Automatic control experiment device for transition metal organic framework synthesis

Abstract

The invention provides an automatic control experiment device for transition metal organic framework synthesis, and relates to the technical field of experiment automatic control. The device comprises a local controller and a plurality of experimental parts, mainly comprises a metal compound, an organic compound, a mixed solvent and an acid source feeding assembly, a synthesis reaction kettle, a temperature adjusting assembly, a washing reaction kettle, a detergent feeding assembly and a yield analysis assembly, and all the parts are electrically connected with the local controller through pipelines. And full-flow automatic control from raw material injection to product washing is realized. The local controller receives experimental parameters and flow information of the remote terminal, generates a control instruction and drives all parts to work cooperatively, and the yield analysis assembly feeds back a yield result in real time, so that experimental optimization is facilitated; according to the invention, the manual intervention is obviously reduced, the accuracy and repeatability of the experiment are improved, and the experiment efficiency and the data management capability are enhanced.

Description

TECHNICAL FIELD

[0001] The present application mainly relates to the technical field of experimental automatic control, and particularly relates to an automatic control experimental device for synthesis of transition metal organic frameworks. BACKGROUND

[0002] Metal-Organic Frameworks (MOFs) are a class of porous crystalline materials formed by the coordination of metal ions or clusters with organic ligands. Due to their unique pore structure, high specific surface area, and adjustable chemical functionality, MOFs have shown great potential in various applications such as catalysis, gas storage, sensing, and drug delivery.

[0003] However, the traditional method has the following limitations:

[0004] Human factor influence: The actual ratio of ingredients may deviate from the ideal value due to human operational errors, leading to inconsistency in experimental results.

[0005] Inaccurate temperature control: During long-term high-temperature heating, the rate of temperature change and stability are difficult to monitor in real time, affecting the uniformity of the reaction and the quality of the product.

[0006] Low efficiency of post-processing: The filtration and washing steps completely rely on manual operation, making it difficult to ensure the thoroughness of washing and the purity of the product, and the operation is tedious and time-consuming.

[0007] Therefore, there is an urgent need for an automatic control experimental device that can achieve high-precision ingredient preparation and real-time temperature monitoring to overcome the limitations of traditional synthesis methods, improve the accuracy and efficiency of transition metal organic framework synthesis, and reduce human factor interference. SUMMARY

[0008] The technical problem to be solved by the present application is to provide an automatic control experimental device for synthesis of transition metal organic frameworks to overcome the shortcomings of the prior art.

[0009] The technical solution of the present application to solve the above technical problems is as follows: An automatic control experimental device for synthesis of transition metal organic frameworks, comprising a local controller and experimental components, wherein the experimental components include metal compound feeding, organic compound feeding assembly, mixed solvent feeding assembly, acid source feeding assembly, synthesis reaction kettle, temperature adjusting assembly, washing reaction kettle, washing agent feeding assembly, and yield analysis assembly, which are electrically connected with the local controller respectively.

[0010] The metal compound feeding assembly, the organic compound feeding assembly, the mixed solvent feeding assembly and the acid source feeding assembly are respectively communicated with the inside of the synthesis reaction kettle through pipelines, the temperature adjusting assembly is installed at the top end of the synthesis reaction kettle, the synthesis reaction kettle is communicated with the washing reaction kettle through a pipeline, and the washing agent feeding assembly is communicated with the washing reaction kettle through a pipeline;

[0011] The local controller is electrically connected with the remote control terminal, and is used for generating a control instruction according to experiment parameters and experiment process information sent by the remote control terminal;

[0012] The experiment component is used for carrying out a synthesis reaction according to the control instruction to obtain a preliminary synthesis product, and carrying out a washing treatment on the synthesis product to obtain a final synthesis product;

[0013] The yield analysis component is electrically connected with the remote control terminal, and is used for weighing the final synthesis product according to a yield analysis instruction sent by the remote control terminal, and carrying out yield calculation based on the weight of the raw material and the weight of the final synthesis product to obtain a yield result, and feeding back the yield result to the remote control terminal.

[0014] On the basis of the above technical solution, the application can also be improved as follows.

[0015] Further, the synthesis reaction is carried out according to the control instruction to obtain a preliminary synthesis product, and specifically:

[0016] The local controller is used for receiving experiment parameters and experiment process information of the remote control terminal, and generating a raw material injection control instruction based on the experiment parameters;

[0017] The metal compound feeding assembly, the organic compound feeding assembly and the mixed solvent feeding assembly are respectively used for obtaining corresponding dosages from the raw material injection control instruction, and injecting the stored metal compound, organic compound and mixed solvent into the synthesis reaction kettle according to the corresponding dosages to form a mixture, and sending a feeding completion signal to the local controller;

[0018] The local controller is further used for generating a dissolution treatment control instruction according to the feeding completion signal and the experiment process, and sending the dissolution treatment control instruction to the synthesis reaction kettle;

[0019] The synthesis reaction kettle is used for obtaining a reaction time from the dissolution treatment control instruction, carrying out ultrasonic treatment on the mixture according to the reaction time, and sending a first-stage reaction completion signal to the local controller when the timing reaches the reaction time;

[0020] The local controller is further used for generating an acid dropwise adding control instruction according to the first-stage reaction completion signal and the experiment process information, and sending the acid dropwise adding control instruction to the acid source feeding assembly.

[0021] The acid source feeding assembly is configured to obtain a corresponding dose from the acid drop control instruction, and to drop the hydrochloric acid aqueous solution into the synthesis reaction kettle according to the corresponding dose, and to send a drop completion signal to the local controller when the dropping is completed;

[0022] The local controller is further configured to generate a temperature control instruction according to the drop completion signal and the experimental procedure information, and to send the temperature control instruction to the temperature adjusting assembly;

[0023] The temperature adjusting assembly is configured to obtain a heating temperature value and a heating time length from the temperature control instruction, to heat the synthesis reaction kettle according to the heating temperature value and the reaction time, to monitor a temperature value in the synthesis reaction kettle in real time, to adjust the real-time temperature value according to the heating temperature value, to cool the synthesis reaction kettle when the reaction time reaches, and to obtain a preliminary synthesis product when the temperature in the kettle reaches a room temperature.

[0024] Further, the synthesis product is subjected to a washing treatment to obtain a final synthesis product, and the washing treatment comprises the following steps:

[0025] The temperature adjusting assembly is further configured to send a second-stage reaction completion signal to the local controller when the temperature in the kettle reaches the room temperature.

[0026] The local controller is further configured to generate a product transfer control instruction and a washing agent feeding instruction according to the second-stage reaction completion signal and the experimental procedure information, and to send the product transfer control instruction and the washing agent feeding instruction to the synthesis reaction kettle and the washing agent feeding assembly, respectively.

[0027] The synthesis reaction kettle is further configured to transfer the synthesis product into the washing reaction kettle according to the product transfer control instruction.

[0028] The washing agent feeding assembly is further configured to obtain a corresponding dose from the washing agent feeding instruction, to add the washing agent into the washing reaction kettle according to the corresponding dose, and to send an addition completion signal to the local controller.

[0029] The local controller is further configured to generate a washing instruction according to the addition completion signal and the experimental procedure information.

[0030] The washing reaction kettle is configured to obtain a washing time from the washing instruction, to wash the preliminary synthesis product according to the washing time, and to obtain the final synthesis product when the washing time reaches.

[0031] Further, the yield analysis assembly comprises a weighing device and an analyzer.

[0032] The weighing device is used to weigh the final synthesis product according to the yield analysis instruction sent by the remote control terminal to obtain the weight value of the final synthesis product;

[0033] The analyzer is used to calculate the theoretical yield of the raw material weight according to a preset chemical reaction formula to obtain the theoretical weight, and calculate the theoretical weight and the weight of the final synthetic product based on the yield formula to obtain the yield result. The yield formula is:

[0034]

[0035] The beneficial effects of the present invention are as follows: through the electrical connection between the local controller and the remote control terminal, remote control and automated operation of the experimental process are realized, manual intervention is reduced, and the accuracy and repeatability of the experiment are improved; the complete experimental process from raw material feeding, reaction control to product washing and yield analysis is covered, forming a complete set of automated experimental systems, thereby improving experimental efficiency; the yield analysis component can feed back the yield results to the remote control terminal in real time, so that the user can understand the experimental progress and results in a timely manner, and facilitate experimental optimization and adjustment. BRIEF DESCRIPTION OF THE DRAWINGS

[0036] Figure 1 A schematic structural diagram of an automatic control experimental device for synthesizing transition metal organic frameworks provided in an embodiment of the present invention.

[0037] In the accompanying drawings, the names of the components represented by the various symbols are as follows:

[0038] 1. Local controller, 2. Metal compound feed assembly, 3. Organic compound feed assembly, 4. Mixed solvent feed assembly, 5. Acid source feed assembly, 6. Synthesis reactor, 7. Washing reactor, 8. Detergent feed assembly, 9. Booster pump, 10. Air exhaust port, 11. Air exhaust port, 12. Equipment cabinet. DETAILED DESCRIPTION

[0039] The principles and features of the present invention are described below with reference to the accompanying drawings. The examples given are only used to explain the present invention and are not used to limit the scope of the present invention.

[0040] Example 1: Figure 1 As shown, an embodiment of the present invention provides an automatic control experimental device for the synthesis of transition metal organic frameworks, comprising a local controller 1 and experimental components installed in an equipment cabinet 12, wherein the experimental components include a metal compound feeding assembly 2, an organic compound feeding assembly 3, a mixed solvent feeding assembly 4, an acid source feeding assembly 5, a synthesis reactor 6, a temperature regulating assembly, a washing reactor 7, a detergent feeding assembly 8, and a yield analysis assembly, which are electrically connected to the local controller 1 respectively;

[0041] The metal compound feeding assembly 2, the organic compound feeding assembly 3, the mixed solvent feeding assembly 4, and the acid source feeding assembly 5 are respectively communicated with the inside of the synthesis reaction kettle 6 through pipes, the temperature adjusting assembly is installed at the top end of the synthesis reaction kettle 6, the synthesis reaction kettle 6 is communicated with the washing reaction kettle 7 through a pipe, and the washing agent feeding assembly 8 is communicated with the washing reaction kettle 7 through a pipe;

[0042] The local controller 1 is electrically connected with the remote control terminal, and is used for generating a control instruction according to experiment parameters and experiment process information sent by the remote control terminal;

[0043] The experiment component is used for performing a synthesis reaction according to the control instruction, obtaining a preliminary synthesis product, and performing a washing treatment on the synthesis product to obtain a final synthesis product;

[0044] The yield analysis assembly is electrically connected with the remote control terminal, and is used for weighing the final synthesis product according to a yield analysis instruction sent by the remote control terminal, performing yield calculation based on the weight of the raw material and the weight of the final synthesis product, obtaining a yield result, and feeding back the yield result to the remote control terminal.

[0045] In the embodiment, the electrical connection specifically refers to that the remote control terminal and the local controller can perform data transmission and instruction control through wired or wireless communication modes (such as Ethernet, Modbus, mqtt+json protocol, etc.).

[0046] And the local controller and the experiment component can realize accurate control of each experiment component through an instruction circuit board and a communication interface (such as RS485, RS232, CAN bus, etc.).

[0047] It should be understood that the experiment process information refers to a detailed instruction set describing specific steps, operation sequences and related parameters of the entire experiment process. The experiment process information clearly defines the execution sequence of each step, ensuring the coherence and logic of the experiment process. For example, the experiment steps are:

[0048] Raw material injection: specify the injection sequence and dosage of the metal compound, the organic compound, the mixed solvent and the acid source.

[0049] Dissolution treatment: set the ultrasonic treatment time and power.

[0050] Acid drop: specify the drop amount and drop speed of the acid source.

[0051] Temperature control: set the heating temperature, heating rate, constant temperature time and cooling rate of the reaction kettle.

[0052] Product transfer: control the operation of transferring the synthesis product from the synthesis reaction kettle to the washing reaction kettle.

[0053] Washing process: Set the amount of detergent, washing time and washing times.

[0054] Yield analysis: Specify the weighing method and yield calculation method of the final product.

[0055] Experimental parameters include specific parameters for each step, such as:

[0056] Raw material injection: Specific dosage of metal compounds, organic compounds, mixed solvents and acid sources.

[0057] Dissolution process: Specific time of ultrasonic treatment (e.g. 30 minutes).

[0058] Acid drop: Specific drop amount (e.g. 1.5 mL) and drop speed (e.g. 0.5 mL / min) of acid source.

[0059] Temperature control: Heating temperature (e.g. 120℃), heating rate (e.g. 10℃ / hour), constant temperature time (e.g. 72 hours) and cooling rate (e.g. 5℃ / hour).

[0060] Product transfer: Specific conditions and time of transfer.

[0061] Washing process: Specific amount of detergent (e.g. 50 mL), washing time (e.g. 10 minutes) and washing times (e.g. 3 times).

[0062] Yield analysis: Weighing method and yield calculation formula of final product.

[0063] The experimental flow information also supports real-time monitoring and feedback mechanism, ensuring that the execution of each step can be fed back to the local controller in time.

[0064] For example: After each step is completed, the relevant components will send a completion signal to the local controller.

[0065] The local controller generates control instructions for the next step according to the completion signal.

[0066] During the experiment, sensors collect data (such as temperature, pH value, pressure, etc.) in real time and feed the data back to the local controller.

[0067] In this embodiment, through the electrical connection between the local controller and the remote control terminal, remote control and automatic operation of the experimental process are realized, reducing manual intervention and improving the accuracy and repeatability of the experiment;

[0068] It covers the complete experimental process from raw material feeding, reaction control to product washing and yield analysis, forming a complete automatic experimental system and improving experimental efficiency;

[0069] The yield analysis component can feed back the yield result to the remote control terminal in real time, so that the user can know the experiment progress and result in time, and the experiment can be optimized and adjusted.

[0070] Preferably, the local controller 1 is configured to receive experiment parameters and experiment process information of the remote control terminal, and generate raw material injection control instructions based on the experiment parameters.

[0071] The metal compound feeding component 2, the organic compound feeding component 3 and the mixed solvent feeding component 4 are configured to obtain corresponding dosages from the raw material injection control instructions, and inject the stored metal compound, organic compound and mixed solvent into the synthesis reactor 6 according to the corresponding dosages to form a mixture, and send a feeding completion signal to the local controller 1.

[0072] The local controller 1 is further configured to generate a dissolution treatment control instruction according to the feeding completion signal and the experiment process, and send the dissolution treatment control instruction to the synthesis reactor 6.

[0073] The synthesis reactor 6 is configured to obtain a reaction time from the dissolution treatment control instruction, and perform ultrasonic treatment on the mixture according to the reaction time, and send a first-stage reaction completion signal to the local controller 1 when the reaction time is reached.

[0074] The local controller 1 is further configured to generate an acid drop control instruction according to the first-stage reaction completion signal and the experiment process information, and send the acid drop control instruction to the acid source feeding component 5.

[0075] The acid source feeding component 5 is configured to obtain a corresponding dosage from the acid drop control instruction, and drop the hydrochloric acid aqueous solution into the synthesis reactor 6 according to the corresponding dosage, and send a drop completion signal to the local controller 1 when the dropping is completed; during the dropping process, a pH sensor monitors the acidity and alkalinity of the solution in real time to ensure the accuracy of the dropping amount, and the pH sensor can send the monitored acidity and alkalinity of the solution to the remote control terminal through the local controller 1 for monitoring.

[0076] The local controller 1 is further configured to generate a temperature control instruction according to the drop completion signal and the experiment process information, and send the temperature control instruction to the temperature adjusting component.

[0077] The temperature adjusting component is configured to obtain a heating temperature value and a heating time length from the temperature control instruction, heat the synthesis reactor 6 according to the heating temperature value and the reaction time, monitor the temperature value in the synthesis reactor 6 in real time, adjust the real-time temperature value according to the heating temperature value, cool the synthesis reactor 6 when the reaction time is reached, and obtain a preliminary synthesis product when the temperature in the reactor reaches the room temperature.

[0078] Specifically, the temperature adjusting assembly controls the temperature sensor according to the set condition, warms the synthesis reactor 6 from room temperature to 120 DEG C for 12 hours, and keeps constant temperature for 3 days, and then cools from 120 DEG C to room temperature for 36 hours.

[0079] In the embodiment, the local controller generates raw material injection control instructions according to experimental parameters, each feeding assembly can accurately control the injection dose of raw materials, ensures the accuracy of experimental ingredients, and reduces human error;

[0080] Through the phased control instructions (such as dissolution treatment control instructions, acid drop control instructions, temperature control instructions, etc.), fine control of the experimental process is realized, and each stage of operation can be strictly performed according to the preset parameters, thereby improving the success rate of the experiment and the quality of the product;

[0081] After each stage is completed, the relevant components send a completion signal to the local controller, and the local controller generates the next control instruction according to the signals, thereby realizing real-time monitoring and feedback of the experimental process and ensuring that the experiment is carried out according to the plan.

[0082] Preferably, the synthesis product is subjected to a washing treatment to obtain a final synthesis product, specifically:

[0083] The temperature adjusting assembly is also used to send a second-stage reaction completion signal to the local controller 1 when the temperature in the reactor reaches the indoor temperature;

[0084] The local controller 1 is also used to generate a product transfer control instruction and a washing agent feeding instruction according to the second-stage reaction completion signal and experimental process information, and send them to the synthesis reactor 6 and the washing agent feeding assembly 8, respectively;

[0085] The synthesis reactor 6 is also used to transfer the synthesis product to the washing reactor 7 according to the product transfer control instruction;

[0086] The washing agent feeding assembly 8 is also used to obtain a corresponding dose from the washing agent feeding instruction, and add the washing agent to the washing reactor 7 according to the corresponding dose, and send an addition completion signal to the local controller 1;

[0087] The local controller 1 is also used to generate a washing instruction according to the addition completion signal and experimental process information;

[0088] The washing reactor 7 is used to obtain a washing time from the washing instruction, and wash the preliminary synthesis product according to the washing time, and obtain a final synthesis product when the washing time arrives.

[0089] In this embodiment, the automatic washing process of the preliminary synthesis product is realized, the amount of detergent added is accurately controlled through the detergent feeding assembly, and the product is washed according to the washing instruction, thereby improving the washing effect and product purity;

[0090] Each stage from the synthesis reaction to the product washing is seamlessly connected, the coherence and efficiency of the experimental process are ensured through the unified scheduling of the local controller, and the manual operation and time waste in the intermediate link are reduced;

[0091] The synthesis reactor can automatically transfer the synthesis product to the washing reactor according to the product transfer control instruction, thereby avoiding the product loss and pollution caused by manual transfer, and improving the safety and reliability of the experiment.

[0092] Preferably, the yield analysis assembly comprises a weighing device and an analyzer;

[0093] The weighing device is used to weigh the final synthesis product according to the yield analysis instruction sent by the remote control terminal, and obtain the weight value of the final synthesis product;

[0094] The analyzer is used to calculate the theoretical yield of the weight of the raw material through a preset chemical reaction formula, obtain a theoretical weight, and calculate the theoretical weight and the weight of the final synthesis product based on a yield formula to obtain a yield result, wherein the yield formula is:

[0095]

[0096] In this embodiment, the yield analysis assembly can accurately measure the weight of the final synthesis product through the weighing device and the analyzer, and calculate the theoretical yield based on the preset chemical reaction formula, thereby obtaining an accurate yield result, which provides reliable data support for experimental evaluation and optimization;

[0097] The yield analysis instruction is introduced to realize the automatic processing and analysis of experimental data, improve the efficiency and accuracy of data processing, and facilitate users to quickly understand the experimental effect, which provides a basis for subsequent adjustment of experimental schemes;

[0098] The yield result can be fed back to the remote control terminal in real time, and the user can view the yield data of the experiment in real time on the remote terminal, discover problems in time and make adjustments, thereby enhancing the visualization and controllability of the experimental process.

[0099] Preferably, the synthesis reactor 6 comprises a first reactor body and a first stirring rod;

[0100] The first kettle body is a cylindrical barrel structure, the kettle cover is installed on the kettle body, the center of the kettle cover is provided with a stirring port, and the stirring end of the first stirring rod extends into the interior of the first kettle body from the stirring port; the kettle cover is provided with a device port for installing the temperature adjusting assembly;

[0101] The washing reaction kettle 7 includes a second kettle body, a second stirring rod, a pH sensor, and a pressure sensor;

[0102] The second kettle body is a cylindrical barrel structure, the second kettle cover is installed on the second kettle body, the center of the second kettle cover is provided with a stirring port, and the stirring end of the second stirring rod extends into the interior of the second kettle body from the second stirring port; the second kettle cover is provided with a plurality of device ports, and the pH sensor and the pressure sensor are installed on the second kettle cover through corresponding device ports.

[0103] Preferably, the first kettle body and the second kettle body are made of high borosilicate glass material.

[0104] In this embodiment, the synthesis reaction kettle and the washing reaction kettle both adopt a cylindrical barrel structure and are equipped with stirring rods, pH sensors, pressure sensors, and other devices. This structural design helps to improve the uniformity and efficiency of the reaction and washing processes, and facilitates real-time monitoring and control of the environmental parameters in the reaction kettle.

[0105] The first kettle body and the second kettle body are made of high borosilicate glass material, which has good chemical stability and thermal stability, can adapt to various chemical reactions and temperature changes, prolongs the service life of the equipment, and reduces the equipment maintenance cost.

[0106] The kettle cover is provided with a plurality of device ports, which provides convenience for installing various functional components, so that the reaction kettle can be flexibly configured according to different experimental requirements, improving the universality and applicability of the equipment.

[0107] Preferably, the metal compound feeding assembly 2, the organic compound feeding assembly 3, the mixed solvent feeding assembly 4, the acid source feeding assembly 5, and the washing agent feeding assembly 8 all include a peristaltic pump 5, a stock solution storage tank 6, and a solenoid valve. The stock solution storage tank 6 is connected to the inlet of the peristaltic pump 5 through a pipeline, the outlet of the peristaltic pump 5 is connected to the corresponding reaction kettle through a pipeline, and the solenoid valve is installed on the pipeline connecting the peristaltic pump 5 and the corresponding reaction kettle.

[0108] In this embodiment, the metal compound feeding assembly, the organic compound feeding assembly, the mixed solvent feeding assembly, the acid source feeding assembly, and the washing agent feeding assembly all include a peristaltic pump, a stock solution storage tank, and a solenoid valve. This combination can achieve accurate delivery and control of raw materials, ensuring that the raw materials are added to the reaction kettle according to the preset dosage and flow rate, improving the accuracy and repeatability of the experiment.

[0109] Through the cooperation of peristaltic pumps and electromagnetic valves, the automation control of the feeding process is realized, the errors and labor intensity of manual operation are reduced, and the efficiency and safety of the experiment are improved.

[0110] Each feeding assembly is connected with the corresponding reaction kettle through a pipeline to form a complete feeding system, which cooperates with the local controller and other experimental components to improve the integration and synergy of the entire experimental device, making the experimental process more smooth and efficient.

[0111] Preferably, the synthesis reaction kettle 6 and the washing reaction kettle 7 are each provided with a booster pump 9, one end of the booster pump 9 is in communication with the inside of the corresponding synthesis reaction kettle 6 and the washing reaction kettle 7 through a pipeline, and the other end is provided with a gas outlet 10.

[0112] In this embodiment, the synthesis reaction kettle and the washing reaction kettle are each provided with a booster pump, one end of the booster pump is in communication with the inside of the reaction kettle, and the other end is provided with a gas outlet. This design can form a certain pressure environment in the reaction kettle, which helps to improve the reaction speed and washing effect, and the gas outlet can be used to exhaust the gas in the reaction kettle to ensure the stability of the pressure in the reaction kettle.

[0113] With the assistance of the booster pump, the mixing and reaction process of the reactants can be accelerated, the experimental period can be shortened, and the experimental efficiency can be improved, especially in some reactions that require high pressure conditions, the role of the booster pump is particularly significant.

[0114] During the washing process, the booster pump can provide sufficient pressure to ensure that the washing agent and the product are in full contact, improving the uniformity and completeness of the washing process and further improving the purity and quality of the product.

[0115] Preferably, the washing reaction kettle 7 is also provided with a nitrogen purging port 11, which is in communication with the inside of the washing reaction kettle 7 through a pipeline.

[0116] In this embodiment, the washing reaction kettle is provided with a nitrogen purging port, which is in communication with the inside of the washing reaction kettle through a pipeline. Nitrogen purging can remove residual gas and impurities in the reaction kettle during the washing process, prevent impurities from contaminating the product, and improve the purity and quality of the product.

[0117] Nitrogen purging can also play a role in stirring and dispersing during the washing process, further optimizing the washing conditions, improving the washing efficiency and effect, and ensuring the smooth progress of the washing process.

[0118] Preferably, the metal compound is zinc nitrate hexahydrate Zn(NO3)2·6H2O, the organic compound is 4,4'-biphenyldicarboxylic dianhydride H4BTDI, and the mixed solvent is a mixed solvent of dimethylformamide DMF and acetonitrile CH3CN.

[0119] In this embodiment, it is clear that the metal compound is zinc nitrate hexahydrate Zn(NO3)2·6H2O, the organic compound is 4,4'-biphenyldicarboxylic dianhydride H4BTDI, and the mixed solvent is a mixed solvent of dimethylformamide DMF and acetonitrile CH3CN. This specific combination of raw materials is suitable for synthesizing a specific transition metal organic framework material, so that the experimental device has a clear application direction and pertinence.

[0120] According to the properties and reaction requirements of these specific raw materials, the operation parameters and process of the experimental device can be optimized to achieve the best experimental results, improve the yield and quality of the product, and provide effective technical support for related research and application.

[0121] By using these specific raw materials and optimized experimental conditions, the repeatability and reliability of the experimental results can be ensured, and repeated experiments can be easily carried out in different laboratories and at different times, providing a stable experimental basis for scientific research and industrial production.

[0122] Those skilled in the art can clearly understand that, for the convenience and brevity of description, the specific working process of the above-described device and unit can refer to the corresponding process in the foregoing method embodiments, which will not be described here.

[0123] In several embodiments provided in the present application, it should be understood that the disclosed devices and methods can be implemented in other ways. For example, the device embodiments described above are only schematic, for example, the division of units is only a logical function division, and actual implementation can have another division manner, for example, multiple units or components can be combined or integrated into another system, or some features can be ignored or not executed.

[0124] The units described as separate components can or can not be physically separate, and the components displayed as units can or can not be physical units, i.e., they can be located in one place, or distributed on multiple network units.

Claims

1. An automatic control experimental device for the synthesis of transition metal organic frameworks, characterized in that: The invention comprises a local controller (1) and an experimental component, wherein the experimental component comprises a metal compound feeding component (2), an organic compound feeding component (3), a mixed solvent feeding component (4), an acid source feeding component (5), a synthesis reactor (6), a temperature regulating component, a washing reactor (7), a detergent feeding component (8) and a yield analysis component, which are electrically connected to the local controller (1) respectively; The metal compound feed assembly (2), the organic compound feed assembly (3), the mixed solvent feed assembly (4), and the acid source feed assembly (5) are respectively connected to the interior of the synthesis reactor (6) through pipelines, the temperature regulating assembly is installed on the top of the synthesis reactor (6), the synthesis reactor (6) is connected to the washing reactor (7) through a pipeline, and the detergent feed assembly (8) is connected to the washing reactor (7) through a pipeline; The local controller (1) is electrically connected to the remote control terminal and is used to generate control instructions according to the experimental parameters and experimental process information sent by the remote control terminal; The experimental component is used to perform a synthesis reaction according to the control instruction to obtain a preliminary synthesis product, and to wash the synthesis product to obtain a final synthesis product; The yield analysis component is electrically connected to the remote control terminal, and is used to weigh the final synthetic product according to the yield analysis instruction sent by the remote control terminal, and calculate the yield based on the weight of the raw materials and the weight of the final synthetic product to obtain the yield result, and feed the yield result back to the remote control terminal.

2. The automatic control experimental device according to claim 1, characterized in that: According to the control instructions, the synthesis reaction is carried out to obtain the preliminary synthesis product, specifically: The local controller (1) is used to receive experimental parameters and experimental process information from the remote control terminal, and generate raw material injection control instructions based on the experimental parameters; The metal compound feed component (2), the organic compound feed component (3) and the mixed solvent feed component (4) are respectively used to obtain corresponding dosages from the raw material injection control instruction, and inject the stored metal compound, organic compound and mixed solvent into the synthesis reactor (6) according to the corresponding dosages to form a mixture, and send a feeding completion signal to the local controller (1); The local controller (1) is further configured to generate a dissolution control instruction according to a feed completion signal and an experimental process, and send the instruction to the synthesis reactor (6); The synthesis reactor (6) is used to obtain a reaction time from the dissolution treatment control instruction, perform ultrasonic treatment on the mixture according to the reaction time, and send a first-stage reaction completion signal to the local controller (1) when the timing reaches the reaction time; The local controller (1) is further configured to generate an acid drop addition control instruction based on the first-stage reaction completion signal and the experimental process information, and send the instruction to the acid source feeding component (5); The acid source feeding component (5) is used to obtain a corresponding dosage from the acid dropwise addition control instruction, and dropwise add the hydrochloric acid aqueous solution into the synthesis reactor (6) according to the corresponding dosage, and send a dropwise addition completion signal to the local controller (1) when the dropwise addition is completed; The local controller (1) is further configured to generate a temperature control instruction based on the drop addition completion signal and the experimental process information, and send the instruction to the temperature adjustment component; The temperature regulating component is used to obtain a heating temperature value and a heating time from the temperature control instruction, heat the synthesis reactor (6) according to the heating temperature value and the reaction time, monitor the temperature value in the synthesis reactor (6) in real time, regulate the real-time temperature value according to the heating temperature value, cool the synthesis reactor (6) when the reaction time is reached, and obtain a preliminary synthesis product when the temperature in the reactor is about to reach the room temperature.

3. The automatic control experimental device according to claim 2, characterized in that: The synthesized product is subjected to a washing treatment to obtain a final synthesized product, specifically: The temperature regulating component is further used to send a second-stage reaction completion signal to the local controller (1) when the temperature in the kettle is about to reach the room temperature; The local controller (1) is further configured to generate a product transfer control instruction and a detergent feeding instruction according to the second stage reaction completion signal and the experimental process information, and send the instructions to the synthesis reactor (6) and the detergent feeding component (8) respectively; The synthesis reactor (6) is further used to transfer the synthesis product to the washing reactor (7) according to the product transfer control instruction; The detergent feeding component (8) is further used to obtain a corresponding dosage from the detergent feeding instruction, add the detergent into the washing reaction kettle (7) according to the corresponding dosage, and send a adding completion signal to the local controller (1); The local controller (1) is further configured to generate a washing instruction according to the addition completion signal and the experimental process information; The washing reaction kettle (7) is used to obtain a washing time from the washing instruction and wash the preliminary synthesis product according to the washing time, and obtain a final synthesis product when the washing time is reached.

4. The automatic control experimental device according to claim 1, characterized in that: The yield analysis component includes a weigher and an analyzer; The weighing device is used to weigh the final synthesis product according to the yield analysis instruction sent by the remote control terminal to obtain the weight value of the final synthesis product; The analyzer is used to calculate the theoretical yield of the raw material weight according to a preset chemical reaction formula to obtain the theoretical weight, and calculate the theoretical weight and the weight of the final synthetic product based on the yield formula to obtain the yield result. The yield formula is:

5. The automatic control experimental device according to claim 1, characterized in that: The synthesis reaction kettle (6) comprises a first kettle body and a first stirring rod; The first kettle body is a cylindrical barrel structure, the kettle cover is installed on the kettle body, a stirring port is provided at the center of the kettle cover, and the stirring end of the first stirring rod extends into the interior of the first kettle body through the stirring port; the kettle cover is provided with a port for installing the temperature adjustment component; The washing reaction kettle (7) comprises a second kettle body, a second stirring rod, a pH sensor and a pressure sensor; The second kettle body is a cylindrical barrel structure, the second kettle cover is installed on the second kettle body, a stirring port is provided at the center of the second kettle cover, and the stirring end of the second stirring rod extends into the interior of the second kettle body through the second stirring port; The second kettle cover is provided with a plurality of equipment ports, and the pH sensor and the pressure sensor are installed on the second kettle cover through the corresponding equipment ports.

6. The automatic control experimental device according to claim 5, characterized in that: The first kettle body and the second kettle body are made of high borosilicate glass.

7. The automatic control experimental device according to claim 1, characterized in that: The metal compound feed assembly (2), the organic compound feed assembly (3), the mixed solvent feed assembly (4), the acid source feed assembly (5) and the detergent feed assembly (8) all comprise a peristaltic pump (5), a stock solution storage tank (6) and a solenoid valve. The stock solution storage tank (6) is connected to the inlet of the peristaltic pump (5) through a pipeline, and the outlet of the peristaltic pump (5) is connected to the corresponding reactor through a pipeline. The solenoid valve is installed on the pipeline connecting the peristaltic pump (5) and the corresponding reactor.

8. The automatic control experimental device according to claim 1, characterized in that: The synthesis reactor (6) and the washing reactor (7) are both provided with a booster pump (9), one end of the booster pump (9) is connected to the interior of the corresponding synthesis reactor (6) and the washing reactor (7) through a pipeline, and the other end thereof is provided with an air extraction port (10).

9. The automatic control experimental device according to claim 8, characterized in that: The washing reactor (7) is also provided with a nitrogen purge port (11), and the nitrogen purge port (11) is communicated with the interior of the washing reactor (7) through a pipeline.

10. The automatic control experimental device according to any one of claims 1 to 9, characterized in that: The metal compound is zinc nitrate hexahydrate Zn(NO3)2·6H2O, the organic compound is 4,4'-biphenyldicarboxylic dianhydride H4BTDI, and the mixed solvent is a mixed solvent of dimethylformamide DMF and acetonitrile CH3CN.

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