High-flux automatic high polymer material development system and control method thereof

Abstract

The invention discloses a high-throughput automatic high polymer material development system and a control method thereof, which can be used for simultaneously preparing different groups of samples and adjusting process parameters to reduce the manufacturing cost according to performance result feedback of the samples. The high-flux automatic high polymer material development system comprises a first automatic weighing and feeding device, a high polymer resin preparation device, a high polymer material compounding device and a second automatic weighing and feeding device, the device further comprises an industrial control system and a high polymer material rheological testing device. The control method comprises the following steps: S1, establishing a control relationship; s2, setting processing technological parameters to produce a high polymer material; s3, detecting and analyzing the performance of the high polymer material; s4, automatically adjusting machining process parameters; s5, continuously producing a new high polymer material; and S6, obtaining a final high polymer material sample, and storing corresponding processing technological parameters. By adopting the high-flux automatic high polymer material development system and the control method thereof, the development efficiency can be improved, and the development cost can be reduced.

Description

Technical Field

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

[0002] Material innovation has always been the core of technological innovation. However, traditionally, the discovery and use of materials rely on luck, scientific intuition, or trial and error, and there is a lot of uncertainty. Material genetic engineering technology is a new model for developing new materials, which not only shortens the R&D cycle, but also reduces R&D costs. High-throughput synthesis and characterization experiments are the basis of the technology, which can complete the preparation of a large number of samples in a short time. Specifically, it is an intelligent control terminal, which is used to input experimental instructions, and call tasks according to the experimental instructions to complete the experimental workflow, automatically complete the formulation and process design, obtain the product, realize the automation of the entire process of high-throughput experiments, and realize intelligent data processing, optimal option screening and experimental report generation.

[0003] At present, high-throughput synthesis and characterization experiments are mainly concentrated in the field of small molecule material development such as drugs. Due to the complex molecular structure, large molecular weight, high viscosity, and diverse aggregation states, polymer materials have complex reaction processes, difficult reaction control, and difficult 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 prepare different groups of samples at the same time and adjust process parameters according to the performance feedback of the samples to reduce production costs and improve development efficiency.

[0005] The technical solution adopted by the present invention to solve the 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 compounding device and a second automatic weighing and feeding device; and also including 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 compounding device are arranged in sequence; the feeding port of the polymer material compounding device is provided with a second automatic weighing and feeding device;

[0007] The polymer material composite device comprises a melt extrusion device and a polymer material molding device; the polymer material testing device is used to detect the performance of the polymer material in a molten state in the melt extrusion device; the polymer material molding device is provided with a sample collection device at the discharge port;

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

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

[0010] Specifically, the sample collecting device adopts a robotic arm automatic collecting 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 adopt gravity-type continuous automatic loading scales.

[0015] Specifically, the polymer resin preparation device adopts a reaction kettle device.

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

[0017] The present invention also provides a control method for a high-throughput automated polymer material development system, which is controlled by an industrial control system; the industrial control system includes an industrial computer; and further includes the following steps:

[0018] S1. Establish control relationship;

[0019] Establishing the corresponding relationship between each performance of the polymer material and each processing parameter in the industrial computer; the process parameters include the addition amount of each component raw material, the addition amount of the catalyst, the addition amount of the additive, the reaction parameters of the polymer resin preparation device and the reaction parameters of the polymer material composite device;

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

[0021] Setting target performance parameters of polymer materials. The industrial computer sets the automatic quantitative parameters of the first automatic weighing and feeding device, the second automatic weighing and feeding device, and the process parameters of the polymer resin preparation device and the polymer material compounding device to produce the polymer materials according to the received target performance parameters of the polymer materials;

[0022] S3. Testing and analysis of polymer material performance;

[0023] Testing the performance parameters of the polymer material obtained by the polymer material composite device through the polymer material testing device; transmitting the detected performance parameters to the industrial control system; the industrial control system compares the detected performance parameters with the target performance parameters to obtain feedback results;

[0024] S4, automatic adjustment of processing parameters;

[0025] The industrial control system adjusts the automatic quantitative measurement of the first automatic weighing and feeding device, the second automatic weighing and feeding device, and the process parameters of the polymer resin preparation device and the polymer material composite device according to the feedback result obtained in step S3;

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

[0027] According to the processing parameters reset in step S4, a new polymer material is prepared by the polymer resin preparation device and the polymer material composite device, and the performance parameters of the new polymer material are tested by the 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 polymer performance parameters actually detected are the same as the target performance parameters; the data is then saved through an industrial computer; stored in a database, and the processing parameters corresponding to the original target performance parameters are replaced.

[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 with equipment for making polymer material samples, and through the control method of the high-throughput automated polymer material development system of the present invention, the preparation of polymer material samples can be carried out automatically and continuously; therefore, the efficiency of sample making can be improved and the cost can be reduced.

[0031] Secondly, the high-throughput automated polymer material development system described in the present application realizes the detection of various properties of polymer materials by setting up polymer material testing equipment, thereby simplifying the steps of polymer material performance detection and improving efficiency;

[0032] Thirdly, the industrial control system can adjust the process parameters of the production equipment in real time based on the polymer material performance parameters detected by the polymer material testing device, thereby avoiding the problem of each sample having to complete the entire process, which causes the polymer material development cycle to be too long. This can effectively improve development efficiency and reduce development costs.

[0033] The control method of the high-throughput automated polymer material development system described in the present application can realize automated control of equipment, achieve intelligent development of polymer materials, improve development efficiency, and reduce costs. BRIEF DESCRIPTION OF THE DRAWINGS

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

[0035] Figure 2 Schematic diagram of the working principle of the high-throughput automated polymer material development system in an embodiment of the present invention;

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

[0037] The diagram indicates: 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 DESCRIPTION

[0038] The present invention is further described below in conjunction with 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 compounding device 300 and a second automatic weighing and feeding device 400; and 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 realize the quantitative addition of raw materials for preparing resin and the quantitative addition of catalyst. The main function of the polymer resin preparation device 200 is to realize the preparation of raw materials to resin. The polymer material composite device 300 is a polymer composite material formed by the reaction of resin and additives. The main function of the polymer material testing device 500 is to realize the performance detection of polymer materials in a 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 port of the polymer material composite device 300 is provided with a second automatic weighing and feeding device 400;

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

[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 deformation 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 adopts a reaction kettle device.

[0046] The polymer material compounding 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; adjust the automatic quantitative of the first automatic weighing and feeding device 100 and the second automatic weighing and feeding device 400 and the process parameters of the polymer resin preparation device 200 and the polymer material composite device 300 according to 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 is controlled by the industrial control system 700 to collect samples.

[0049] like Figure 2 As shown in the specific working process:

[0050] The first automatic weighing and feeding device 100 and the second automatic weighing and feeding device 400 are used to weigh a certain amount of monomer resin raw materials and catalysts, and are fed into the polymer resin reaction equipment 200 through the feeding device, and react for a fixed time at the set temperature and pressure to obtain a high molecular weight polymer resin material, and the polymer material melt is added to the polymer material composite equipment 300 through the interface, and a certain amount of additives are added through the second automatic weighing and feeding device 400, and the temperature and pressure of the polymer material composite equipment 300 are set to prepare the polymer material, and the wire is cooled, and part of the polymer material is sent to the polymer material testing device 500 for detection to obtain performance parameters, and the remaining polymer material is collected by the sample collection device 600, and automatically labeled and stored. The industrial control system 700 stores the performance parameters obtained by the test device, analyzes, obtains the parameters that need to be adjusted, and sets the parameters for the next iteration.

[0051] In a feasible embodiment, in order to facilitate control, further, the sample collection device 600 adopts a robotic arm automatic collection device.

[0052] The present invention also provides a control method for the high-throughput automated polymer material development system, which is controlled by an industrial control system; the industrial control system 700 includes an industrial computer; specifically, Figure 3 As shown, the following steps are also included:

[0053] S1. Establish control relationship;

[0054] Establishing the corresponding relationship between each performance of the polymer material and each processing parameter in the industrial computer; the process parameters include the addition amount of each component raw material, the addition amount of the catalyst, the addition amount of the additive, the reaction parameters of the polymer resin preparation device 200 and the reaction parameters of the polymer material composite device 300;

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

[0056] Setting target performance parameters of the polymer material. 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 and the process parameters of the polymer resin preparation device 200 and the polymer material composite device 300 to produce the polymer material according to the received target performance parameters of the polymer material;

[0057] S3. Testing and analysis of polymer material performance;

[0058] The polymer material testing device 500 detects the performance parameters of the polymer material obtained by the polymer material composite device 300; 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 to obtain feedback results;

[0059] S4, automatic adjustment of processing parameters;

[0060] The industrial control system 700 adjusts the automatic quantitative of the first automatic weighing and feeding device 100 and the second automatic weighing and feeding device 400 and the process parameters of the polymer resin preparation device 200 and the polymer material composite device 300 according to the feedback result 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 tested 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 polymer performance parameters actually detected are the same as the target performance parameters; the data is then saved through an industrial computer; stored in a database, and the processing parameters corresponding to the original target performance parameters are replaced.

[0065] Example

[0066] The high-throughput automated polymer material development system and control method of the present invention are used to prepare poly(hexamethylene terephthalamide) / polyamide 66-glass fiber PA6T / 66-GF material with a tensile strength of 200 MPa, a tensile modulus of 7.3 GPa, a melting point of 305°C, and a heat deformation temperature of 180°C.

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

[0068] The following steps are involved:

[0069] 1. Establish a control relationship

[0070] Establishing the corresponding relationship between each performance of the polymer material and each processing parameter in the industrial computer; the process parameters include the addition amount of each component raw material, the addition amount of the catalyst, the addition amount of the additive, the reaction parameters of the polymer resin preparation device 200 and the reaction parameters of the polymer material composite device 300;

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

[0072] The melting point of the material is low, so increase the content of terephthalic acid; poor rheological properties will increase the content of oxalic acid; the viscosity of the material is low, so adjust the amount of catalyst; low mechanical properties, increase the content of additive glass fiber; the torque of the polymer material composite equipment is too large, so increase the processing temperature of the polymer material composite equipment; there are black spots, bubbles and other phenomena in the material, so adjust the system temperature and pressure.

[0073] 2. Set processing parameters to produce polymer materials

[0074] Setting target performance parameters of the polymer material. 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 and the process parameters of the polymer resin preparation device 200 and the polymer material composite device 300 to produce the polymer material according to the received target performance parameters of the polymer material;

[0075] Specifically, a certain amount of monomer resin raw materials and catalysts are weighed through 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 specifically weighed at 6.6 Kg, 8.7 Kg and 12.8 Kg, and are fed into the polymer resin reaction equipment 200 through the feeding device. The reaction is carried out for 20 minutes at a set temperature of 280°C and a pressure of 0.1MP to obtain a high molecular weight polymer resin material, and the polymer material melt is added to the polymer material composite equipment 300 through the interface.

[0076] A quantitative amount of additives is added through the second automatic weighing and feeding device 400, and the glass fiber is specifically weighed 11.3 kg. The temperature and pressure of the polymer material composite equipment 300 are set, and the polymer material is prepared under the condition of a step-by-step temperature increase of 300° C.-320° C., and the pull rod is cooled.

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

[0078] The polymer material testing device 500 detects the performance parameters of the polymer material obtained by the polymer material composite device 300; 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 to obtain feedback results. The polymer material testing device 500 detects that the performance parameters of the obtained polymer material are: tensile strength 180MPa, tensile modulus 6.7GPa, melting point 280℃, and thermal deformation temperature 160℃. Since the performance parameters of the prepared polymer material are inconsistent with the target parameters; therefore, the processing parameters are adjusted in real time in the subsequent steps.

[0079] 4. Automatic adjustment of processing parameters

[0080] The industrial control system 700 adjusts the weights of terephthalic acid, adipic acid and hexamethylenediamine in the first automatic weighing and feeding device 100 to 8.4Kg, 7.3Kg and 12.5Kg according to the feedback results obtained in step 3, and maintains the reaction temperature of the polymer resin preparation device 200 at 290°C, the pressure at 0.1MP and the reaction time at 20 minutes; the specific weighing of the automatic quantitative glass fiber of the second automatic weighing and feeding device 400 is adjusted to 12.5Kg, 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 processing parameters reset in step 4; prepare resin by polymer resin preparation device 200, load terephthalic acid, adipic acid and hexamethylenediamine into polymer resin preparation device 200, react for 20 minutes at set temperature 290°C and pressure 0.1MP, adjust the specific weighing of automatic quantitative glass fiber of second automatic weighing and feeding device 400 to 12.5Kg, and keep the other parameters consistent with step 4, prepare new polymer material by polymer material composite device 300, and test the performance parameters of new polymer material by polymer material testing device 500, tensile strength 200MPa, tensile modulus 7.3GPa, melting point 305°C, thermal deformation temperature 180°C. The performance parameters of the polymer material are consistent with the target parameters, so there is no need to adjust the process parameters, and keep the corresponding process parameters to continue production.

[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 polymer performance parameters actually detected are the same as the target performance parameters; then save the data through an industrial computer; store it in a 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 compounding device (300) and a second automatic weighing and feeding device (400); characterized in that: Also included is 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 port of the polymer material composite device (300) is provided with a second automatic weighing and feeding device (400); The polymer material composite device (300) comprises a melt extrusion device (310) and a polymer material forming device (320); the polymer material testing device (500) is used to detect the performance of the polymer material in a molten state in the melt extrusion device (310); the polymer material forming device (320) is provided with a sample collecting device (600) at the material outlet; The industrial control system (700) is used to receive polymer material properties detected by a polymer material testing device (500); and to adjust the automatic quantitative control of a first automatic weighing and feeding device (100) and a second automatic weighing and feeding device (400) as well as process parameters of a polymer resin preparation device (200) and a 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).

2. The high-throughput automated polymer material development system according to claim 1, characterized in that: The sample collection device (600) is an automatic collection device using a robotic arm.

3. The high-throughput automated polymer material development system according to claim 1, characterized in that: 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.

4. The high-throughput automated polymer material development system according to claim 3, characterized in that: The polymer material testing device (500) comprises a torque rheometer, a differential scanning calorimeter, and a tensile tester.

5. The high-throughput automated polymer material development system according to any one of claims 1 to 4, characterized in that: The industrial control system (700) adopts a centralized control system.

6. The high-throughput automated polymer material development system according to claim 5, characterized in that: The first automatic weighing and feeding device (100) and the second automatic weighing and feeding device (400) adopt gravity-type continuous automatic charging scales.

7. The high-throughput automated polymer material development system according to claim 6, characterized in that: The polymer resin preparation device (200) adopts a reaction kettle.

8. The high-throughput automated polymer material development system according to claim 5, characterized in that: The polymer material compounding device (300) adopts a twin-screw or multi-screw extruder.

9. A control method for a high-throughput automated polymer material development system as claimed in any one of claims 1 to 8, using an industrial control system for control; Features: The industrial control system (700) comprises an industrial computer; and further comprises the following steps: S1. Establish control relationship; Establishing a corresponding relationship between various properties of polymer materials and various processing parameters in an industrial computer; the processing parameters include the addition amount of each component raw material, the addition amount of the catalyst, the addition amount of the additive, the reaction parameters of the polymer resin preparation device (200) and the reaction parameters of the polymer material composite device (300); S2. Setting processing parameters to produce polymer materials; Setting target performance parameters of the polymer material, 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) and the process parameters of the polymer resin preparation device (200) and the polymer material compounding device (300) based on the received target performance parameters of the polymer material to produce the polymer material; S3. Testing and analysis of polymer material performance; Using a polymer material testing device (500) to test the performance parameters of the polymer material obtained by the polymer material composite device (300); transmitting the detected performance parameters to an industrial control system (700); and the industrial control system (700) comparing the detected performance parameters with target performance parameters to obtain feedback results; S4, automatic adjustment of processing parameters; The industrial control system (700) adjusts the automatic quantitative of the first automatic weighing and feeding device (100) and the second automatic weighing and feeding device (400) and the process parameters of the polymer resin preparation device (200) and the polymer material composite device (300) according to the feedback result 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 a polymer resin preparation device (200) and a polymer material composite device (300), and the performance parameters of the new polymer material are tested by a 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 polymer performance parameters actually detected are the same as the target performance parameters; the data is then saved through an industrial computer; stored in a database, and the processing parameters corresponding to the original target performance parameters are replaced.

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