the entire reaction process are achieved through programming, solving the safety risk problems in laboratories in experiments such as high temperature, high pressure, toxic and harmful, and radioactive experiments.

[0007] In order to solve the above technical problems, the present invention adopts the following technical solutions:

[0008] A fully automatic intrinsically safe experimental robot platform based on microfluidic technology, including: automatic pumping and sampling system, microchip reactor, automatic sample receiving system, automatic cleaning system, precise control system, multifunctional online detection system, intelligent control software;

[0009] Automatic pumping injection system: used to accurately and automatically pump reagents and samples into the microchip reactor;

[0010] Microchip reactor: It has a micron-scale channel structure, which is used to achieve fast and uniform chemical reactions and easy to control reaction conditions;

[0011] Automatic sampling system: used to automatically collect reaction products to avoid safety risks caused by manual operation.

[0012] Automatic cleaning system: used to automatically clean the microchip reactor and pipelines after the experiment to prevent reagent residue;

[0013] Precision control system: used for real-time monitoring and adjustment of temperature, pressure, flow rate, and residence time parameters to achieve precise control of chemical reaction conditions;

[0014] Multifunctional online detection system: Integrates microscope observation, online pH value, potential, fluorescence, and laser Raman detection methods to monitor key parameters and product characteristics during the reaction in real time;

[0015] Intelligent control software: used to realize automatic control, parameter optimization and data analysis of the entire experimental process through programming;

[0016] The robotic platform is centered around the microchip reactor, with its front end connected to the automatic pumping and sampling system via a corrosion-resistant pipeline, and its rear end connected to the automatic sampling system via a pressure-adaptive valve. The embedded units of the precision control system are distributed in each hardware module, and the central processing unit is located in an explosion-proof cabinet at the rear of the platform, which regulates temperature, pressure, and flow rate in real time. The multifunctional online detection system is arranged around the microchannel and coupled to the channel through an optical window. The automatic cleaning system is located at the bottom of the platform and is connected to the reactor and pipeline loop through a multi-way valve group. The intelligent control software runs on an industrial computer, integrates all subsystem data through the EtherCAT bus, and drives the AI ​​optimization algorithm and safety protocol.

[0017] Preferably, the automatic pumping injection system consists of a high-precision syringe pump, corrosion-resistant piping and leak-proof sealing valve, supports multi-channel reagent synchronous delivery, and has a flow rate range of 0.1-100 mL / min;

[0018] The microchip reactor has a built-in microfluidic structure, can withstand temperatures of -50°C to 200°C, pressures of 0.1-20 MPa, and a surface roughness of ≤0.1 μm;

[0019] The automatic sample collection system integrates a pressure-adaptive valve and a sealed collection container to support the safe transfer of high-temperature, radioactive or toxic products;

[0020] The automatic cleaning system is equipped with a multi-stage cleaning module, with a cleaning efficiency of ≥99.9% and a residual detection limit of ≤1ppm;

[0021] The precise control system monitors and adjusts temperature, pressure, and flow rate in real time, and has built-in multi-level safety thresholds. When the pressure is greater than 10MPa, the speed is reduced, and when it is greater than 20MPa, an emergency shutdown is performed.

[0022] The multifunctional online detection system synchronously integrates a high-temperature and high-pressure microscope, an online Raman spectrometer, a pH / potential sensor, and a fluorescence detection module, and the data fusion analysis error is ≤1%;

[0023] The intelligent control software is based on an automatic parameter optimization model using a machine learning algorithm, supports experimental program programming, multimodal data visualization, and security log generation, and has ISO 13849-1 certified fault self-diagnosis capabilities.

[0024] Preferably, the accuracy of the high-precision injection pump is ±0.1μL, and the material of the corrosion-resistant pipeline is PTFE or titanium alloy; the microchip reactor is made of silicon carbide ceramic or sapphire, and the channel width of the built-in microfluidic structure is 50-500μm, and the aspect ratio is ≥5:1; the response time of the integrated pressure adaptive valve is ≤10ms; the multi-stage cleaning module is acid / alkali / solvent cleaning liquid switching; the precise control system monitors and adjusts the temperature ±0.1℃, pressure ±0.01MPa, and flow rate ±0.5% of the set value in real time; the resolution of the high-temperature and high-pressure microscope is ≤1μm, the detection limit of the online Raman spectrometer is 0.1mol / L, the accuracy of the pH / potential sensor is ±0.01, and the excitation wavelength of the fluorescence detection module is 200-900nm.

[0025] Preferably, the microchip reactor can be modularly replaced to adapt to different experimental scenarios, including high-temperature synthesis and nanomaterial preparation, and the interface is standardized to support rapid installation and sealing detection with a leakage rate of <0.1 μL / min.

[0026] Preferably, the automatic pumping injection system is equipped with an ultrasonic mixer to achieve instantaneous and uniform mixing of reagents in the microchannel, with a mixing time of ≤10ms.

[0027] Preferably, the frequency of the ultrasonic mixer is 20-40 kHz.

[0028] Preferably, the multifunctional online detection system supports plug-and-play detection modules, including an expandable mass spectrometry interface and a dynamic light scattering DLS particle size analysis module with a range of 1-1000nm, and the electromagnetic compatibility between modules meets the IEC61000 standard, with crosstalk ≤-60dB.

[0029] Preferably, the intelligent control software has a built-in radioactive experiment-specific protocol, automatically generates a waste treatment report that complies with IAEA standards, and realizes data intercommunication with the laboratory information management system LIMS through the OPC UA protocol.

[0030] Preferably, the platform is designed with a negative pressure isolation cavity, and the toxic gas leakage concentration is <1ppm, which complies with OSHA standards.

[0031] Preferably, the thickness of the lead shielding layer is ≥2 mm.

[0032] Compared with the prior art, the present invention has achieved the following technical effects:

[0033] (1) Intrinsic safety: The entire experiment is closed and automated, avoiding manual contact with harmful reagents or dangerous reaction conditions, and achieving inherently safe experimental operations;

[0034] (2) High efficiency and precision: The microchip reactor achieves rapid reaction, reduces the amount of reagents used, and accurately controls parameters, thereby improving experimental efficiency and data reproducibility;

[0035] (3) Multifunctional detection: Integrate multiple online detection methods to obtain reaction information in real time, facilitating process monitoring and result analysis;

[0036] (4) Intelligent optimization: Integrating multiple detection methods into one, achieving comprehensive and real-time monitoring of the reaction process, providing support for parameter optimization and process control; through software programming, parameter optimization can be automatically performed to find the optimal reaction conditions;

[0037] (5) Collaborative design of intrinsic safety and extreme performance: Breaking through the bottleneck of limited performance of traditional safety equipment, achieving high-throughput reactions under extreme conditions (800°C / 200MPa) with zero leakage;

[0038] (6) Ultra-high throughput microfluidic chip: 3D microfluidic structure based on MEMS technology (aspect ratio ≥ 10:1), single chip integrating 10+ parallel reaction units, increasing the throughput to 100 times that of traditional methods;

[0039] (7) Wide applicability: The platform can be used in experiments under various hazardous conditions such as high temperature, high pressure, toxic and harmful substances, and radioactivity, and has broad application prospects;

[0040] (8) Cross-scale integration of micro-nano manufacturing, functional materials and industrial interconnection: From nanoscale microfluidic processing to factory-level system interconnection, covering the entire technology stack from laboratory to industrialization. BRIEF DESCRIPTION OF THE DRAWINGS

[0041] Figure 1 This is a structural diagram of a fully automatic intrinsically safe experimental robot platform based on microfluidic technology in the present invention. DETAILED DESCRIPTION

[0042] The following will clearly and completely describe the technical solutions in the embodiments of the present invention in conjunction with the accompanying drawings. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.

[0043] The present invention discloses a fully automatic intrinsically safe experimental robot platform based on microfluidic technology, comprising: an automatic pumping and sampling system, a microchip reactor, an automatic sample receiving system, an automatic cleaning system, a precise control system, a multifunctional online detection system, and intelligent control software; wherein,

[0044] Automatic pumping injection system: used to accurately and automatically pump reagents and samples into the microchip reactor;

[0045] Microchip reactor: It has a micron-scale channel structure, which is used to achieve fast and uniform chemical reactions and easy to control reaction conditions;

[0046] Automatic sampling system: used to automatically collect reaction products to avoid safety risks caused by manual operation.

[0047] Automatic cleaning system: used to automatically clean the microchip reactor and pipelines after the experiment to prevent reagent residue;

[0048] Precision control system: used for real-time monitoring and adjustment of temperature, pressure, flow rate, and residence time parameters to achieve precise control of chemical reaction conditions;

[0049] Multifunctional online detection system: Integrates microscope observation, online pH value, potential, fluorescence, and laser Raman detection methods to monitor key parameters and product characteristics during the reaction in real time;

[0050] Intelligent control software: used to realize automatic control, parameter optimization and data analysis of the entire experimental process through programming;

[0051] The robotic platform is centered around a microchip reactor, with the front end connected to an automatic pumping and sampling system via corrosion-resistant piping, and the back end connected to an automatic sampling system via a pressure-adaptive valve. Embedded units of the precise control system are distributed across the hardware modules, with the central processing unit located in an explosion-proof cabinet at the rear of the platform, enabling real-time regulation of temperature, pressure, and flow rate. A multifunctional online detection system is arranged around the microchannel and coupled to the channel through an optical window. The automatic cleaning system is located at the bottom of the platform, connected to the reactor and pipeline loop through a multi-way valve group. The intelligent control software runs on an industrial computer, integrating all subsystem data through the EtherCAT bus to drive AI optimization algorithms and safety protocols.

[0052] The automatic pumping injection system consists of a high-precision syringe pump, corrosion-resistant piping and leak-proof sealing valves, supporting the simultaneous delivery of multi-channel reagents with a flow rate range of 0.1-100mL / min;

[0053] The microchip reactor has a built-in microfluidic structure, can withstand temperatures from -50°C to 200°C, pressures from 0.1 to 100 MPa, and a surface roughness of ≤0.1 μm;

[0054] The automatic sampling system integrates a pressure-adaptive valve and a closed collection container to support the safe transfer of high-temperature, radioactive or toxic products;

[0055] The automatic cleaning system is equipped with a multi-stage cleaning module, with a cleaning efficiency of ≥99.9% and a residual detection limit of ≤1ppm;

[0056] The precise control system monitors and adjusts temperature, pressure, and flow rate in real time, and has built-in multi-level safety thresholds. When the pressure is >10MPa, the speed is reduced, and when it is >20MPa, the machine is shut down immediately.

[0057] The multifunctional online detection system synchronously integrates a high-temperature and high-pressure microscope, an online Raman spectrometer, a pH / potential sensor, and a fluorescence detection module, with a data fusion analysis error of ≤1%;

[0058] The intelligent control software is based on an automatic parameter optimization model using machine learning algorithms. It supports experimental program programming, multimodal data visualization, and security log generation, and has ISO 13849-1 certified fault self-diagnosis capabilities.

[0059] The high-precision injection pump has an accuracy of ±0.1μL, and the corrosion-resistant pipeline is made of PTFE or titanium alloy; the microchip reactor is made of silicon carbide ceramic or sapphire, and the channel width of the built-in microfluidic structure is 50-500μm, with an aspect ratio of ≥5:1; the response time of the integrated pressure adaptive valve is ≤10ms; the multi-stage cleaning module switches between acid / alkali / solvent cleaning liquids; the precise control system monitors and adjusts the temperature in real time to ±0.1℃, the pressure to ±0.01MPa, and the flow rate to ±0.5% of the set value; the resolution of the high-temperature and high-pressure microscope is ≤1μm, the detection limit of the online Raman spectrometer is 0.1mol / L, the accuracy of the pH / potential sensor is ±0.01, and the excitation wavelength of the fluorescence detection module is 200-900nm.

[0060] The microchip reactor can be replaced modularly to adapt to different experimental scenarios, including high-temperature synthesis, radioactive labeling, and nanomaterial preparation. The standardized interface design supports rapid installation and sealing detection with a leakage rate of <0.1μL / min.

[0061] The automatic pumping injection system is equipped with an ultrasonic mixer to achieve instantaneous and uniform mixing of reagents in the microchannel, with a mixing time of ≤10ms.

[0062] The frequency of the ultrasonic mixer is 20-40 kHz.

[0063] The multifunctional online detection system supports plug-and-play detection modules, including an expandable mass spectrometry interface and a dynamic light scattering (DLS) particle size analysis module with a range of 1-1000nm. The electromagnetic compatibility between modules meets the IEC 61000 standard, with crosstalk ≤-60dB.

[0064] The intelligent control software has a built-in special protocol for radioactive experiments, automatically generates waste disposal reports that comply with IAEA standards, and realizes data interoperability with the laboratory information management system LIMS through the OPC UA protocol.

[0065] The platform uses a lead shielding layer and a negative pressure isolation chamber design to ensure that the radiation leakage rate of radioactive experiments is less than 0.1μSv / h and the toxic gas leakage concentration is less than 1ppm, which complies with OSHA standards.

[0066] The thickness of the lead shielding layer is ≥2mm.

[0067] Example 1: Safety experiment of high temperature and high pressure reaction

[0068] 1. System composition

[0069] Automatic pumping injection system: including high-precision syringe pump and high-temperature and high-pressure resistant injection pipeline for accurate delivery of liquid reagents;

[0070] Microchip reactor: Made of high-temperature and high-pressure resistant materials (such as silicon and ceramics), with a built-in microfluidic structure, it can withstand temperatures up to 200°C and pressures up to 20MPa;

[0071] Automatic sample collection system: composed of a high-pressure valve and a collection container to ensure safe collection of products under high pressure;

[0072] Automatic cleaning system: equipped with high-pressure cleaning liquid pump and cleaning pipeline, it can clean the residue in the reactor under high temperature and high pressure conditions;

[0073] Precise control system: equipped with high-precision temperature controller, pressure sensor and flow controller to monitor and adjust reaction conditions in real time;

[0074] Multifunctional online detection system: integrated with high temperature and high pressure microscope and online Raman spectrometer to observe the morphology of reactants and detect changes in chemical bonds;

[0075] Intelligent control software: establishes a control interface for experimental parameters, programmable settings for temperature, pressure, flow rate, etc., and records data in real time;

[0076] 2. Experimental Procedure

[0077] Reagent preparation: Load reagent A and reagent B that require high temperature and high pressure reaction into the injector respectively;

[0078] System startup: Open the intelligent control software and set the initial reaction conditions: temperature 200°C, pressure 15 MPa, flow rate 10 μL / min;

[0079] Automatic injection: The syringe pump pumps reagents A and B into the microchip reactor synchronously at the set flow rate;

[0080] Reaction: Inside the microchip reactor, reagents A and B rapidly mix and react under high temperature and pressure;

[0081] Online detection: Observe the morphological changes of the reaction through a microscope, and use Raman spectrometer to detect the chemical structure of reactants and products in real time;

[0082] Parameter adjustment: Based on real-time detection data, the intelligent control software automatically optimizes temperature and pressure to achieve optimal reaction efficiency;

[0083] Product collection: The reaction products are collected into a pressure-resistant container through an automatic sampling system;

[0084] Automatic cleaning: After the experiment, the automatic cleaning system is started and the reactor and pipelines are flushed with cleaning fluid under high pressure.

[0085] 3. Experimental Results

[0086] Efficient reaction: The entire reaction process is completed within seconds, which greatly shortens the time compared to traditional high-temperature and high-pressure reactions;

[0087] Safe and reliable: fully automated operation without manual intervention, eliminating the safety risks of high temperature and high pressure operations;

[0088] Data recording: The intelligent control software saves all experimental parameters and test data for subsequent analysis.

[0089] Example 2: Safe synthesis of toxic and hazardous substances

[0090] 1. System composition

[0091] Automatic pumping injection system: The injection pipeline is made of corrosion-resistant materials (such as PTFE) to prevent the corrosion of toxic reagents to the equipment;

[0092] Microchip reactor: Made of inert glass and designed with microfluidic structure, it reduces reagent usage and reaction residues.

[0093] Automatic sampling system: closed collection system to prevent leakage of toxic products;

[0094] Automatic cleaning system: Uses special neutralizing liquid or solvent to automatically clean residual toxic substances;

[0095] Precise control system: real-time monitoring of reaction temperature and flow rate to ensure the reaction proceeds under safe conditions;

[0096] Multifunctional online detection system: equipped with online pH meter and electrochemical sensor to monitor pH value and potential changes during the reaction process;

[0097] Intelligent control software: can program reaction conditions and has safety alarm function.

[0098] 2. Experimental Procedure

[0099] Reagent preparation: Place toxic reagents C and D into sealed injectors respectively;

[0100] System startup: Set reaction conditions: temperature 25°C, flow rate 5 μL / min, and turn on the safety monitoring module;

[0101] Automatic injection: Reagents C and D enter the microchip reactor at a set ratio and flow rate;

[0102] Reaction proceeds: In the microfluidic channel, C and D mix rapidly, and the target reaction occurs;

[0103] Online detection: pH meter and electrochemical sensor monitor the pH value and potential of the reaction solution in real time to determine the reaction progress;

[0104] Safety monitoring: If an abnormality is detected, such as pH value outside the safe range, the system automatically stops sampling and initiates emergency treatment;

[0105] Product collection: Products are automatically collected into sealed containers to prevent toxic substances from leaking;

[0106] Automatic cleaning: Use neutralizing liquid to clean the equipment to ensure no residue.

[0107] 3. Experimental Results

[0108] Safety assurance: fully enclosed operating procedures and real-time monitoring ensure the safe handling of toxic and hazardous substances;

[0109] Reaction efficiency: Microchip reactors increase reaction rates, reduce reagent usage and waste generation;

[0110] Data acquisition: Real-time monitoring data helps optimize reaction conditions and improves experimental reproducibility and reliability.

[0111] Example 3: Radioisotope labeling experiment

[0112] 1. System composition

[0113] Automatic pumping injection system: The injection pipeline is made of radiation-resistant titanium alloy and equipped with a leak-proof sealing valve to ensure the safe delivery of radioactive reagents;

[0114] The integrated dual-channel syringe pump has an accuracy of ±0.1μL, supporting precise mixing of trace reagents;

[0115] Microchip reactor: lined with a lead shielding layer with a thickness of 2mm, radiation leakage rate <0.1μSv / h, in line with GB 18871-2002 standard;

[0116] The microchannel is made of quartz with a channel width of 100μm, which is corrosion-resistant and easy to decontaminate.

[0117] Automatic sampling system: equipped with a lead-shielded sealed collection container (compliant with IAEA standards) to support automatic sealing and classification of radioactive waste liquid;

[0118] Built-in radiation sensor to monitor the container surface dose rate in real time, threshold alarm: >0.5μSv / h.

[0119] Precise control system: integrated radiation dose monitoring module to display the radiation level inside and outside the reactor in real time;

[0120] Temperature control range: -20℃ to 100℃ (for low temperature labeling reaction);

[0121] Multifunctional online detection system: equipped with a scintillator detector to monitor the radioactivity in the reaction solution in real time, with a detection limit of 1Bq / mL;

[0122] Integrated micro mass spectrometry module MS for mass spectrometry analysis of isotope-labeled products;

[0123] Intelligent control software: dedicated interface for radioactive experiments, supporting marker path programming, such as 1 4 Synthetic route of C-labeled glucose.

[0124] Automatically generate radioactive waste disposal logs to comply with nuclear safety regulations.

[0125] 2. Experimental Procedure

[0126] Reagent preparation:

[0127] Will 14 C-labeled precursors (such as NaH 14 CO3) and non-radioactive substrate (such as glucose) are loaded into radiation-proof injectors respectively.

[0128] System startup:

[0129] The radiation safety mode was turned on and the initial conditions were set as follows: temperature 25°C, flow rate 2 μL / min, and reaction time 10 min.

[0130] Automatic injection:

[0131] The syringe pump pumps in a 1:1 volume ratio simultaneously 14 C precursor and substrate solution enter the microchip reactor.

[0132] The reaction proceeds:

[0133] In the microchannel, 1 4 The C precursor and the substrate undergo a labeling reaction under the action of a catalyst, with a residence time of ≤30 seconds.

[0134] Online detection:

[0135] The scintillator detector monitors the activity of the reaction solution in real time, and the mass spectrometer module analyzes the molecular weight of the labeled product with an error of ≤0.01Da.

[0136] Security Monitoring:

[0137] If the radiation dose exceeds the limit, the system automatically cuts off the injection and activates emergency shielding.

[0138] Product collection:

[0139] The labeled product is transferred to a closed container through a lead shielded pipe, and the waste liquid enters a dedicated storage tank.

[0140] Automatic cleaning:

[0141] Use EDTA complex cleaning solution to circulate and flush the system to remove radioactive residues, with a cleaning efficiency of ≥99.9%.

[0142] 3. Experimental Results

[0143] Labeling efficiency: 1 4 The efficiency of C-labeled glucose reached 97.3% (compared to 85% by the traditional method), and the isotope distribution was uniform (RSD < 2%).

[0144] Safety: The operator's radiation exposure during the entire process is 0μSv, and the risk of waste liquid leakage is reduced by 100%.

[0145] Data recording: The software automatically generates radioactivity-time curves, mass spectra, and security logs, supporting traceability audits.

[0146] Example 4: Controllable Synthesis of Nanomaterials

[0147] 1. System composition

[0148] Automatic pumping injection system: multi-channel gradient pump, flow rate range 0.1-10mL / min, accuracy ±0.5%, supports dynamic ratio adjustment of precursor solution;

[0149] Equipped with an ultrasonic mixer to ensure uniform nucleation of nanocrystal nuclei;

[0150] Microchip reactor: Design a multi-stage microfluidic structure with a width of 200 μm and a depth of 50 μm, and control the crystal growth time by flow rate gradient;

[0151] Made of glass, resistant to high temperature (≤200℃) and strong acid / alkali environment;

[0152] Automatic sampling system: integrated centrifugal separation module, capable of online separation of nanoparticles and reaction solution (speed ≤ 10,000 rpm);

[0153] Precise control system: Dynamically adjust the temperature gradient (±0.1°C) and flow rate gradient (±0.01mL / min) within the microchannel;

[0154] Multifunctional online detection system: Online dynamic light scattering (DLS) module: real-time monitoring of nanoparticle size distribution, ranging from 1-1000nm, with a resolution of ±1nm;

[0155] UV-Vis spectrometer: detects plasmon resonance peaks (such as the 520nm absorption peak of gold nanoparticles);

[0156] Intelligent control software: built-in nanosynthesis process library (such as gold, silver, and quantum dot synthesis templates), supports one-click start of optimization process;

[0157] Automatically adjust flow rate and temperature based on feedback data to achieve precise dimensional control.

[0158] 2. Experimental Procedure

[0159] Reagent preparation:

[0160] Precursor solution: chloroauric acid (HAuCl4, 0.1 mM) and sodium citrate (1% w / v) were loaded into the injector respectively.

[0161] System startup:

[0162] Select the "Gold Nanoparticle Synthesis" template and set the target particle size to 20 nm (PDI ≤ 0.1).

[0163] Automatic injection:

[0164] HAuCl4 and sodium citrate were pumped into the microchannel at a flow rate ratio of 10:1 by a gradient pump and mixed rapidly.

[0165] The reaction proceeds:

[0166] The nucleation was completed at 80°C in the primary microchannel, and the growth time was controlled at 25°C in the secondary microchannel with a residence time of 2 minutes.

[0167] Online detection:

[0168] DLS displays the particle size distribution in real time, with an average size of 19.8 nm and PDI = 0.08, and UV-Vis monitors the peak intensity at 520 nm.

[0169] Parameter adjustment:

[0170] The software automatically fine-tunes the sodium citrate flow rate (+5%) to compensate for particle size deviations.

[0171] Product collection:

[0172] The nanoparticle solution is purified by the centrifugal module and collected, and the waste liquid enters the recovery pipeline.

[0173] Automatic cleaning:

[0174] Use aqua regia to circulate and clean the system to ensure that no metal residue remains.

[0175] 3. Experimental Results

[0176] Size control: The average size of gold nanoparticles is 20.1 nm (20.5 nm for the traditional batch method), and the dispersion index PDI is 0.07 (PDI for the traditional method is 0.25).

[0177] Synthesis efficiency: The output in continuous flow mode reaches 5g / h (0.5g / h in traditional method), and the reagent utilization rate is increased by 90%.

[0178] Data recording: The software generates particle size distribution diagrams, UV-Vis spectra and process parameter curves, and supports the export of ISO quality reports.

[0179] The comparison of implementation effects is shown in Table 1;

[0180] Table 1:

[0181]

[0182] like Figure 1 The figure shows the structure of a fully automatic intrinsically safe experimental robot platform based on microfluidic technology of the present invention; wherein,

[0183] 1. Automatic pumping injection system

[0184] Position relationship: Located at the front end of the platform, it is directly connected to the inlet of the microchip reactor through a corrosion-resistant pipe (PTFE / titanium alloy). The pipe interface adopts a quick-release seal design and complies with the ISO 2852 standard.

[0185] Working principle:

[0186] Multi-channel synchronous delivery: The flow rate of each channel (0.1-100mL / min) is controlled by a high-precision syringe pump (±0.1μL) according to the preset program, and the pressure feedback regulating valve is combined to dynamically balance the flow fluctuation;

[0187] Anti-leakage control: The sealing valve adopts double O-ring redundant sealing. When the pressure sensor detects abnormal pressure drop in the pipeline (>5% of the set value), the corresponding channel will be closed immediately and the alarm will be triggered;

[0188] Ultrasonic mixing: An ultrasonic transducer (20-40kHz) is integrated before the microchannel inlet to achieve molecular-level mixing of reagents within 10ms through the cavitation effect.

[0189] 2. Microchip Reactor

[0190] Position relationship: Located in the core area of ​​the platform, it is connected to the sampling system, sample receiving system and detection module through standardized interfaces.

[0191] Working principle:

[0192] Extreme condition tolerance: Silicon carbide ceramic microchannels (aspect ratio ≥ 5:1) have been optimized through finite element thermodynamic simulation to maintain a deformation rate of < 0.01% at 500°C / 100MPa.

[0193] Mass transfer enhancement: Laser-etched periodic grooves on the microchannel surface with a depth of 10 μm and a spacing of 200 μm induce Dean vortices, which increase mass transfer efficiency by 3 times under laminar flow conditions.

[0194] Modular replacement: Magnetic positioning pins and pneumatic locking devices enable quick disassembly and assembly within 1 minute. The sealing test uses helium mass spectrometry leak detection method, with a leakage rate of <0.1μL / min.

[0195] 3. Automatic sample receiving system

[0196] Position relationship: Located downstream of the microchip reactor outlet, connected to a sealed collection container (316L stainless steel) through a high-pressure metal bellows.

[0197] Working principle:

[0198] Pressure adaptive transfer: When the reactor outlet pressure exceeds the threshold (0.1MPa), the piezoelectric ceramic valve (response time ≤ 10ms) opens, and the product enters the collection tank protected by inert gas after passing through the cooling coil (liquid nitrogen quenching);

[0199] Safety protection: Radioactive or toxic products pass through the lead shielding layer with a thickness of 2mm, and are monitored by the wrapped double-layer glass window. The negative pressure in the tank is maintained at -50Pa, and the leakage rate is <1ppm.

[0200] 4. Automatic cleaning system

[0201] Position relationship: integrated at the bottom of the platform, cyclically connected to the microchip reactor, pipelines and detection modules through a multi-way valve group;

[0202] Working principle:

[0203] Multi-stage cleaning procedure: nitric acid (68%), sodium hydroxide (1 M), and supercritical CO2 were injected sequentially, and residues were removed by pulse jet (flow rate 50 mL / min). The cleaning efficiency was verified in real time by online UV spectroscopy (254 nm);

[0204] Residue monitoring: After cleaning, X-ray fluorescence (XRF) is used to detect surface metal residues (limit <1ppm), and the data is uploaded to the LIMS system for archiving.

[0205] 5.Precise control system

[0206] Position relationship: Embedded control units are distributed in each subsystem, and the central processing unit is located in the explosion-proof cabinet at the rear of the platform;

[0207] Working principle:

[0208] Multi-parameter closed-loop control:

[0209] Temperature: The reactor's peripheral thermocouple (K type) and Peltier module are regulated by PID algorithm to achieve ±0.1°C steady-state control;

[0210] Pressure: Based on the Bernoulli equation, the pressure difference caused by the change in flow rate is dynamically compensated, and the piezoelectric sensor (0.01MPa accuracy) is linked to the proportional valve for adjustment;

[0211] Flow rate: The syringe pump stepper motor uses closed-loop encoder feedback, and the flow fluctuation is suppressed to ±0.5%;

[0212] Safety interlock: When the pressure is >80MPa, the gradient deceleration is triggered (the flow rate drops by 10% every 10 seconds); when it is >90MPa, the electromagnetic brake locks the pump shaft within 0.1 seconds.

[0213] 6. Multifunctional online detection system

[0214] Positional relationship: The detection module is arranged around the microchip reactor and coupled to the flow channel optical window through a fiber collimator (SMA905 interface);

[0215] Working principle:

[0216] Multimodal data fusion:

[0217] Raman spectroscopy: A 785 nm laser was used to collect characteristic peaks of the reactants (signal-to-noise ratio > 100:1) through a confocal probe (NA = 0.7), and the concentration was quantitatively analyzed using a PLS algorithm (error ≤ 0.1 mol / L).

[0218] High-temperature and high-pressure microscope: sapphire window, 1 mm thick, with a long working distance objective (20×, WD = 15 mm), for real-time observation of particle nucleation at 500°C (resolution 1 μm);

[0219] DLS particle size analysis: The 633 nm laser scattering signal is processed by an autocorrelator, and the PDI value of the nanoparticles is dynamically fed back to adjust the flow rate to maintain monodispersity (PDI ≤ 0.08);

[0220] Plug and play expansion: The mass spectrometer interface uses a molecular pump cascade pumping (ultimate vacuum 10 -6 Pa), and continuous sampling was achieved through a fused silica capillary (ID = 50 μm).

[0221] 7. Intelligent control software

[0222] Position relationship: Runs on an industrial-grade industrial computer (IP67 protection) and interacts with hardware via the EtherCAT bus;

[0223] Working principle:

[0224] AI optimization experiment: Based on the Bayesian optimization algorithm, with product yield / purity as the objective function, 4 Automatically search for optimal conditions (temperature / pressure / flow rate combination) within the level parameter space, and the learning efficiency is 50 times higher than the grid method.

[0225] Safety protocol: In radioactive experiment mode, the software forcibly enables triple redundant sensor calibration, and waste disposal reports are automatically embedded in the IAEA standard format, including nuclide activity, half-life, and packaging code.

[0226] Data interconnection: Synchronize experimental data (including raw spectra and video streams) to LIMS via the OPC UA protocol, supporting SQL queries and SPC statistical analysis.

[0227] This platform redefines the automation paradigm for high-risk chemical experiments through the integration of precision mechatronics design and AIoT, providing disruptive tools for fields such as pharmaceuticals and energy materials.

[0228] The working principle of the platform of the present invention:

[0229] The pumping system delivers two phases of reagents according to a program. After ultrasonic mixing, they enter the microfluidic channel and react under extreme conditions (500°C / 100 MPa). The online detection module captures spectra and microscopic images in real time, and the data is fed back to the control system for dynamic parameter adjustment. After the reaction is completed, the product is hermetically transferred through the sample receiving system, and the cleaning system automatically flushes away residuals and verifies cleanliness through XRF. The software integrates machine learning and security protocols to achieve closed-loop control of the entire experimental process, multimodal data visualization, and compliance report generation.

[0230] In summary, the present invention achieves safe, efficient, and precise operation under hazardous experimental conditions through automated and intelligent system design; it integrates multiple online detection methods and intelligent control software, which can monitor and adjust experimental parameters in real time, optimize reaction conditions, and improve experimental efficiency and reliability of results; it greatly reduces the safety risks of laboratory personnel, improves experimental efficiency and data quality, and promotes the development of the field of hazardous experiments.

[0231] The above description is merely a preferred embodiment of the present invention and does not limit the technical scope of the present invention. Therefore, any minor modifications, equivalent changes and modifications made to the above embodiments based on the technical essence of the present invention are still within the scope of the technical solution of the present invention.

Claims

1. A fully automatic intrinsically safe experimental robot platform based on microfluidic technology, characterized by: include: Automatic pumping sampling system, microchip reactor, automatic sample receiving system, automatic cleaning system, precise control system, multifunctional online detection system, intelligent control software; among them, Automatic pumping injection system: used to accurately and automatically pump reagents and samples into the microchip reactor; Microchip reactor: It has a micron-scale channel structure, which is used to achieve fast and uniform chemical reactions and easy to control reaction conditions; Automatic sampling system: used to automatically collect reaction products, avoiding safety risks caused by manual operation; Automatic cleaning system: used to automatically clean the microchip reactor and pipelines after the experiment to prevent reagent residue; Precision control system: used for real-time monitoring and adjustment of temperature, pressure, flow rate, and residence time parameters to achieve precise control of chemical reaction conditions; Multifunctional online detection system: Integrates microscope observation, online pH value, potential, fluorescence, and laser Raman detection methods to monitor key parameters and product characteristics during the reaction in real time; Intelligent control software: used to realize automatic control, parameter optimization and data analysis of the entire experimental process through programming; The robotic platform is centered around the microchip reactor, with its front end connected to the automatic pumping and sampling system via a corrosion-resistant pipeline, and its rear end connected to the automatic sampling system via a pressure-adaptive valve. The embedded units of the precision control system are distributed in each hardware module, and the central processing unit is located in an explosion-proof cabinet at the rear of the platform, which regulates temperature, pressure, and flow rate in real time. The multifunctional online detection system is arranged around the microchannel and coupled to the channel through an optical window. The automatic cleaning system is located at the bottom of the platform and is connected to the reactor and pipeline loop through a multi-way valve group. The intelligent control software runs on an industrial computer, integrates all subsystem data through the EtherCAT bus, and drives the AI ​​optimization algorithm and safety protocol.

2. The fully automatic intrinsically safe experimental robot platform based on microfluidic technology according to claim 1 is characterized in that: The automatic pumping injection system consists of a high-precision syringe pump, corrosion-resistant piping and leak-proof sealing valves, supports multi-channel reagent synchronous delivery, and has a flow rate range of 0.1-100mL / min; The microchip reactor has a built-in microfluidic structure, can withstand temperatures of -50°C to 200°C, pressures of 0.1-20 MPa, and a surface roughness of ≤0.1 μm; The automatic sample collection system integrates a pressure-adaptive valve and a sealed collection container to support the safe transfer of high-temperature, radioactive or toxic products; The automatic cleaning system is equipped with a multi-stage cleaning module, with a cleaning efficiency of ≥99.9% and a residual detection limit of ≤1ppm; The precise control system monitors and adjusts temperature, pressure, and flow rate in real time, and has built-in multi-level safety thresholds. When the pressure is greater than 10MPa, the speed is reduced, and when it is greater than 20MPa, an emergency shutdown is performed. The multifunctional online detection system synchronously integrates a high-speed camera, a microscope, an online Raman spectrometer, a pH / potential sensor, and a fluorescence detection module, and the data fusion analysis error is ≤1%; The intelligent control software is based on an automatic parameter optimization model using a machine learning algorithm, supports experimental program programming, multimodal data visualization, and security log generation, and has ISO 13849-1 certified fault self-diagnosis capabilities.

3. The fully automatic intrinsically safe experimental robot platform based on microfluidic technology according to claim 2 is characterized in that: The accuracy of the high-precision injection pump is ±0.1μL, and the material of the corrosion-resistant pipeline is PTFE or titanium alloy; the microchip reactor is made of glass, resin, silicon carbide ceramic or sapphire, and the channel width of the built-in microfluidic structure is 50-500μm, with an aspect ratio of ≥5:1; the response time of the integrated pressure adaptive valve is ≤10ms; the multi-stage cleaning module is acid / alkali / solvent cleaning liquid switching; the precise control system monitors and adjusts the temperature ±0.1℃, pressure ±0.01MPa, and flow rate ±0.5% of the set value in real time; the resolution of the high-temperature and high-pressure microscope is ≤1μm, the detection limit of the online Raman spectrometer is 0.1mol / L, the accuracy of the pH / potential sensor is ±0.01, and the excitation wavelength of the fluorescence detection module is 200-900nm.

4. The fully automatic intrinsically safe experimental robot platform based on microfluidic technology according to claim 1 is characterized in that: The microchip reactor can be modularly replaced to adapt to different experimental scenarios, including high-temperature synthesis and nanomaterial preparation. The interface is standardized to support rapid installation and sealing detection with a leakage rate of <0.1μL / min.

5. The fully automatic intrinsically safe experimental robot platform based on microfluidic technology according to claim 1 is characterized in that: The automatic pumping injection system is equipped with an ultrasonic mixer to achieve instantaneous and uniform mixing of reagents in the microchannel, with a mixing time of ≤10ms.

6. The fully automatic intrinsically safe experimental robot platform based on microfluidic technology according to claim 5 is characterized in that: The frequency of the ultrasonic mixer is 20-40 kHz.

7. The fully automatic intrinsically safe experimental robot platform based on microfluidic technology according to claim 1 is characterized in that: The multifunctional online detection system supports plug-and-play detection modules, including an expandable mass spectrometry interface and a dynamic light scattering (DLS) particle size analysis module with a range of 1-1000nm. The electromagnetic compatibility between modules meets the IEC 61000 standard, with crosstalk ≤-60dB.

8. The fully automatic intrinsically safe experimental robot platform based on microfluidic technology according to claim 1 is characterized in that: The platform uses a lead shielding layer and a negative pressure isolation cavity design to ensure that the radiation leakage rate of radioactive experiments is less than 0.1μSv / h and the toxic gas leakage concentration is less than 1ppm, which meets OSHA standards.

9. The fully automatic intrinsically safe experimental robot platform based on microfluidic technology according to claim 1 is characterized in that: The thickness of the lead shielding layer is ≥2 mm.

Images