Intelligent management platform for catalyst synthesis and control method thereof

Abstract

The invention discloses a catalyst synthesis intelligent management platform and a control method thereof, and relates to the technical field of catalyst synthesis intelligent management, and the platform comprises a catalyst pretreatment automation system which is used for carrying out the storage, transfer and split charging of a catalyst sample, carrying out the automatic control of catalyst reaction equipment, and determining the pretreatment information of the catalyst sample; the preprocessing information comprises storage, transfer, split charging and catalyst reaction information; the catalyst characterization automation system is used for collecting characterization data in real time and monitoring the characterization data in real time through butt joint of central control software and each piece of automation characterization equipment; the automatic catalyst reaction evaluation system is used for introducing an automatic high-temperature reaction kettle reaction system and screening out a catalyst meeting expected performance requirements, and the intelligent management platform for catalyst synthesis integrates automatic synthesis, high-precision characterization and efficient evaluation.

Description

Technical Field

[0001] This application relates to the technical field of intelligent management of catalyst synthesis, and particularly to an intelligent management platform for catalyst synthesis and its control method. Background Art

[0002] With the rapid development of new materials and new energy technologies, catalyst and material synthesis, as an indispensable part of industrial chemical reactions, the efficiency of its research and development and evaluation directly affects the commercialization process of new technologies.

[0003] The traditional processes of catalyst preparation, characterization, and evaluation have exposed obvious shortcomings. In the preparation process, it is difficult to accurately control key parameters such as raw material ratio and synthesis temperature by manual operation, which not only leads to poor batch stability of products but also consumes a large amount of labor and time costs. During the characterization process, numerous analytical instruments operate independently, and data collection is scattered. Researchers need to spend a lot of energy integrating data and are prone to human errors. In the evaluation stage, relying on manual recording of experimental results and comparative analysis of performance, the efficiency is extremely low, and it is difficult to quickly screen out high-performance catalysts. Aiming at the problems existing in traditional catalyst R & D laboratories, such as cumbersome operation processes, insufficient experimental accuracy, chaotic data management, difficult interdisciplinary cooperation, and slow commercialization of scientific research results, and being difficult to meet the requirements of modern catalyst R & D for efficient, precise, and intelligent management, in order to improve the efficiency and quality of catalyst and material research, realize the digital and intelligent development needs in the field of catalyst synthesis, and build a leading catalyst synthesis and characterization intelligent laboratory in the industry, a design and planning of the central laboratory is carried out, and there is an urgent need for an intelligent management platform for catalyst synthesis that integrates automated synthesis, high-precision characterization, and efficient evaluation. Summary of the Invention

[0004] The purpose of this application is to provide an intelligent management platform for catalyst synthesis and its control method, which integrates automated synthesis, high-precision characterization, and efficient evaluation, and can improve the R & D efficiency and enhance the experimental accuracy.

[0005] To achieve the above purpose, this application provides the following solutions:

[0006] In the first aspect, this application provides an intelligent management platform for catalyst synthesis, including:

[0007] An automated catalyst pretreatment system for automatically controlling the storage, transfer, sub-packaging, and catalyst reaction equipment of catalyst samples, and determining the pretreatment information of catalyst samples; the pretreatment information includes storage, transfer, sub-packaging, and catalyst reaction information;

[0008] An automated catalyst characterization system for docking with each automated characterization device through the central control software to collect characterization data in real time and monitor the characterization data in real time;

[0009] A catalyst reaction evaluation automation system is used to introduce an automated high-temperature reactor reaction system to screen out catalysts that meet the expected performance requirements.

[0010] In a second aspect, the present application provides a control method for the catalyst synthesis intelligent management platform described in the first aspect, including:

[0011] Automatically control the storage, transfer, sub-packaging, and catalyst reaction equipment of catalyst samples using the catalyst pretreatment automation system to determine the pretreatment information of the catalyst samples; the pretreatment information includes storage, transfer, sub-packaging, and catalyst reaction information;

[0012] Use the catalyst characterization automation system to connect with each automated characterization device through the central control software to collect characterization data in real time and monitor the characterization data in real time;

[0013] Use the catalyst reaction evaluation automation system to screen out catalysts that meet the expected performance requirements.

[0014] According to the specific embodiments provided by the present application, the following technical effects are disclosed:

[0015] The present application provides a catalyst synthesis intelligent management platform and its control method. Through the catalyst pretreatment automation system, the sample storage, sample transfer, sample sub-packaging, and catalyst reaction equipment are automatically controlled, and the processes of sample warehousing, storage, retrieval, use, and return are managed; the catalyst characterization automation system connects with each automated characterization device through the central control software to collect characterization data in real time and monitor the characterization data in real time; an automated high-temperature reactor reaction system is introduced to screen out catalysts that meet the expected performance requirements, providing a catalyst synthesis intelligent management platform integrating automated synthesis, high-precision characterization, and efficient evaluation, and solving the problems existing in traditional catalyst R & D laboratories, such as cumbersome operation processes, insufficient experimental accuracy, chaotic data management, difficult interdisciplinary cooperation, and slow commercialization of scientific research results, which are difficult to meet the requirements of modern catalyst R & D for efficient, precise, and intelligent management. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] In order to more clearly illustrate the technical solutions in the embodiments of the present application or the prior art, the following will briefly introduce the drawings required for use in the embodiments. Obviously, the drawings in the following description are only some embodiments of the present application. For those of ordinary skill in the art, other drawings can be obtained based on these drawings without creative efforts.

[0017] Figure 1 It is a block diagram of a catalyst synthesis intelligent management platform provided in Embodiment 1 of the present application;

[0018] Figure 2 Schematic architecture diagram of an intelligent management platform for catalyst synthesis provided in Embodiment 1 of this application;

[0019] Figure 3 Schematic flowchart of a control method for an intelligent management platform for catalyst synthesis provided in Embodiment 2 of this application. Detailed implementation manners

[0020] Next, the technical solutions in the embodiments of this application will be clearly and completely described in conjunction with the accompanying drawings in the embodiments of this application. Obviously, the described embodiments are only a part rather than all of the embodiments of this application. All other embodiments obtained by those of ordinary skill in the art based on the embodiments in this application without creative efforts shall fall within the protection scope of this application.

[0021] To make the above objectives, features, and advantages of this application more obvious and understandable, the following provides a more detailed description of this application in conjunction with the accompanying drawings and specific implementation manners.

[0022] Embodiment 1

[0023] As Figure 1 shown, this embodiment provides an intelligent management platform for catalyst synthesis, including: an automated catalyst pretreatment system, an automated catalyst characterization system, and an automated catalyst reaction evaluation system.

[0024] After preparing a catalyst sample through the automated catalyst preparation system in this application, subsequent processing is performed through the automated catalyst pretreatment system, the automated catalyst characterization system, and the automated catalyst reaction evaluation system.

[0025] The automated catalyst pretreatment system is used to automatically control the storage, transfer, sub-packaging, and catalyst reaction equipment of the catalyst sample, and determine the pretreatment information of the catalyst sample; the pretreatment information includes storage, transfer, sub-packaging, and catalyst reaction information. The catalyst reaction equipment includes a muffle furnace and an atmosphere furnace.

[0026] The automated catalyst characterization system is used to interface with each automated characterization device through the central control software to collect characterization data in real time and monitor the characterization data in real time.

[0027] The automated catalyst reaction evaluation system is used to introduce an automated high-temperature reaction kettle reaction system to screen out catalysts that meet the expected performance requirements.

[0028] The intelligent management platform for catalyst synthesis includes a laboratory central control system (ImagicOS central control system), which is used to comprehensively manage the catalyst preparation automation system, catalyst pretreatment automation system, catalyst characterization automation system, and catalyst reaction evaluation automation system. The laboratory central control system mainly realizes functions such as equipment control, resource dashboard, experiment monitoring, project management, experimental process management, full-process information traceability, human-computer interaction, warehousing management, permission management, data analysis and processing, and intelligent expansion. This laboratory central control system needs to integrate the existing systems of each instrument manufacturer to form an end-to-end integrated software control.

[0029] To ensure that the future expansion needs of the laboratory can be met, the platform must have high scalability. The system design should reserve sufficient interfaces and modular design, so that new equipment and technologies can be easily integrated without disturbing the existing operations. In addition, the system architecture should support horizontal expansion to adapt to the increasing data processing and storage requirements brought by the growth of the laboratory scale. At the same time, the system should follow open standards and industry general protocols to ensure compatibility with future technologies and interoperability with other systems.

[0030] In addition, to support the forward-looking compatibility of AI models, when building this platform, the rapid development of cutting-edge technologies such as artificial intelligence and large models and future integration needs must be fully considered. Therefore, the system architecture should have forward-looking technical adaptability to ensure seamless integration of more advanced AI algorithms and computing models that will emerge in the future. Modular and open interfaces should be adopted in the design so that the system functions can be upgraded and expanded without interrupting the existing services. At the same time, the system should support flexible API integration and data exchange formats to ensure compatibility with emerging technologies, so that AI technologies such as machine learning and deep learning can be efficiently integrated in subsequent development, maintaining the technical leading position of the laboratory platform in the field of catalyst research and development.

[0031] The architecture of the intelligent management platform for catalyst synthesis is as Figure 2 shown.

[0032] (1) Catalyst pretreatment automation system: It includes sample storage, sample transfer, sample sub-packaging, automated muffle furnace, and automated atmosphere furnace, which can realize intelligent and digital management of samples, intelligent sub-packaging, and automated transfer to each automated platform.

[0033] The catalyst pretreatment automation system includes a sample storage management system, an automated solid powder sub-packaging system, and a sample calcination functional island.

[0034] 1. Main functions of the sample storage management system: Connect with the background database through an intelligent software system to achieve functions such as intelligent access, automatic inventory, and real-time monitoring of samples or consumables; all item in-and-out and in-stock situations can be queried at any time to realize intelligent inventory management and improve work efficiency.

[0035] This sample storage management system has the following advantages: Diversified storage: It can store various specifications of consumables, including but not limited to reagent bottles, sample bottles, etc.; Maintainability and cleanliness: Made of corrosion-resistant stainless steel, modular design, easy to clean and maintain; Fast sampling: The average sampling time < 20s; Easy to operate: It can be configured with a touch screen, with a friendly interface to achieve user-friendly interaction; Automatic barcode scanning function: Operations are recorded in real time and information can be traced; Easy expandability: Compatible with subsequent laboratory automation equipment integration; The weighing record of samples can be realized.

[0036] The working process of the sample storage management system includes: warehousing, sampling, returning samples, outbound, returning to the warehouse, and decoding. The sample storage management system includes: a three-dimensional storage rack for storing sample master tubes; a transfer rack for temporarily storing and transferring sample master tubes; a screen for displaying the sample management UI interface, presenting sample information, and operating the in-and-out and sample entry processes; a manual barcode scanner for manually scanning sample racks and sample tubes to complete the in-and-out and sample entry operations; two automatic barcode scanners, one for the robotic arm in the three-dimensional warehouse work area to automatically scan sample racks, and the other for the robotic arm operation in the sorting work area to scan the dispensing rack and the selected sample tubes; a weighing balance, to the thousandth place, for weighing and recording the in-and-out and newly entered sample tubes in the sorting and selection work area; an interaction position, an Automated Guided Vehicle (AGV, also known as a collaborative robot) and a human interaction position with the storage station for picking up, placing, and entering samples, and can place sample tube transfer racks and sample tube storage racks. The number of sample master tubes needs to be set in advance, and empty codes are assigned to the sample master tubes and pallet racks in advance.

[0037] (1) Storage: (When newly manufactured samples or raw materials are first stored in the sample storage functional island): Manually place the sample bottles to be stored on the empty sample bottle rack; Manually log in to the system and manually enter the sample information form; Manually place the sample bottle rack at the transfer position and prompt the system to start storage; Control the secondary robotic arm of the AGV to grab the sample bottle rack for scanning to obtain information related to the sample bottle rack and the corresponding sample bottles at the position; Control the secondary robotic arm to grab the sample bottles for scanning and transfer them to the balance for weighing, and the quality data is automatically generated in the sample information form, as shown in Table 1; After all sample bottles are weighed, control the secondary robotic arm to grab the sample bottle rack and transfer it to the first designated position A on the guide rail; The guide rail moves the sample bottle rack to the second designated position B, and control the main robotic arm of the AGV to grab the sample bottle rack and transfer it to the storage rack for storage. The system automatically updates the corresponding position information of the storage rack and the sample bottle rack, and the storage is completed. The guide rail is used to convey the sample bottle rack to the designated position.

[0038] Table 1 Sample Information Form

[0039]

[0040] (2) Sampling (Retrieving stored samples or raw materials): Manually log in to the system and initiate a sampling application; Control the main robotic arm to grab the target sample rack on the storage rack and place it at the second designated position B, and at the same time control the secondary robotic arm to grab the empty sample bottle rack and transfer it to the transfer position; The guide rail transfers the target sample rack to the first designated position A; The secondary robotic arm picks the target sample bottles at A and transfers them to the empty sample bottle rack at the transfer position; The system feeds back instructions (0 indicates that all sample picking is completed; 1 indicates that the main robotic arm needs to transfer from the storage rack to other target sample racks); After all sample picking is completed, control the main robotic arm to retrieve the sample bottle rack on the guide rail back to the storage rack for resetting and update the storage rack information; At the same time, control the secondary robotic arm to grab the sample bottle rack at the transfer position for scanning, and grab the sample bottles in the rack one by one for scanning and weighing to generate a sample information outbound form; Manually take away the sample bottle rack from the transfer position, and the manual sampling is completed.

[0041] (3) Returning Samples (Returning the taken samples or raw materials to the sample storage functional island): Manually log in to the system and initiate a sample return application; Manually place the sample bottle rack at the transfer position, and the system receives the return instruction and starts the return process; Control the secondary robotic arm to scan the sample bottle rack at the transfer position to obtain information related to the sample bottle rack and the corresponding sample bottles; Control the secondary robotic arm to grab the sample bottles, scan them, and transfer them to the balance for weighing, and the quality data is automatically updated in the sample information form; At the same time, control the main robotic arm to grab the sample bottle rack on the storage rack and transfer it to the first designated position A through the guide rail; Control the secondary robotic arm to transfer the sample bottles to the sample bottle rack at the first designated position A; The guide rail moves the sample bottle rack to the second designated position B, and the main robotic arm grabs the sample bottle rack and transfers it to the storage rack for storage; Control the secondary robotic arm to transfer the empty sample bottle rack at the transfer position to the empty rack.

[0042] (4) Outbound (when the sample or raw material is consumed or below the set minimum storage quantity, select and retrieve, unbind and update the storage island database): When the system receives the outbound instruction, it starts the outbound process; control the main robotic arm to grab the target sample rack on the storage rack and place it at the second designated position B on the guide rail. At the same time, the secondary robotic arm grabs the empty sample bottle rack and transfers it to the transfer position; the guide rail transfers the target sample rack to the first designated position A; the secondary robotic arm picks the target sample bottle at the first designated position A and transfers it to the empty sample bottle rack at the transfer position; the system feeds back the instruction (0 indicates that all samples have been picked, 1 indicates that the main robotic arm needs to transfer other target sample racks from the storage rack); after all samples have been picked, control the main robotic arm to retrieve the sample bottle rack on the guide rail back to the storage rack for reset and update the storage rack information; at the same time, the secondary robotic arm grabs the sample bottle rack at the transfer position for scanning the code, and grabs the sample bottles in the rack one by one for scanning and weighing to generate the sample information outbound form; the AGV picks up the sample bottle rack from the transfer position.

[0043] (5) Return to the warehouse: When the system receives the return to the warehouse instruction, it starts the return process; the secondary robotic arm scans the code of the sample bottle rack at the transfer position to obtain the relevant information of the sample bottle rack and the corresponding sample bottles; the secondary robotic arm grabs the sample bottles, scans the code, and transfers them to the balance for weighing, and the quality data is automatically updated in the sample information table; at the same time, control the main robotic arm to grab the sample bottle rack on the storage rack and transfer it to the first designated position A through the guide rail; the secondary robotic arm transfers the sample bottles to the sample bottle rack at the first designated position A; the guide rail moves the sample bottle rack to the second designated position B, control the main robotic arm to grab the sample bottle rack and transfer it to the storage rack for storage; the secondary robotic arm transfers the empty sample bottle rack at the transfer position to the empty material rack.

[0044] (6) Decoding (unbind the QR code): When the sample is used up or the storage quantity of the sample is below the set value, manually delete the QR code information through the barcode scanner. It is also possible to scan the QR code information of the sample through a handheld computer (Personal Digital Assistant, PDA) or a tablet computer (PAD) to unbind the QR code and delete the QR code information of the sample.

[0045] 2. Main functions of the automated solid powder dispensing system: Complete the weighing of samples with specified weights. The automated sample weighing module, including a linear vibrator, an oscillation buffer, an oscillation base, and a weighing balance, adopts an electromagnetic vibration form. According to different samples, the accuracy of sample delivery volume is controlled through the oscillation frequency, oscillator voltage control, and programming algorithm. In addition, the weighing balance is equipped with a multi-stage shock absorption platform, which can effectively eliminate slight vibrations. The automated solid powder dispensing system can cooperate with the mobile AGV to achieve the dispensing and transfer of samples.

[0046] Balance accuracy (full range / fine range): 0.1 mg; Applicable range (full range / fine range): 220 g; Balance linear error: ≤0.4 mg; Repeatability: 0.2 mg; Stabilization time: 2 s. Cover opening method: Rotating cover opening method; Weighing calibration: With automatic calibration function for weights, and upload calibration data, and operate after passing the qualification; Weighing speed: The speed of weighing one sample is <3 min; Software interface of the automated solid powder dispensing system: The automated solid powder dispensing system can also visualize the sample parameter information, and through the software interface, the sample positions on the operation table can be intuitively viewed, meeting the functions of selecting the sample weighing container according to the project category, editing the weighed amount, and editing key parameters such as the sample weighing mode; It has an automatic cover opening and closing function, and can open and close the sample bottle and the secondary bottle.

[0047] Each device of the automated sample weighing module is equipped with an interface for independent communication, and can cooperate with a collaborative robot to complete automatic sample picking and placing; It can perform mid-course sample insertion and operations such as raising the work priority. Identification and code assignment transfer of the sample to be weighed: The device is equipped with a barcode recognition component, which facilitates the transfer and information transmission of the sample after the sample unpacking and dispensing main pipe; The weighing data can be automatically uploaded to the system, and the real-time conveying quality of the sample can be obtained. It has high safety: The human-machine interaction system is equipped with safety protection measures and alarm prompts, and has an anti-static function; In terms of data security, it is required that the data be automatically stored locally, with a permission viewing function, and the data is traceable; In terms of sample inspection safety, a weighing operation monitoring program is set up and a whistle warning is given when an abnormal situation occurs during weighing. The equipment operation noise requirement is less than 55 dB; The equipment is equipped with overload protection and leakage protection devices. When the equipment malfunctions or fails, necessary protection measures are provided to ensure that the equipment and products are still in a safe state. The equipment is provided with an emergency stop switch, and the emergency stop switch should be set in an easy-to-operate position; When the equipment is in the running state, pressing the emergency stop switch will immediately stop the equipment; After the emergency stop switch is reset, the equipment can only enter the running state after performing the reset and start operations.

[0048] The catalyst pretreatment automation system includes an automated sample weighing module. The automated sample weighing module is used to determine the real-time conveying quality of the sample in the form of electromagnetic vibration.

[0049] The working process of the automated solid powder dispensing system includes consumable warehousing, consumable rack outbound, consumable rack inbound, and dispensing.

[0050] (1) Consumable warehousing (into the main pipe rack): Manually put the cleaned consumables on the consumable rack and place them on the main pipe rack; Manually log in to the system and enter the corresponding position information of the consumable number and the consumable rack (such as the 20th quartz crucible is placed at the 1st position on the 1st B1 crucible rack).

[0051] (2) Consumable Rack Outbound (Out of the Main Pipe Rack): The AGV robotic arm grabs the target consumable rack and scans the code for outbound; after all consumable racks are out of the warehouse, the system updates the information of the main pipe rack; meanwhile, the AGV cart transfers the consumable rack to the transfer position of the functional island (such as sample sub-packaging, physical and chemical adsorption, XRF testing, etc.).

[0052] (3) Consumable Rack Inbound (Into the Sub-Pipe Rack): The five-axis robotic arm grabs the consumable rack at the transfer position, scans the code, and transfers it to the sub-pipe rack; after all consumable racks are in the warehouse, the system updates the information of the sub-pipe rack and the consumable rack.

[0053] (4) Sub-packaging: The AGV cart transfers the sample bottle rack that needs sample sub-packaging to the transfer position; the five-axis robotic arm grabs the sample bottle rack, scans the code to obtain the task information; the five-axis robotic arm grabs the sample bottle, scans the code, and transfers it to the switch cover module to open the lid; after opening the lid, it is transferred to the jitter weighing device (balance dumping position); the five-axis robotic arm grabs the target consumable rack from the sub-pipe rack according to the task information, scans the code and transfers it to the transfer position; the five-axis robotic arm sequentially grabs the consumables (such as quartz crucibles) to the balance weighing position; after the balance returns to zero, it starts jitter weighing; after weighing is completed, the five-axis robotic arm grabs the consumables to the original position of the consumable rack, and the system generates a sub-packaging information form; the five-axis robotic arm transfers the sample bottle on the jitter weighing device to the switch cover module to close the lid; after closing the lid, it is transferred to the original position of the sample bottle rack; repeat the above operations until all sample sub-packaging is completed.

[0054] 3. The sample roasting functional island includes an atmosphere furnace and a muffle furnace. The main functions of the sample roasting functional island are: it can be equipped with an automated robotic arm or a mobile AGV to achieve all-weather and uninterrupted high-throughput sample sintering; an automatically loaded high-temperature furnace can maintain good temperature field uniformity, and the samples are loaded and unloaded electrically or pneumatically, which is convenient for loading and unloading materials; the equipment has an interface with independent communication, which can cooperate with a collaborative robot to complete automatic sample placement, automatic furnace door closing, automatic heating, constant temperature, and cooling, automatically open and take out the samples, and can perform multiple cycle operations. Multiple devices work together with a robotic hand (robotic arm) to truly achieve all-weather and uninterrupted high-throughput sample sintering. Its rated working temperature is not lower than 100°C. The atmosphere furnace and the muffle furnace have the advantages of uniform temperature field, low surface temperature, and long on-line life.

[0055] Muffle furnace: It has a large interface operating system that is simple and easy to understand, comprehensively displaying the status of multiple temperature zones; one-key start / stop, with functions of automatic recording and preset process heating curves; it can pre-store custom formula processes for calling at any time, has a USB interface to read recording curves; is reserved with a communication interface, can be connected to a PC or a wireless router to achieve remote control; opens the communication protocol to existing customers to connect the device with a collaborative robot for unmanned operation; is equipped with an automatic temperature control system; can be intelligently programmable to control the constant temperature with a control accuracy of ±1°C, that is, the difference between the real-time temperature and the target temperature of the muffle furnace is within the constant temperature control accuracy range; the sample stage is made of refractory materials; the maximum working temperature: not less than 1600°C; can be coordinated with a collaborative robot. A ventilation fan is reserved above the muffle furnace.

[0056] Atmosphere furnace: The maximum temperature is 1200°C (less than 0.5 hours); the continuous working temperature is not less than 1000°C; the heating zone length: 300mm, the constant temperature zone length: 100mm (+ / -5°C); the maximum heating rate: ≤20°C / min; PID automatic temperature control system (Eurotherm 3008p high-precision instrument); intelligently programmable to control the temperature with a preset temperature control accuracy range of ±1°C, so that the difference between the real-time temperature and the target temperature of the atmosphere furnace is within the constant temperature control accuracy range; equipped with a PC communication connection port; the sample stage bracket has a position for the collaborative robot to grab. The gas demand of the atmosphere furnace: set according to user needs, for example, it can be set as: one-way air, one-way hydrogen, one-way nitrogen, with self-provided gas source and secondary pressure reducing valve, and the outlet of the pressure reducing valve is connected to a 1 / 4 pipe. A ventilation fan is reserved above the atmosphere furnace

[0057] The working process of the sample roasting function island is as follows: (1) Roasting: The AGV cart transports the crucible rack to the transfer position of the roasting function island; the corresponding equipment automatically opens the door, and the corresponding equipment refers to the atmosphere furnace and the muffle furnace; the AGV robotic arm grabs the crucible and places it at the corresponding position of the equipment; after all crucibles are placed, the equipment automatically closes the door and performs automatic operations according to the roasting conditions; Sampling after roasting: After roasting, when the equipment cools down to room temperature (target temperature), the equipment automatically opens the door; the AGV cart receives the instruction and transfers to the corresponding position of the roasting function island; the AGV robotic arm grabs the crucible and places it back at the corresponding position of the crucible rack on the transfer position; after all crucibles are grabbed, the AGV cart transfers the crucible rack to other function islands for the next operation; at the same time, the equipment automatically closes the door.

[0058] The catalyst pretreatment automation system includes an automatic temperature control module, which is used to collect the reaction temperature during the sample roasting process of the atmosphere furnace and the muffle furnace to obtain the real-time temperature, and automatically control the real-time temperature so that the difference between the real-time temperature and the target temperature is within the preset temperature control accuracy range.

[0059] (II) Catalyst characterization automation system, including automated Raman spectroscopy analysis subsystem, automated inductively coupled plasma optical emission spectroscopy subsystem (ICP-OES), automated X-ray diffraction analysis subsystem (XRD), automated X-ray fluorescence analysis subsystem (XRF), automated physical and chemical adsorption subsystem, and automated infrared analysis subsystem. The control software is connected to each automated characterization equipment, and the automatic control and data acquisition are monitored in real time, realizing automated control and real-time monitoring of catalysts as well as data collection and upload.

[0060] (1) Automated Raman spectroscopy analysis subsystem, used to: obtain spectral data of catalyst samples; determine the type of chemical substance in the catalyst samples based on the spectral data of the catalyst samples. It includes a Raman spectrometer and a nanolaser, and can use a DXR3 Raman spectrometer. The automated Raman spectroscopy analysis subsystem integrates automation, intelligence and precise analysis. It uses the principle of Raman scattering to instantly capture the "spectral fingerprint" of the catalyst sample, accurately and qualitatively identify chemical substances and various materials, and is committed to providing repeatable and high-precision experimental results with reliable performance and easy maintenance.

[0061] The technical parameters are set as follows: spectral resolution <2cm(-1); spectral repeatability is better than ±0.2cm(-1); the software automatically aligns all optical paths: automatically aligns the laser excitation optical path to the sample point that coincides with the optical axis to achieve optical path coaxiality and energy optimization. All alignments do not require opening the optical table or manual alignment; automatic exposure and acquisition function, no need to explore experimental conditions, you can get the best Raman spectrum information; it has an automatic fluorescence background subtraction function; to avoid spectral deformation and distortion, there is no need to use the laser micro-difference method of subtracting the fluorescence background by changing the laser output frequency to perform a difference spectrum on the Raman spectrum; to ensure the wavelength accuracy and precision of long-term spectrum acquisition or Raman imaging, real-time X-axis calibration is used: Acquisition spectrum Real-time calibration can be performed during the Raman imaging process, without the need for an external calibration source or manual operation; automatic noise background removal; fully automatic calibration system: built-in standard white light source, the software automatically calibrates the vertical coordinate Raman light intensity; built-in neon atomic line, the software can automatically run the entire spectrum wavenumber calibration; all calibrations are completely manual and can be completed with a click of the mouse; Raman spectroscopy software includes various advanced functions such as instrument control, data acquisition, spectrum processing and curve fitting; universal sampling table accessories: the software automatically identifies and reports the serial number, easily switches between different sample accessories, accurately locates, and can be replaced with other accessories without shutting down; flat universal sample holder, detects different forms of samples such as plastic bags or glass bottles.

[0062] The workflow is as follows: 1) Power on / off: There is a physical button. It is recommended to power on and off manually, once at the start and end of each day's experiment (the instrument needs to be preheated for 20 minutes before testing). 2) Automated testing: The AGV cart transports the sample vial rack containing the Raman samples to be tested to the transfer position of the Raman spectroscopy functional island; the AGV robotic arm sequentially grabs the sample vials and places them on the sampling platform; the Raman spectrometer conducts automated testing; after the testing is completed, the AGV robotic arm places the sample vials back on the sample vial rack at the transfer position; the AGV robotic arm grabs the next sample vial until all samples are tested; after all samples are tested, the AGV cart transfers the consumable rack to other functional islands for the next operation.

[0063] (2) The automated inductively coupled plasma optical emission spectrometry subsystem is used for: using the high-temperature excitation source generated by inductively coupled plasma to atomize and excite the catalyst sample to obtain the wavelengths and intensities of the characteristic spectral lines of the detected elements in the catalyst sample; determining the types of the detected elements based on the wavelengths and intensities of the characteristic spectral lines of the detected elements; and determining the contents of the detected elements in the catalyst sample according to the quantitative relationship between the intensities of the characteristic spectral lines of the detected elements and the element concentrations.

[0064] Main functions: The automated inductively coupled plasma optical emission spectrometry subsystem realizes the full-process automation of sample loading and unloading, acid addition, lid opening and closing, heating, acid expulsion, volume fixing, mixing, automatic sample injection, automatic analysis, and automatic uploading of analysis data. It combines the automatic digestion technology with the ICP-OES analysis method, uses the high-temperature excitation source generated by inductively coupled plasma to atomize and excite the catalyst sample, accurately determines the element types by detecting the wavelengths and intensities of the characteristic spectral lines of the elements, and precisely calculates the contents of each element according to the quantitative relationship between the spectral line intensities and the element concentrations, providing key data support for many fields such as material composition analysis, environmental monitoring, and geological exploration.

[0065] The automated inductively coupled plasma optical emission spectrometry subsystem has the following performance advantages:

[0066] ① Self-excited all-solid-state RF power supply: The self-excited all-solid-state RF power supply, with full digital control, continuously adjustable power, has stronger sample adaptability; the classic water-cooled design enables rapid heat dissipation while ensuring excellent stability and reliability of the power supply;

[0067] ② New generation vertical torch bidirectional observation technology: Axial observation obtains high sensitivity, radial observation avoids matrix interference, the vertical torch design can avoid high-salt deposition, extend the service life of the torch, and at the same time reduce the argon consumption, lowering the instrument usage cost;

[0068] ③ Stable sampling system: Multiple digital mass flow controllers precisely control each path of argon gas to ensure the stability of measurement data; High-precision multi-channel peristaltic pumps can support internal standard solutions, hydride generators, etc. according to requirements while ensuring stable sampling, which is beneficial for the analysis of complex samples; Removable torch tube, quick plug-and-play connection, self-collimating installation. For different applications, only the central tube needs to be replaced, greatly reducing the usage cost; Cold cone interface, without the consumption of cutting gas.

[0069] ④ Higher sensitivity and reliability: Adopt an echelle two-dimensional spectroscopic system. There are no moving parts in the entire optical system, and all optical elements are sealed in a constant temperature system at a temperature of 36 ± 0.1 °C; A CCD detector with millions of pixels and innovative back-illumination technology. There is no light conversion chemical coating on the surface of the detector, and the detector will not be damaged and replaced due to coating aging.

[0070] The automated inductively coupled plasma emission spectroscopy subsystem includes a fully automated super microwave chemical workstation, a rapid sampling system, and an inductively coupled plasma spectrometer.

[0071] 1) Fully automated super microwave chemical workstation, including a microwave digestion module, a fully automated acid addition module, a standard addition module, and a volume fixing module.

[0072] Microwave digestion module: Load inert gas in a closed reaction chamber and achieve efficient digestion of samples under ultra-high temperature and ultra-high pressure through microwave heating. All samples placed in the reaction chamber are digested at the same temperature and pressure. The microwave power is 1200W, the maximum temperature is 300 °C, the maximum working pressure is 20 Mpa, the volume of the reaction chamber is 1L, the number of chambers is 4, and the digestion throughput is 8 * 35 ml.

[0073] Fully automated acid addition module: Each peristaltic pump independently adds reagents. The wetted material is PTFE material, which can resist strong acids. The strong acid storage area is equipped with an air filter element and a one-way valve to effectively prevent impurities in the air from entering the reagent bottle and prevent acid leakage; It has a reagent volume detection system that gives an alarm prompt when the reagent remaining amount is insufficient and gives an alarm in time when the liquid level in the waste liquid tank reaches the dangerous level.

[0074] Standard addition module: Accurately add standards with a high-precision syringe pump. Add inert gas at 4 - 10 MPa to the chamber in advance to digest the sample under high pressure, with overpressure protection and automatic pressure relief; The microwave is enclosed in a metal chamber to avoid leakage.

[0075] Volume fixing module: Use an ultrasonic sensor to accurately fix the volume. The volume fixing accuracy is < 1% @ 50 ml; The volume fixing range is 5 ml - 50 ml. Anti-corrosion design: PTFE operation platform, all-PFA pipeline design.

[0076] 2) The rapid sampling system includes: Torch tube: A detachable torch tube with quick plug-and-play connection, and an optional sampling system resistant to high salts or HF; Peristaltic pump: A 12-roller, 4-channel peristaltic pump with a pump speed continuously adjustable from 0 to 125 rpm; The rapid sampling system has a rapid sampling function, enabling rapid sample extraction within one minute, reducing reagent consumption, having a shorter running time, and lower energy and argon consumption.

[0077] 3) The inductively coupled plasma spectrometer includes a detection unit: A CCD detector with ≥1 million pixels, single exposure; CCD imaging size: ≥24.5 mm × 24.5 mm; Pixel-level cooling: TEC cooling encapsulated inside the sensor, with a cooling temperature ≥ -15°C; There is no light-converting chemical coating on the detector surface, preventing detector damage and replacement due to coating aging; Constant temperature: ≤36°C, precision ±0.1°C; Focal length: ≤390 mm; Wavelength range: ≥165 - 850 nm, full wavelength coverage; Wavelength calibration: Each time the instrument is ignited, only the C, N, and Ar spectral lines are used for automatic spectral position correction without the need for a wavelength calibration solution; Full-spectrum real-time calibration technology: Using the interference-free neon characteristic spectral line to perform real-time correction on the fine spectral offset to ensure long-term stability; A self-excited all-solid-state radio frequency power supply with a power of ≥700 - 1350 W, continuously adjustable by 1 W, and a maximum of 1600 W; A vertical torch tube for bidirectional observation in the axial and radial directions; The linear dynamic range of the measured spectral line: ≥105 (measured with Mn257.6 nm, correlation coefficient ≥0.999); For the measurement of a 1 ppm or 10 ppm multi-element mixed standard solution, the RSD of repeated measurements ten times ≤ 0.5%; For the measurement of a 1 ppm or 10 ppm multi-element mixed standard solution, the long-term stability RSD for 4 hours ≤ 1%.

[0078] The working process of the automated inductively coupled plasma emission spectrometry subsystem specifically includes: 1) Manual preparation: Manually configure the standard solution mother liquor and place the mother liquor at the designated position before each test (the validity period of the mother liquor is 1 day); Manually clean the PTFE tank body in the digestion tank once a day / week. 2) Test process: The AGV cart transports the consumable rack (digestion tube) containing the ICP sample to be tested to the transfer position of the ICP-OES test function island; The robotic arm grabs the consumable rack (digestion tube) at the transfer position, scans the code, and then returns it to the transfer position; The microwave digestion module automatically opens the door, and the digestion tank automatically opens the lid; The robotic arm grabs the consumable rack at the transfer position and transfers it to the corresponding digestion tank; The digestion tank automatically closes the lid, and the microwave digestion module automatically closes the door; The fully automatic heavy metal analysis system (microwave digestion module, rapid sampling system, and ICP-OES) performs automated testing according to the preset parameters. 3) End of test: After the test is completed, the digestion tank in the microwave digestion module automatically opens the lid; After waiting for the acid mist in the cavity to be exhausted (set a fixed waiting time), the microwave digestion module has an automated door opening function; The robotic arm grabs the consumable rack in the digestion tank and transfers it to the transfer position; After all the consumable racks are transferred, the AGV cart grabs the consumable rack at the transfer position and transfers it to the transfer position of other function islands; At the same time, the digestion tank automatically closes the lid, and the microwave digestion module automatically closes the door.

[0079] (3) The automated X-ray diffraction analysis subsystem is used for: performing full-automatic X-ray diffraction analysis on catalyst samples to obtain the X-ray diffraction analysis results of the catalyst samples. For full-automatic X-ray diffraction analysis and characterization of materials such as catalysts. The equipment has an interface with independent communication, cooperates with the sample preparation equipment, and the collaborative robot completes automatic sample loading, automatic sample unloading, and can perform multiple cycle operations, record and transmit the analysis results, and cooperate with the robotic arm to achieve all-weather uninterrupted high-throughput sample detection.

[0080] The automated X-ray diffraction analysis subsystem includes an automated X-ray diffractometer, an AGV composite robot, a dedicated robotic arm, and an instrument control program. In cooperation with the intelligent laboratory software platform, it must achieve the following functions: It can achieve the AGV composite robot grabbing the sample cup and placing it on the sample stage of the automated X-ray diffractometer (X-ray diffractometer) or the reverse process, complete full-automatic operations such as automatic sample loading, automatic sample unloading, and automatic transfer, testing, and data transmission, minimize manual operations as much as possible, and improve the experimental efficiency.

[0081] Automatically control the tube voltage, tube current, light shutter, and ray tube aging training of the X-ray generator; Control the goniometer to perform continuous or step scanning while collecting diffraction data; Perform routine processing on the diffraction data: automatic peak searching, manual peak searching, integral intensity, peak height, centroid, background subtraction, smoothing, peak shape amplification, spectrum comparison, etc., to obtain the X-ray diffraction analysis results of the catalyst samples.

[0082] The workflow of the automated X-ray diffraction analysis subsystem specifically includes: 1) warehousing of consumable racks (into the tablet rack): the AGV cart delivers the consumable rack (sample table) and consumable rack (disposable funnel) to the transfer position of the XRD test function island; the robotic arm grabs the consumable rack at the transfer position, scans the code, and transfers it to the tablet rack; after all consumable racks are put into storage, the system updates the tablet rack and consumable rack information. 2) XRD automated testing: The AGV delivers the consumable rack containing the sample (cup) to the transfer position of the XRD test function island; at the same time, the robotic arm grabs the consumable rack (sample table) and the consumable rack (disposable funnel) on the tableting rack to the transfer position; the robotic arm grabs the consumable rack (sample table), consumable rack (disposable funnel) and consumable rack (sample cup) at the transfer position, scans the code and puts them back to the transfer position; the robotic arm grabs the sample table in sequence at the transfer position and transfers it to the sample loading position of the tableting device; the robotic arm grabs the disposable funnel and fixes it just above the sample loading position; the robotic arm grabs the sample cup in sequence, moves it to the funnel position and flips it over Sample, the sample is transferred to the sample table through the funnel, and an information table is automatically generated at this time; after pouring, the robot arm transfers the sample cup and the used funnel to the initial position of the transfer position; the robot arm grabs the sample table and transfers it to the tablet pressing position of the tablet pressing device; the tablet pressing device presses the tablet; the XRD automatically opens the door; the robot arm grabs the sample table and transfers it to the specified position of the XRD; the XRD automatically closes the door and starts the test; after the test is completed, the robot arm grabs the sample table and transfers it to the initial position of the transfer position; repeat the above operations until all sample tests are completed; the AGV grabs the consumables rack on the transfer position and transfers it to the transfer position of other functional islands.

[0083] (4) An automated X-ray fluorescence analysis subsystem, used to: perform fully automated X-ray fluorescence analysis on catalyst samples to obtain X-ray fluorescence analysis results of the catalyst samples.

[0084] The automated X-ray fluorescence analysis subsystem includes an automated X-ray fluorescence analyzer, an AGV composite robot, a dedicated robotic arm, and an instrument control program. In conjunction with the intelligent laboratory software platform, the following functions must be realized: the AGV composite robot can grab the sample cup and place it on the sample table of the automated X-ray fluorescence analyzer or the reverse process (the reverse process refers to the AGV composite robot grabbing the sample cup from the sample table of the automated X-ray fluorescence analyzer to complete the unloading and transfer process), complete automatic loading, unloading, and transfer, testing, data transmission, and other fully automatic operations, minimize manual operations, and improve experimental efficiency.

[0085] Measuring element range: from sodium (Na) to uranium (U); Element content analysis range: 1 ppm - 99.99% (the analysis range varies for different materials); Elements analyzed simultaneously: dozens of elements can be measured at one time; Analysis accuracy: 0.05% (for samples with a content higher than 96%, 21 - time test stability); Collimator: 8; X - ray filters: 5 types; X - ray irradiation area: Φ8mm, 6mm, 4mm, 3mm, 2mm, 1mm, 0.5mm, 0.1mm; Measuring method: energy dispersive type; State of the measurement object: solids, liquids, powders and films, no pretreatment required; Sample chamber volume: 320mm x 100mm; Measuring time: 30 seconds - 200 seconds; Detector energy resolution: 145 ± 5 eV; Element analysis software methods: internal standard method, qualitative, quantitative analysis, FP method, EC method and multiple function methods.

[0086] The working process of the fully automatic X - ray fluorescence analysis specifically includes: The AGV cart transports the consumable rack containing the XRF samples to be tested to the transfer position of the XRF test functional island; The robotic arm grabs the consumable rack at the transfer position, scans the code and then puts it back to the transfer position; The robotic arm grabs the sample cup on the consumable rack and transfers it to the lid - closing module to close the lid; After the lid - closing is completed, the robotic arm grabs the sample cup and transfers it to the test buffer position; The robotic arm grabs the sample cup from the test buffer position and transfers it to the designated position of the XRF instrument for automated testing; During the XRF instrument testing process, the robotic arm grabs the remaining sample cups to complete the lid - closing operation; After the testing is completed, the robotic arm grabs the sample cup and puts it back to the initial position of the consumable rack; After all the samples are tested, the AGV cart grabs the consumable rack at the transfer position and transfers it to the transfer position of other functional islands.

[0087] (5) Automated physical and chemical adsorption subsystem, used for: respectively performing physical adsorption treatment and chemical adsorption treatment on the catalyst sample to obtain the physical adsorption treatment and chemical adsorption treatment of the catalyst sample. It is divided into a physical adsorption module and a chemical adsorption module. It is used for the full - automatic physical / chemical adsorption analysis and characterization of materials such as catalysts. The equipment has an interface with independent communication, cooperates with a collaborative robot to complete automatic sample loading, automatic sample unloading, automated analysis and detection, can perform multiple cycle operations, record and transmit the analysis results back, realize all - weather uninterrupted high - throughput sample detection, minimize human operation as much as possible, and improve the experimental efficiency.

[0088] Technical parameters: The physical adsorption analysis part can achieve automatic analysis and automatic degassing functions, and has the ability to quickly analyze specific surface area and mesopore size distribution; the mesopore analysis module has 2 mesopore analysis stations, 1 P0 station and a pressure control proportional valve; each analysis station has a set of independent 1000 torr pressure sensors and manifold systems; Pressure sensors: A total of 4 1000 torr pressure sensors (2 in the analysis station, 1 in the independent P0 station, and 1 in the degassing station system); Pressure sensor accuracy: ±0.1% full scale; P / P0 partial pressure measurement range: 5×10 -4 -0.998; Specific surface area range: 0.01 m2 / g to no upper limit (N2); Pore size test range: 0.35 - 500 nm; Pressure resolution: 3×10 -5torr (0.0039Pa, 1000torr range); Specific surface test repeatability: ±0.5% (based on random standard samples); Adsorbate: N2, CO2, CH4, H2, O2, Ar, Kr and other non-corrosive gases; Configure PFC modulation valve group to ensure that the system is vacuumed in proportion to prevent powder separation and high vacuum pumping speed is too slow; The instrument host adopts a new 32-bit chip and circuit system to ensure analysis accuracy from the circuit hardware; The entire adsorption and desorption isotherm analysis process can be completed within 8 hours; It can display the remaining amount of liquid nitrogen in real time; when the liquid nitrogen is insufficient, there is an alarm display on the instrument panel and computer system; Intelligent degassing station module: 32-bit electronic circuit, with 2 degassing ports, cooperate with the sample pretreatment of the mesoporous analysis station; the degassing station is equipped with a pressure sensor and an automatic lifting furnace, which can monitor and output the temperature rise curve and residual pressure curve in real time, and the temperature control accuracy is better than 1°C; after the degassing is completed, the robot can automatically unload the sample tube and install it to the analysis station port; the degassing station adopts a computer-controlled program heating system, and the evacuation rate can be set in sections. Configure the PFC modulation valve group to ensure that the system is vacuumed in proportion to prevent powder precipitation and the problem of too slow pumping speed in high vacuum; degassing temperature range: ambient temperature to 450°C; heating rate: 0.1°C increment, digital setting, computer program control; backfill gas: user-selectable, helium or adsorbed gas. Degassing sensor: The degassing station is equipped with a 1000torr pressure sensor to ensure that the degassing pressure can be measured in real time; intelligent air cooling system: can quickly cool down the sample after processing. An aluminum alloy heating furnace with fast heating and uniform heating is used to replace the traditional heating pack; graphical software is used to facilitate the setting of degassing temperature and pressure. The unique intelligent mode can automatically determine the degassing completion degree and display the degassing status of the sample in real time; the vacuum pump group is a pump group composed of 2 mechanical pumps; the mechanical pump is built into a silent box, and the noise is no more than 40 decibels; it provides large flow and high vacuum dual-channel interfaces, serves the analysis station and degassing station at the same time, and can prevent cross-contamination of multiple analysis modules and degassing station modules; data analysis and processing software: it can complete all instrument control and data analysis during analysis, and can provide isotherm data information, calculate specific surface area, pore size distribution and total pore volume.

[0089] Workflow of the physical adsorption module: The experimenter places the clean sample tube on the material rack. All physical adsorption sample tubes have a unique coding identification, and the system records the positioning of the material rack. The AGV obtains the test instruction and receives the task. The mobile robot grabs the sample tube from the rack and transfers it to the automatic sample loader for sample loading. In this process, the system will call the positioning information of the filled sample for automatic sample selection. The robotic arm grabs the sample tube filled with the sample and sequentially transfers it to the automatic dryer, and completes the connection between the sample tube and the dryer to achieve programmed locking and sealing. The automatic drying equipment performs full-automatic degassing and dehydration treatment of the sample according to the preset parameters, including establishing a vacuum environment, programmed temperature rise, pressure detection, temperature recovery, and backfilling gas. After the degassing and dehydration program is completed, the robotic arm unloads the sample tube from the automatic dryer, places the sample tube on the weighing balance for weighing, and the program automatically calculates the weight of the sample after dehydration and degassing by the weight loss method and pushes it to the main control software. After weighing, the robotic arm automatically unloads the sample tube, installs the filling rod, installs it at the analysis station port of the physical adsorption instrument host and locks it tightly. A Dewar flask filled with liquid nitrogen is placed at the lifting tray of the physical adsorption instrument host. The physical adsorption instrument host starts automatic analysis work according to the program and parameter settings, including self-check of the functions of key components, establishment of a high-vacuum environment, vacuum degassing, dead volume test, adsorption and desorption analysis, room temperature recovery, and backfilling gas. After the analysis program is completed, the robotic arm starts, unloads the sample tube and transfers it to the waste material rack. The data is uploaded and synchronized to the central control system, and the instrument and equipment are in an idle state and can accept the next round of automated detection. If all the detection work is completed, the system automatically shuts down.

[0090] The working process of the chemisorption module includes: The experimenter places the clean sample tube on the material rack. All chemisorption sample tubes have a unique coding identification, and the system records the positioning of the material rack. The AGV obtains the test instruction and receives the task. The mobile robot grabs the sample tube from the rack and transfers it to the automatic sampler for sample loading. In this process, the system will call the positioning information of the filled sample for automatic sample selection. The robotic arm grabs the sample tube filled with the sample and places it on the weighing balance for weighing. The program automatically calculates the weight of the sample after dehydration and degassing by the weight loss method and pushes it to the main control software. After weighing, the robotic arm automatically unloads the sample tube, installs it at the analysis station port of the chemisorption instrument host and locks it tightly. The programmed temperature rise electric furnace of the chemisorption instrument is in the standby state. The chemisorption instrument host starts the automatic analysis work according to the program and parameter settings, including self-check of key component functions, inert gas flow degassing, sample chemical reaction pretreatment, programmed temperature rise analysis, restoration to room temperature and purge of the analysis system. After the analysis program is completed, the robotic arm starts, unloads the sample tube and transfers it to the waste material rack. The analysis data is uploaded and synchronized to the central control system. The instrument and equipment are in the vacant state and can accept the next round of automated detection. If all the detection work is completed, the system will automatically shut down. There is an exhaust hood above the chemisorption module, and one exhaust port is reserved for air circulation.

[0091] (6) The automated infrared analysis subsystem is used for: obtaining the infrared spectral data of the catalyst sample; analyzing the catalyst sample based on the infrared spectral data to obtain the infrared analysis result of the catalyst sample.

[0092] The automated infrared analysis subsystem is used for the full-automatic infrared spectral analysis and characterization of materials such as catalysts. The equipment has an interface with independent communication. After manual sample preparation and loading are completed, it cooperates to complete automated sample replacement, automated analysis and detection, records and transmits the analysis results back, realizes all-weather uninterrupted high-throughput sample detection, minimizes manual operations as much as possible, and improves experimental efficiency. The automated infrared analysis subsystem includes an infrared spectrometer and an in-situ cell.

[0093] The technical parameters of the infrared spectrometer are set as follows: spectral range: 7800 - 350 cm-1; spectral resolution: better than 0.25 cm-1; signal-to-noise ratio better than 50000:1 (1-minute scan, 4 cm-1 resolution); ASTM linearity index: deviation from 0.0% T not exceeding 0.1% T; aperture: computer-controlled variable aperture; scan speed: not less than 20 spectra / second (DTGS detector); wavenumber accuracy: better than 0.01 cm-1. The infrared spectrometer includes the following components: infrared light source: high-efficiency infrared light source, with the highest energy value in the mid-infrared fingerprint region, 10-year warranty; interferometer: using a magnetically levitated flat mirror (not a solid-angle mirror), 10-year warranty; dynamic collimation: having a real-time automatic high-speed scanning dynamic collimation control function, more than 100,000 times per second; detector: high-efficiency DTGS detector; beam splitter: KBr beam splitter in the mid-infrared band; laser: semiconductor laser, 10-year warranty; permanent collimation optical path: the optical bench adopts a permanent collimation optical path design, without the need for manual adjustment by the user during use. All components adopt a pin-to-pin positioning method, plug-and-play. This embodiment can use a Nicolet Fourier transform infrared spectrometer.

[0094] In-situ cell: At least 3 gases can be introduced, and the in-situ cell is filled at a specific flow rate; the controllable temperature range of the in-situ cell is room temperature to 600 °C, and the temperature control accuracy is ±1 °C; the in-situ cell can be evacuated, equipped with a vacuum gauge to measure the vacuum degree; liquid probe molecule vapor can be introduced to conduct liquid probe molecule adsorption experiments; the in-situ cell can move directionally, the moving speed is not less than 1 mm / s, and the moving accuracy is ±0.5 mm; the sample cell can install at least 6 samples to be tested and cooperate with external instruments to detect them one by one; the analysis process can be combined according to customer needs, and any combination of heating, gas filling, evacuation, filling atomized solution, and infrared detection can be carried out. Gas requirements for the in-situ cell: 3 gas paths include 1 path of N2, 1 path of 10% N2 / 90% H2, and 1 path of CO, equipped with a secondary pressure reducing valve, the outlet is 6 mm quick-connect or quick-plug, and the pressure reduction is ≤1.6 MPa.

[0095] The working process of infrared spectroscopy testing is as follows: The AGV transports the consumable rack containing the infrared samples to be tested to the transfer position of the infrared spectroscopy functional island; manually log in to the system and receive the sub-packaging information form, as shown in Table 2; manually use the tablet pressing device to press the tablet, weigh and record the mass; manually load it into the in-situ cell; after manually inputting the information form, click test, and the infrared spectroscopy system starts automatic operation (ventilation, heating, testing, etc.); after the test is completed, the system starts to cool down; wait until it cools down to room temperature, then manually disassemble the sample from the in-situ cell; manually discard the sample and clean the in-situ cell.

[0096] Table 2 Sub-packaging information form

[0097]

[0098] (3) Catalyst Reaction Evaluation Automation System: An automated high-temperature reactor reaction system is introduced to achieve efficient evaluation of catalyst performance under high-temperature and high-pressure reaction conditions. More evaluation devices can be added in the later stage to realize more-dimensional evaluation of catalysts.

[0099] The automated high-temperature reactor reaction system is used for the full-automatic high-temperature reactor evaluation of materials such as catalysts. The equipment has an interface with independent communication, and cooperates with a collaborative robot to complete automatic feeding, automated reaction, automated addition of internal standards, automated sampling, filtration, recording, and transmission of reaction data of samples, realizing all-weather high-temperature reactor evaluation of samples, minimizing manual operations as much as possible, and improving experimental efficiency.

[0100] Technical parameters of the automated high-temperature reactor reaction system: Maximum production capacity of the equipment: Determined by the single test duration of the evaluation experiment. Compatibility of the detection channel number: 4 independent channels. (Can be upgraded and expanded in the later stage); The whole machine has the ability to be upgraded and transformed in the later stage, with reserved positions and ports; The designed temperature of the high-temperature reactor is not lower than 250°C, the designed pressure is not lower than 10 Mpa, the effective volume is not lower than 50 ml, and the material can withstand the wear and corrosion of the materials in the conventional high-temperature reactor test; The display accuracy of the solvent automatic feeding system is not lower than 0.01 g, and the control accuracy of the gas-phase feeding is not lower than 0.1 sccm; The temperature control accuracy of the high-temperature reactor system is not lower than ±1°C, and the pressure control accuracy is not lower than ±0.1 Mpa. All photoelectric switches equipped with the equipment have the ability to verify anti-interference. The equipment PLC has data ports (RS232, RS422, RJ45). Air pressure switch protection function. An obvious emergency stop switch needs to be installed within one meter of the personnel operation, and electrical installation has leakage protection. One drain pipe is reserved to be consistent with the incoming water pipe.

[0101] The working process of the automated high-temperature reactor reaction system includes catalyst evaluation and sample loading and testing.

[0102] 1) Catalyst evaluation: The AGV cart transports the consumable rack (sample cup) containing the catalyst to be evaluated to the transfer position of the high-temperature reactor functional island; the robotic arm grabs the consumable rack at the transfer position, scans the code, and then returns it to the transfer position; according to the number of samples in the consumable rack, the corresponding number of reactors in the automated high-temperature reactor reaction system starts to automatically feed the solvent, and the sealing ring is opened and the reactor body is lowered; the robotic arm grabs the sample cup on the consumable rack, transfers it to the balance for weighing, and records the weight as X1; the robotic arm grabs the sample cup at the balance, transfers it above the reactor body, and flips (shakes) the sample in the sample cup; after pouring is completed, the robotic arm transfers the sample cup to the balance again for weighing, records the weight as Y1, and automatically calculates the mass of the added sample as X1 - Y1; repeat the above weighing operation until all samples are added to the corresponding reactors; the robotic arm grabs the reaction liquid bottle and transfers it to the switch cover module to open the lid; the robotic arm grabs the reaction liquid bottle and transfers it to the balance for weighing, records the weight as X2; the pipetting device sucks the reaction liquid from the reaction liquid bottle and adds it to the reactor body, and at the same time as the suction is completed, records the balance weight as Y2, and automatically calculates the mass of the added reaction liquid as X2 - Y2; after all the reaction liquids are added, the high-temperature reactor system automatically rises and seals the reactor body; at the same time, the robotic arm grabs the reaction liquid bottle at the balance, transfers it to the switch cover module to close the lid and then returns it to its original position; the high-temperature reactor system starts the automated operation (low-pressure purge - pressure holding test - programmed temperature rise - pressure control - start reaction - reaction end - pressure relief - open seal - lower reactor body); the robotic arm grabs the internal standard liquid bottle and transfers it to the switch cover module to open the lid; the robotic arm grabs the internal standard liquid bottle and transfers it to the balance for weighing, records the weight as X3; the pipetting device sucks the internal standard liquid from the internal standard liquid bottle and adds it to the reactor body, and at the same time as the suction is completed, records the balance weight as Y3, and automatically calculates the mass of the added internal standard liquid as X3 - Y3; after all the internal standard liquids are added, the high-temperature reactor system automatically raises the reactor body and seals it; at the same time, the robotic arm grabs the internal standard liquid bottle at the balance, transfers it to the switch cover module to close the lid and then returns it to its original position; the robotic arm grabs the consumable rack (filter tube) at the material rack, scans the code, and then returns it to the material rack; the robotic arm grabs the filter tube, scans the code, and transfers it to the sampling position. After the high-temperature reactor system is pressurized to 0.15 - 0.3 MPa, the discharge valve is automatically opened; set the sampling time, close the sampling valve when the time is up, and the robotic arm grabs the filter tube and transfers it to the filtering device for filtering; after filtering is completed, it is returned to the consumable rack (original position) on the material rack; the AGV cart grabs the consumable rack (empty sample cup) at the transfer position and transfers it to the transfer position of other functional islands; at the same time, the high-temperature reactor system automatically completes the cleaning and purging and returns to the initial position, waiting for the next round of reaction evaluation.

[0103] 2) Sample loading test: The five-axis robotic arm grabs the consumable rack on the rack, transfers it to the barcode scanning module for scanning, and then puts it back on the rack; the five-axis robotic arm grabs the filter tube (sample injection bottle) on the consumable rack, scans it with the barcode scanning module, and transfers it to the fixed hole position of the chromatographic injector; if there is more than one sample, repeat the above step, and at the same time, the system controls the chromatographic injector to automatically rotate to an empty hole position to the specified position and wait for sample loading; the system controls the automated chromatographic test; after the test is completed, the five-axis robotic arm grabs the sample injection bottle and puts it back to the original position on the original consumable rack; the AGV cart grabs the consumable rack on the rack and transfers it to the transfer position of other functional islands.

[0104] The overall laboratory planning in this application is divided into the construction of an automated catalyst preparation system, the construction of an automated catalyst pretreatment system, the construction of an automated catalyst characterization system, the construction of an automated catalyst reaction evaluation system, and the construction of an integrated overall solution system; at the same time, physical spaces such as logistics channels and viewing corridors are reserved. In the form of an independent station, each automated device works in parallel to achieve high throughput. A remote experiment operation platform is configured to allow researchers to remotely control experimental equipment and experimental processes, improving the flexibility and response speed of experiments.

[0105] This application aims to establish an intelligent management platform for catalyst synthesis that integrates automated synthesis, high-precision characterization, and efficient evaluation. Combining with an AI computing platform, it promotes the innovation and development of catalyst research and development technologies, and has the following advantages:

[0106] (1) Improve R & D efficiency: Through the automated preparation and characterization system, rapid synthesis and screening of catalysts are realized, significantly reducing the cycle time from concept to laboratory prototype.

[0107] (2) Enhance experimental accuracy: Utilize high-precision automated equipment and a strict quality control system to ensure the accuracy and repeatability of the catalyst preparation, characterization, and evaluation processes, reducing human errors.

[0108] (3) Achieve intelligent management: Develop a comprehensive laboratory information management system to realize intelligent management of laboratory drugs, instruments, experimental processes, and data assets, improving the transparency and efficiency of laboratory operations.

[0109] (4) Promote interdisciplinary cooperation: Establish an open laboratory platform to encourage researchers in multiple disciplinary fields such as materials science, chemical engineering, and data analysis to cooperate, promoting the development of innovative thinking and interdisciplinary research.

[0110] (5) Facilitate the commercialization of scientific research results: By accelerating the catalyst development process, shortening the time from laboratory to market for products, and promoting the rapid transformation and commercialization of scientific research results.

[0111] (6) Attempt to establish industry standards: Through the efficient operation and innovative practices of the laboratory, participate in formulating industry standards for catalyst R & D and evaluation, and promote the technological progress and quality improvement of the entire industry.

[0112] Example 2

[0113] As Figure 3 shown, this example provides a control method for the catalyst synthesis intelligent management platform described in Example 1, including the following steps.

[0114] Step S1: Use the catalyst pretreatment automation system to automatically control the storage, transfer, sub-packaging, and catalyst reaction equipment of the catalyst sample, and determine the pretreatment information of the catalyst sample; the pretreatment information includes storage, transfer, sub-packaging, and catalyst reaction information.

[0115] Step S2: Use the catalyst characterization automation system to connect with each automated characterization device through the central control software, and collect and monitor the characterization data in real time.

[0116] Step S3: Use the catalyst reaction evaluation automation system to screen out catalysts that meet the expected performance requirements.

[0117] The technical features of the above embodiments can be combined arbitrarily. For the sake of brevity of description, not all possible combinations of the technical features in the above embodiments are described. However, as long as there is no contradiction in the combination of these technical features, it should be considered as the scope described in this specification.

[0118] Specific examples are used in this article to elaborate on the principles and implementation methods of this application. The descriptions of the above embodiments are only used to help understand the method and its core idea of this application; at the same time, for those of ordinary skill in the art, based on the idea of this application, there will be changes in the specific implementation methods and application scopes. In summary, the content of this specification should not be construed as a limitation to this application.

Claims

1. A catalyst synthesis intelligent management platform, characterized in that, The catalyst synthesis intelligent management platform includes: A catalyst pretreatment automation system for automatically controlling the storage, transfer, sub-packaging, and catalyst reaction equipment of catalyst samples to determine the pretreatment information of the catalyst samples; the pretreatment information includes storage, transfer, sub-packaging, and catalyst reaction information; A catalyst characterization automation system for docking with each automated characterization device through a central control software to collect characterization data in real time and monitor the characterization data in real time; A catalyst reaction evaluation automation system for introducing an automated high-temperature reaction kettle reaction system to screen out catalysts that meet the expected performance requirements.

2. The intelligent management platform for catalyst synthesis according to claim 1, wherein The catalyst pretreatment automation system includes an automated sample weighing module, and the automated sample weighing module is used to control the mass of sample conveyance in the form of electromagnetic vibration.

3. The intelligent management platform for catalyst synthesis according to claim 1, wherein The catalyst pretreatment automation system includes an automatic temperature control module, and the automatic temperature control module is used to control the reaction temperature of the sample.

4. The intelligent management platform for catalyst synthesis according to claim 1, wherein The catalyst characterization automation system includes an automated Raman spectroscopy analysis subsystem, and the automated Raman spectroscopy analysis subsystem is used to: obtain the spectral data of the catalyst sample; determine the types of chemical substances of the catalyst sample according to the spectral data of the catalyst sample.

5. The intelligent management platform for catalyst synthesis according to claim 1, characterized in that The catalyst characterization automation system includes an automated X-ray diffraction analysis subsystem; the automated X-ray diffraction analysis subsystem is used to: perform a full-automatic X-ray diffraction analysis on the catalyst sample to obtain the X-ray diffraction analysis result of the catalyst sample.

6. The intelligent management platform for catalyst synthesis according to claim 1, characterized in that, The catalyst characterization automation system includes an automated X-ray fluorescence analysis subsystem; the automated X-ray fluorescence analysis subsystem is used to: perform a full-automatic X-ray fluorescence analysis on the catalyst sample to obtain the X-ray fluorescence analysis result of the catalyst sample.

7. The intelligent management platform for catalyst synthesis according to claim 1, characterized in that, The catalyst characterization automation system includes an automated physical and chemical adsorption subsystem; the automated physical and chemical adsorption subsystem is used to: perform physical adsorption treatment and chemical adsorption treatment on the catalyst sample respectively to obtain the physical adsorption treatment and chemical adsorption treatment of the catalyst sample.

8. The catalyst synthesis intelligent management platform according to claim 1, characterized in that, The catalyst characterization automation system includes an automated inductively coupled plasma emission spectrometry subsystem; the automated inductively coupled plasma emission spectrometry subsystem is used to: use the high-temperature excitation source generated by inductively coupled plasma to atomize and excite the catalyst sample to obtain the wavelengths and intensities of the characteristic spectral lines of the detected elements of the catalyst sample; Determine the types of detected elements according to the wavelengths and intensities of the characteristic spectral lines of the detected elements; Determine the contents of each detected element in the catalyst sample according to the quantitative relationship between the intensities of the characteristic spectral lines of the detected elements and the element concentrations.

9. The intelligent management platform for catalyst synthesis according to claim 1, wherein, The catalyst characterization automation system includes an automated infrared analysis subsystem; the automated infrared analysis subsystem is used to: obtain the infrared spectral data of the catalyst sample; analyze the catalyst sample according to the infrared spectral data to obtain the infrared analysis result of the catalyst sample.

10. A control method for a catalyst synthesis intelligent management platform according to any one of claims 1-9, characterized in that, The control method includes: Automatically control the storage, transfer, sub-packaging, and catalyst reaction equipment of catalyst samples using a catalyst pretreatment automation system, and determine the pretreatment information of the catalyst samples; the pretreatment information includes storage, transfer, sub-packaging, and catalyst reaction information; Use a catalyst characterization automation system to interface with each automated characterization device through a central control software, and collect characterization data in real time and monitor the characterization data in real time; Use a catalyst reaction evaluation automation system to screen out catalysts that meet the expected performance requirements.

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