High-throughput automated polymer material development system and control method thereof

Abstract

The application discloses a kind of high-throughput automation high polymer material development system and control method thereof, which can prepare different groups of samples simultaneously, and adjust process parameters to reduce production cost according to the performance results of samples. The high-throughput automation high polymer material development system includes a first automatic weighing feeding device, a polymer resin preparation device, a polymer material compounding device and a second automatic weighing feeding device. It also includes an industrial control system and a polymer material rheological testing device. The control method includes the following steps: S1, establishing a control relationship; S2, setting the processing parameters to produce polymer materials; S3, detecting and analyzing the performance of polymer materials; S4, automatically adjusting the processing parameters; S5, continuously producing new polymer materials; S6, obtaining the final polymer material sample and saving the corresponding processing parameters. The high-throughput automation high polymer material development system and its control method can improve development efficiency and reduce development cost.

Description

Technical Field

[0001] This invention relates to the field of polymer material development, and in particular to a high-throughput automated polymer material development system. Background Technology

[0002] Materials innovation has always been at the heart of technological progress. However, traditionally, the discovery and use of materials have relied on luck, scientific intuition, or trial and error, resulting in significant uncertainty. Materials genome engineering technology offers a new model for developing new materials, not only shortening the R&D cycle but also reducing costs. High-throughput synthesis and characterization experiments form the foundation of this technology, enabling the preparation of large numbers of samples in a short time. Specifically, intelligent control terminals are used to input experimental instructions and retrieve tasks to complete the experimental workflow, automatically completing formulation and process design to obtain products. This achieves full automation of the high-throughput experimental process, enabling intelligent data processing, optimal option selection, and experimental report generation.

[0003] Currently, high-throughput synthesis and characterization experiments mainly focus on the development of small molecule materials such as pharmaceuticals. Due to their complex molecular structures, large molecular weights, high viscosity, and diverse aggregation states, polymer materials present challenges such as complex reaction processes, high reaction control requirements, and significant difficulties in equipment development. Summary of the Invention

[0004] The technical problem to be solved by the present invention is to provide a high-throughput automated polymer material development system that can simultaneously prepare different groups of samples and adjust process parameters based on the performance results of the samples to reduce manufacturing costs and improve development efficiency.

[0005] The technical solution adopted by this invention to solve its technical problem is: a high-throughput automated polymer material development system, including a first automatic weighing and feeding device, a polymer resin preparation device, a polymer material composite device, and a second automatic weighing and feeding device; it also includes an industrial control system and a polymer material testing device;

[0006] The first automatic weighing and feeding device, the polymer resin preparation device, and the polymer material composite device are arranged in sequence; the feed inlet of the polymer material composite device is equipped with a second automatic weighing and feeding device.

[0007] The polymer material composite device includes a melt extrusion device and a polymer material forming device; the polymer material testing device is used to detect the properties of the polymer material in the molten state in the melt extrusion device; the outlet of the polymer material forming device is equipped with a sample collection device;

[0008] The industrial control system is used to receive the properties of polymer materials detected by the polymer material testing device; and to adjust the automatic quantitative control of the first automatic weighing and feeding device and the second automatic weighing and feeding device, as well as the process parameters of the polymer resin preparation device and the polymer material composite device according to the detected properties of polymer materials.

[0009] The sample collection device is electrically connected to the industrial control system, and the sample collection is controlled by the industrial control system.

[0010] Specifically, the sample collection device employs a robotic arm automatic collection device.

[0011] Specifically, the process parameters of the polymer resin preparation device include reaction temperature, reaction pressure, and reaction time; the process parameters of the polymer material composite device include composite process temperature, rotation speed, and time.

[0012] Specifically, the polymer material testing device includes a torque rheometer, a differential scanning calorimeter, and a tensile tester.

[0013] Specifically, the industrial control system adopts a centralized control system.

[0014] Specifically, the first automatic weighing and feeding device and the second automatic weighing and feeding device are gravity-type continuous automatic loading scales.

[0015] Specifically, the polymer resin preparation device is a reaction vessel.

[0016] Specifically, the polymer material composite device uses a twin-screw or multi-screw extruder.

[0017] This invention also provides a control method for a high-throughput automated polymer material development system, employing an industrial control system; the industrial control system includes an industrial computer; and further includes the following steps:

[0018] S1. Establish control relationships;

[0019] Establish the correspondence between various properties of polymer materials and various processing parameters in an industrial computer; the process parameters include the amount of each component raw material added, the amount of catalyst added, the amount of additive added, the reaction parameters of the polymer resin preparation device, and the reaction parameters of the polymer material composite device.

[0020] S2. Set processing parameters to produce polymer materials;

[0021] The target performance parameters of the polymer material are set, and the industrial computer, based on the received target performance parameters of the polymer material, sets the automatic quantitative parameters of the first automatic weighing and feeding device and the second automatic weighing and feeding device, as well as the process parameters of the polymer resin preparation device and the polymer material composite device to produce the polymer material.

[0022] S3. Performance testing and analysis of polymer materials;

[0023] The performance parameters of the polymer material obtained by the polymer material composite device are detected by the polymer material testing device; the detected performance parameters are transmitted to the industrial control system; the industrial control system compares the detected performance parameters with the target performance parameters and obtains feedback results.

[0024] S4. Automatic adjustment of processing parameters;

[0025] The industrial control system adjusts the automatic quantitative control of the first automatic weighing and feeding device and the second automatic weighing and feeding device, as well as the process parameters of the polymer resin preparation device and the polymer material composite device, based on the feedback results obtained in step S3.

[0026] S5. Continuous production of new polymer materials;

[0027] New polymer materials are prepared by a polymer resin preparation device and a polymer material composite device according to the re-set processing parameters in step S4, and the performance parameters of the new polymer materials are detected by a polymer material testing device.

[0028] S6. Obtain the final polymer material sample and save the corresponding processing parameters;

[0029] The new performance parameters obtained in step S5 are compared with the target performance parameters. If the performance parameters are different from the target performance parameters, steps S3, S4, and S5 are repeated until the actual detected polymer performance parameters are the same as the target performance parameters. Then, the data is saved through an industrial computer and stored in a database, replacing the processing parameters corresponding to the original target performance parameters.

[0030] The beneficial effects of the present invention are as follows: The high-throughput automated polymer material development system of the present invention forms an automated production line by making polymer material sample preparation equipment, and through the control method of the high-throughput automated polymer material development system of the present invention, polymer material sample preparation can be carried out automatically and continuously; thus, it can improve the efficiency of sample preparation and reduce costs.

[0031] Secondly, the high-throughput automated polymer material development system described in this application simplifies the steps of polymer material performance testing and improves efficiency by setting up polymer material testing equipment to detect various properties of polymer materials.

[0032] Furthermore, by using an industrial control system to monitor the performance parameters of polymer materials detected by the polymer material testing device, the process parameters of the production equipment can be adjusted in real time. This avoids the problem of each sample having to complete the entire process, which would otherwise result in an excessively long polymer material development cycle. This approach can effectively improve development efficiency and reduce development costs.

[0033] The control method of the high-throughput automated polymer material development system described in this application can realize automated control of equipment, intelligent development of polymer materials, improve development efficiency, and reduce costs. Attached Figure Description

[0034] Figure 1 This is a schematic diagram of the structure of the high-throughput automated polymer material development system in an embodiment of the present invention;

[0035] Figure 2 This is a schematic diagram illustrating the working principle of the high-throughput automated polymer material development system in this embodiment of the invention;

[0036] Figure 3 This is a flowchart of the control method for a high-throughput automated polymer material development system in an embodiment of the present invention;

[0037] Icon markings: 100 - First automatic weighing and feeding device, 200 - Polymer resin preparation device, 300 - Polymer material composite device, 400 - Second automatic weighing and feeding device, 500 - Polymer material testing device, 600 - Sample collection device, 700 - Industrial control system. Detailed Implementation

[0038] The present invention will be further described below with reference to the accompanying drawings and embodiments.

[0039] like Figure 1 As shown, the high-throughput automated polymer material development system includes a first automatic weighing and feeding device 100, a polymer resin preparation device 200, a polymer material composite device 300, and a second automatic weighing and feeding device 400; it also includes an industrial control system 700 and a polymer material testing device 500.

[0040] The main function of the first automatic weighing and feeding device 100 is to quantitatively add raw materials for resin preparation and to quantitatively add catalysts. The main function of the polymer resin preparation device 200 is to prepare resin from raw materials. The polymer material composite device 300 is used to react resin and additives to form polymer composite materials. The main function of the polymer material testing device 500 is to perform performance testing on polymer materials in the molten state.

[0041] The first automatic weighing and feeding device 100, the polymer resin preparation device 200, and the polymer material composite device 300 are arranged in sequence; the feed inlet of the polymer material composite device 300 is provided with a second automatic weighing and feeding device 400.

[0042] The polymer composite device 300 includes a melt extrusion device 310 and a polymer molding device 320; the polymer testing device 500 is used to detect the properties of the polymer material in the molten state in the melt extrusion device 310; and the outlet of the polymer molding device 320 is provided with a sample collection device 600.

[0043] Specifically, the polymer material testing device 500 includes a torque rheometer, a differential scanning calorimeter, and a tensile tester. The polymer material testing device 500 can detect the rheological properties, melting point, heat distortion temperature, tensile strength, and tensile modulus of the sample.

[0044] The first automatic weighing and feeding device 100 and the second automatic weighing and feeding device 400 are gravity-type continuous automatic loading scales.

[0045] The polymer resin preparation device 200 is a reaction vessel.

[0046] The polymer material composite device 300 adopts a twin-screw or multi-screw extruder.

[0047] The industrial control system 700 is used to receive the polymer material properties detected by the polymer material testing device 500; and to adjust the automatic quantitative control of the first automatic weighing and feeding device 100 and the second automatic weighing and feeding device 400, as well as the process parameters of the polymer resin preparation device 200 and the polymer material composite device 300, based on the detected polymer material properties; specifically, the industrial control system 700 adopts a centralized control system. The process parameters of the polymer resin preparation device 200 include reaction temperature, reaction pressure, and reaction time; the process parameters of the polymer material composite device 300 include composite process temperature, rotation speed, and time.

[0048] The sample collection device 600 is electrically connected to the industrial control system 700, and the sample collection is controlled by the industrial control system 700.

[0049] like Figure 2 As shown, the specific work process is as follows:

[0050] A fixed amount of monomer resin raw materials and catalyst are weighed by the first automatic weighing and feeding device 100 and the second automatic weighing and feeding device 400, and fed into the polymer resin reaction equipment 200 through the feeding device. The reaction is carried out at a set temperature and pressure for a fixed time to obtain a high molecular weight polymer resin material. The polymer material melt is added to the polymer material composite equipment 300 through an interface, and a fixed amount of additives are added through the second automatic weighing and feeding device 400. The temperature and pressure of the polymer material composite equipment 300 are set to prepare the polymer material. The material is then cooled by strands, and a portion of the polymer material is sent to the polymer material testing device 500 to obtain performance parameters. The remaining polymer material is collected by the sample collection device 600, automatically labeled, and stored. The industrial control system 700 stores and analyzes the performance parameters obtained from the testing device, determines the parameters that need adjustment, sets the parameters, and performs the next iteration.

[0051] In one feasible embodiment, for ease of control, the sample collection device 600 further employs a robotic arm automatic collection device.

[0052] This invention also provides a control method for the high-throughput automated polymer material development system, employing an industrial control system; the industrial control system 700 includes an industrial computer; specifically as follows... Figure 3 As shown, it also includes the following steps:

[0053] S1. Establish control relationships;

[0054] Establish the correspondence between various properties of polymer materials and various processing parameters in an industrial computer; the process parameters include the amount of each component raw material added, the amount of catalyst added, the amount of additive added, the reaction parameters of the polymer resin preparation device 200 and the reaction parameters of the polymer material composite device 300.

[0055] S2. Set processing parameters to produce polymer materials;

[0056] The target performance parameters of the polymer material are set, and the industrial computer sets the automatic quantitative parameters of the first automatic weighing and feeding device 100 and the second automatic weighing and feeding device 400, as well as the process parameters of the polymer resin preparation device 200 and the polymer material composite device 300 to produce the polymer material.

[0057] S3. Performance testing and analysis of polymer materials;

[0058] The polymer material performance parameters obtained from the polymer material composite device 300 are detected by the polymer material testing device 500; the detected performance parameters are transmitted to the industrial control system 700; the industrial control system 700 compares the detected performance parameters with the target performance parameters and obtains feedback results.

[0059] S4. Automatic adjustment of processing parameters;

[0060] The industrial control system 700 adjusts the automatic quantitative control of the first automatic weighing and feeding device 100 and the second automatic weighing and feeding device 400, as well as the process parameters of the polymer resin preparation device 200 and the polymer material composite device 300, based on the feedback results obtained in step S3.

[0061] S5. Continuous production of new polymer materials;

[0062] According to the processing parameters reset in step S4, a new polymer material is prepared by the polymer resin preparation device 200 and the polymer material composite device 300, and the performance parameters of the new polymer material are detected by the polymer material testing device 500.

[0063] S6. Obtain the final polymer material sample and save the corresponding processing parameters;

[0064] The new performance parameters obtained in step S5 are compared with the target performance parameters. If the performance parameters are different from the target performance parameters, steps S3, S4, and S5 are repeated until the actual detected polymer performance parameters are the same as the target performance parameters. Then, the data is saved through an industrial computer and stored in a database, replacing the processing parameters corresponding to the original target performance parameters.

[0065] Example

[0066] Poly(hexamethylene terephthalamide) / polyamide 66-glass fiber PA6T / 66-GF material was prepared using the high-throughput automated polymer material development system and control method described in this invention. The material has a tensile strength of 200 MPa, a tensile modulus of 7.3 GPa, a melting point of 305 °C, and a heat distortion temperature of 180 °C.

[0067] The monomers required for the synthesis of poly(hexamethylene terephthalamide) / polyamide 66-glass fiber PA6T / 66-GF material are terephthalic acid, adipic acid, and hexamethylenediamine. The catalyst is sodium hypophosphite, and the additive required is glass fiber.

[0068] Includes the following steps:

[0069] 1. Establish control relationships

[0070] Establish the correspondence between various properties of polymer materials and various processing parameters in an industrial computer; the process parameters include the amount of each component raw material added, the amount of catalyst added, the amount of additive added, the reaction parameters of the polymer resin preparation device 200 and the reaction parameters of the polymer material composite device 300.

[0071] Specifically, the adjustment relationship between polymer material performance parameters and processing parameters is as follows:

[0072] If the material has a low melting point, increase the terephthalic acid content; if the rheological properties are poor, increase the oxalic acid content; if the material has low viscosity, adjust the amount of catalyst; if the mechanical properties are low, increase the glass fiber content of the additives; if the torque of the polymer composite equipment is too high, increase the processing temperature of the polymer composite equipment; if there are black spots or bubbles in the material, adjust the system temperature and pressure.

[0073] 2. Setting processing parameters for the production of polymer materials

[0074] The target performance parameters of the polymer material are set, and the industrial computer sets the automatic quantitative parameters of the first automatic weighing and feeding device 100 and the second automatic weighing and feeding device 400, as well as the process parameters of the polymer resin preparation device 200 and the polymer material composite device 300 to produce the polymer material.

[0075] Specifically, a certain amount of monomer resin raw materials and catalyst are weighed by the first automatic weighing and feeding device 100 and the second automatic weighing and feeding device 400. In the supplementary embodiment, terephthalic acid, adipic acid, and hexamethylenediamine are weighed to 6.6 kg, 8.7 kg, and 12.8 kg, respectively, and fed into the polymer resin reaction equipment 200 through the feeding device. The reaction is carried out at a set temperature of 280°C and a pressure of 0.1 MPa for 20 minutes to obtain a high molecular weight polymer resin material. The polymer material melt is then added to the polymer material composite equipment 300 through the interface.

[0076] A fixed amount of additives are added through the second automatic weighing and feeding device 400. The glass fiber is weighed to 11.3 kg. The temperature and pressure of the polymer composite equipment 300 are set, and the polymer material is prepared under the step temperature increase condition of 300℃-320℃, followed by strand cooling.

[0077] 3. Performance testing and analysis of polymer materials

[0078] The performance parameters of the polymer material obtained from the polymer composite device 300 are detected by a polymer material testing device 500. The detected performance parameters are transmitted to an industrial control system 700. The industrial control system 700 compares the detected performance parameters with the target performance parameters and obtains feedback results. The polymer material testing device 500 detected the following performance parameters for the obtained polymer material: tensile strength 180 MPa, tensile modulus 6.7 GPa, melting point 280℃, and heat distortion temperature 160℃. Since the performance parameters of the prepared polymer material are inconsistent with the target parameters, the processing parameters are adjusted in real time in subsequent steps.

[0079] 4. Automatic adjustment of processing parameters

[0080] The industrial control system 700 adjusts the weighing of terephthalic acid, adipic acid, and hexamethylenediamine in the first automatic weighing and feeding device 100 to 8.4 kg, 7.3 kg, and 12.5 kg, respectively, based on the feedback results obtained in step 3. It maintains the reaction temperature of the polymer resin preparation device 200 at 290°C, the pressure at 0.1 MPa, and the reaction time at 20 minutes. The automatic quantitative weighing of glass fiber in the second automatic weighing and feeding device 400 is adjusted to 12.5 kg, and the temperature of the polymer material composite device 300 is adjusted to 325-330°C.

[0081] 5. Continuous production of new polymer materials

[0082] According to the re-set processing parameters in step 4, resin is prepared by the polymer resin preparation device 200. Terephthalic acid, adipic acid, and hexamethylenediamine are added to the polymer resin preparation device 200 and reacted for 20 minutes at a set temperature of 290℃ and a pressure of 0.1 MPa. The automatic quantitative glass fiber weighing device 400 is adjusted to 12.5 kg, and other parameters remain consistent with step 4. A new polymer material is prepared by the polymer material composite device 300. The performance parameters of the new polymer material are tested by the polymer material testing device 500: tensile strength 200 MPa, tensile modulus 7.3 GPa, melting point 305℃, and heat distortion temperature 180℃. The performance parameters of this polymer material are consistent with the target parameters, therefore no process parameter adjustment is required, and production continues with the corresponding process parameters maintained.

[0083] 6. Obtain the final polymer material sample and save the corresponding processing parameters.

[0084] Compare the new performance parameters obtained in step 5 with the target performance parameters. If the performance parameters are different from the target performance parameters, repeat steps 3, 4, and 5 until the actual detected polymer performance parameters are the same as the target performance parameters. Then, save the data through an industrial computer, store it in the database, and replace the processing parameters corresponding to the original target performance parameters.

Claims

1. A high-throughput automated polymer material development system, comprising a first automatic weighing and feeding device (100), a polymer resin preparation device (200), a polymer material composite device (300), and a second automatic weighing and feeding device (400); characterized in that: It also includes an industrial control system (700) and a polymer material testing device (500); The first automatic weighing and feeding device (100), the polymer resin preparation device (200), and the polymer material composite device (300) are arranged in sequence; the feed inlet of the polymer material composite device (300) is provided with a second automatic weighing and feeding device (400); The polymer composite device (300) includes a melt extrusion device (310) and a polymer molding device (320); the polymer testing device (500) is used to detect the performance of the polymer material in the melt state in the melt extrusion device (310); the polymer molding device (320) is provided with a sample collection device (600) at the discharge port; The industrial control system (700) is used to receive the polymer material properties detected by the polymer material testing device (500); and to adjust the automatic quantitative control of the first automatic weighing and feeding device (100) and the second automatic weighing and feeding device (400) as well as the process parameters of the polymer resin preparation device (200) and the polymer material composite device (300) according to the detected polymer material properties. The sample collection device (600) is electrically connected to the industrial control system (700), and the sample collection is controlled by the industrial control system (700). The process parameters of the polymer resin preparation device (200) include reaction temperature, reaction pressure, and reaction time; the process parameters of the polymer material composite device (300) include composite process temperature, rotation speed, and time. The polymer material testing device (500) includes a torque rheometer, a differential scanning calorimeter, and a tensile tester.

2. The high-throughput automated polymer material development system as described in claim 1, characterized in that: The sample collection device (600) adopts an automatic collection device with a robotic arm.

3. The high-throughput automated polymer material development system as described in any one of claims 1 or 2, characterized in that: The industrial control system (700) adopts a centralized control system.

4. The high-throughput automated polymer material development system as described in claim 3, characterized in that: The first automatic weighing and feeding device (100) and the second automatic weighing and feeding device (400) are gravity-type continuous automatic loading scales.

5. The high-throughput automated polymer material development system as described in claim 4, characterized in that: The polymer resin preparation device (200) is a reaction vessel.

6. The high-throughput automated polymer material development system as described in claim 3, characterized in that: The polymer composite device (300) adopts a twin-screw or multi-screw extruder.

7. A control method for the high-throughput automated polymer material development system as described in any one of claims 1 to 6, wherein an industrial control system is used for control; Its features are: The industrial control system (700) includes an industrial computer; it also includes the following steps: S1. Establish control relationships; Establish the correspondence between various properties of polymer materials and various processing parameters in an industrial computer; the process parameters include the amount of each component raw material added, the amount of catalyst added, the amount of additive added, the reaction parameters of the polymer resin preparation device (200) and the reaction parameters of the polymer material composite device (300). S2. Set processing parameters to produce polymer materials; The target performance parameters of the polymer material are set. The industrial computer, through the received target performance parameters of the polymer material, sets the automatic quantitative parameters of the first automatic weighing and feeding device (100) and the second automatic weighing and feeding device (400), as well as the process parameters of the polymer resin preparation device (200) and the polymer material composite device (300) to produce the polymer material. S3. Performance testing and analysis of polymer materials; The polymer material performance parameters obtained by the polymer material composite device (300) are detected by the polymer material testing device (500); the detected performance parameters are transmitted to the industrial control system (700); the industrial control system (700) compares the detected performance parameters with the target performance parameters and obtains feedback results. S4. Automatic adjustment of processing parameters; The industrial control system (700) adjusts the automatic quantitative control of the first automatic weighing and feeding device (100) and the second automatic weighing and feeding device (400) as well as the process parameters of the polymer resin preparation device (200) and the polymer material composite device (300) based on the feedback results obtained in step S3. S5. Continuous production of new polymer materials; According to the processing parameters reset in step S4, a new polymer material is prepared by the polymer resin preparation device (200) and the polymer material composite device (300), and the performance parameters of the new polymer material are detected by the polymer material testing device (500). S6. Obtain the final polymer material sample and save the corresponding processing parameters; The new performance parameters obtained in step S5 are compared with the target performance parameters. If the performance parameters are different from the target performance parameters, steps S3, S4, and S5 are repeated until the actual detected polymer performance parameters are the same as the target performance parameters. Then, the data is saved through an industrial computer and stored in a database, replacing the processing parameters corresponding to the original target performance parameters.

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