Concentration equipment and concentration method for preparing silk fibroin aqueous solution
The silk protein concentration device addresses efficiency and stability issues by integrating water bath heating and dynamic regulation, achieving uniform heating and rapid bubble removal for stable silk protein concentration.
Patent Information
- Application Number
- CN202510707490.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-05-29
- Publication Date
- 2025-07-15
AI Technical Summary
The existing silk fibroprotein aqueous solution concentration equipment has poor balance of efficiency and stability during heating, which can easily lead to silk fibroprotein denaturation, and the existing stirring method can easily generate bubbles and lead to protein denaturation.
The heating method of combining drainage components and hydrothermal components is adopted, and the stirring mechanism and the flow guide components are combined for gradient heating and defoaming treatment. The heating speed, vacuum degree, stirring speed and stabilizer release speed are dynamically controlled by the control system to ensure the stability and uniformity of the silk fibroprotein aqueous solution.
It realizes efficient and stable concentration of silk fibroprotein aqueous solution, avoids thermal denaturation and bubble generation, and is suitable for automated production scenarios.
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Figure CN120305699A_ABST
Abstract
Description
Technical Field
[0001] The present invention belongs to the technical field of silk fibroin aqueous solution concentration, and particularly relates to a concentration device and a concentration method for preparing silk fibroin aqueous solution. Background Art
[0002] In the process of preparing an aqueous solution of silk fibroin, it is necessary to dissolve it, and then purify and concentrate it to obtain an aqueous solution with a certain concentration for subsequent use. The existing concentration of the aqueous solution generally involves heating the aqueous solution to reduce the water content in the aqueous solution by evaporating water, so as to achieve the purpose of increasing the concentration. However, the method of evaporating water by heating has high energy consumption, and silk fibroin is sensitive to heat. High temperature (>40°C) will destroy its β-sheet structure, resulting in irreversible denaturation or gelation.
[0003] When the existing concentration device for preparing silk fibroin aqueous solution concentrates the silk fibroin aqueous solution, due to the use of a single fixed heating method, the silk fibroin is prone to heat denaturation during the heating process. And if the method of stirring and mixing is used to improve the uniformity of heat absorption of the silk fibroin, bubbles are easily generated during the stirring and mixing, and the bubbles easily cause the silk fibroin at the gas-liquid interface to denature. Therefore, the core contradiction in the concentration of silk fibroin aqueous solution is the balance between efficiency and stability. Summary of the Invention
[0004] The purpose of the embodiments of the present invention is to provide a concentration device and a concentration method for preparing silk fibroin aqueous solution, aiming to solve the problem of poor balance between efficiency and stability during the concentration of silk fibroin aqueous solution.
[0005] The present invention is implemented as follows. A concentration device for preparing silk fibroin aqueous solution includes a workbench. The workbench is fixedly connected with a concentration barrel. A drainage component is arranged outside the concentration barrel. The drainage component can drive the silk fibroin aqueous solution in the concentration barrel to circulate. A hydrothermal component is arranged outside the drainage component. The hydrothermal component can perform water bath heating on the silk fibroin aqueous solution in the drainage component;
[0006] An electric rod is fixedly connected to the bottom of the concentration barrel. The telescopic part of the electric rod is connected with a stirring mechanism and a flow splitting component. The flow splitting component is below the stirring mechanism. The stirring mechanism can mix and stir the silk fibroin aqueous solution and heat it. The stirring mechanism can also add a stabilizer to the silk fibroin aqueous solution. The flow splitting component can filter the bubbles in it. The stirring mechanism is also connected with a diversion component. The diversion component can drive the vertical mixing of the silk fibroin aqueous solution, and the diversion component can also drive the defoaming agent particles to dissolve faster;
[0007] The upper part of the concentration barrel is sealed with a cover plate, which is connected to a feed box and a vacuum pump. A second solenoid valve is provided at the discharge pipe of the feed box in the concentration barrel. A condensation and drying system is usually included between the vacuum pump and the concentration barrel, which includes an evaporation flask, a low-temperature cold trap, a condensation receiving flask, and a drying tower, for collecting water vapor in a low-pressure environment, and ensuring the safety and repeatability of the silk fibroin concentration process;
[0008] A control system, which can generate a control model based on the heating rate of the silk fibroin aqueous solution, the vacuum degree elevation rate in the concentration barrel, the stirring rate of the stirring mechanism, and the stabilizer feeding rate, and improve the stability during the concentration process of the silk fibroin aqueous solution through the control model;
[0009] A visual detector is provided on the inner end face of the cover plate. When the bubble density in the concentration barrel increases, the control system can also control the drainage component, the stirring mechanism, the diversion component, and the shunt component to carry out defoaming treatment.
[0010] In a further technical solution, the drainage component includes a spiral water pipe and a first water pump. The spiral water pipe is spirally arranged around the outer wall of the concentration barrel. The lower end of the spiral water pipe is connected to the concentration barrel through the first water pump, and the upper end of the spiral water pipe is directly connected to the concentration barrel. A semi-permeable membrane for filtering bubbles is provided at the upper end of the spiral water pipe, and electromagnetic cut-off valves are provided at both ends of the spiral water pipe.
[0011] In a further technical solution, the hydrothermal component includes a hydrothermal sleeve and a water tank. The hydrothermal sleeve and the water tank are both fixedly connected to the workbench. The hydrothermal sleeve fits the spiral water pipe. Both ends of the hydrothermal sleeve are connected to the water tank, and a second water pump is provided at one end of the hydrothermal sleeve. An electric heater and a first temperature sensor are provided in the water tank.
[0012] In a further technical solution, the stirring mechanism includes a sleeve, an electric heating pipe, a stirring rod, and a driving component;
[0013] The sleeve is rotationally connected to the telescopic part of the electric rod. The telescopic part of the electric rod is fixedly connected with a mechanism box. A driving component capable of driving the sleeve to rotate is provided in the mechanism box. The sleeve is connected with a plurality of electric heating pipes, and the electric heating pipes are connected with a plurality of stirring rods. An electric heater is provided in the electric heating pipe. The driving component is composed of a motor and a gear transmission pair, and the motor drives the sleeve to rotate through the gear transmission pair.
[0014] In a further technical solution, the diversion component includes a support frame, a diversion plate, and a filter plate;
[0015] The support frame is fixedly connected to the sleeve. The two ends of the support frame are respectively rotatably connected with a flow guide plate and a filter plate, and the flow guide plate and the filter plate are inclined and abutted against both sides of the support frame. Electromagnets are arranged on both sides of the support frame, and a button battery for supplying power to the electromagnets is arranged in the support frame. The button battery is electrically connected to the control system.
[0016] A further technical solution is that the flow splitting assembly includes a baffle plate, a flow guide groove and a filter net;
[0017] The baffle plate is fixedly connected to the telescopic part of the electric rod. A plurality of flow guide grooves are obliquely arranged on the baffle plate, and a filter net is arranged perpendicular to the end face of the baffle plate in the flow guide groove.
[0018] A further technical solution is that a cavity is formed between the middle section of the telescopic part of the electric rod and the sleeve. Antifoaming agent particles are stored in the cavity. One-way solenoid valves are arranged at one ends of the electric heating tubes connected to the cavity, and a plurality of blanking holes are arranged on the electric heating tubes.
[0019] A further technical solution is that the control system includes:
[0020] A monitoring module, which includes a second temperature sensor arranged in the concentration tank, a pressure vacuum gauge arranged in the concentration tank, and an encoder electrically connected to the stirring mechanism;
[0021] A processing module, which is used to record the temperature rising speed of the temperature sensor, the vacuum degree rising speed displayed by the pressure vacuum gauge, the stirring speed value of the stirring mechanism measured by the encoder, and the feeding speed of the stabilizer in the feed box calculated by the opening size of the one-way solenoid valve, and generate a control coefficient according to the calculated temperature rising speed, vacuum degree rising speed, stirring speed and stabilizer feeding speed. When the control coefficient exceeds the preset threshold range, a judgment information is generated at this time;
[0022] A control module, which is used to control the hydrothermal component, the stirring mechanism, the one-way solenoid valve and the vacuum pump.
[0023] A further technical solution is that the generation method of the control coefficient is:
[0024] The measured temperature rising speed, vacuum degree rising speed, stirring speed and stabilizer feeding speed are subjected to maximum-minimum normalization processing and then weighted processing, and finally a control coefficient is generated:
[0025] SCI = w1V T +w2V w +w3V P +w4V s
[0026] Among them, w1, w2, w3, and w4 are the weights of the temperature rise rate, vacuum degree increase rate, stirring speed, and stabilizer feeding speed on the stability during the concentration process of the silk fibroin aqueous solution (in the actual production process, the change in the secondary structure of silk fibroin (β-sheet content) can be monitored by FTIR, and the weights of w1, w2, w3, and w4 can be dynamically optimized), and w1 + w2 + w3 + w4 = 1; V T is the temperature rise rate of the silk fibroin aqueous solution in the concentration tank after normalization processing, V w is the vacuum degree increase rate in the concentration tank, V P is the stirring speed of the stirring mechanism, V s is the stabilizer feeding speed; SCI is the regulation coefficient.
[0027] Compared with the prior art, the beneficial effects of the present invention are:
[0028] 1. The regulation system can generate a regulation model based on the heating rate of the silk fibroin aqueous solution, the vacuum degree increase rate in the concentration tank, the stirring speed of the stirring mechanism, and the stabilizer feeding speed. The regulation system can maintain the stability of silk fibroin under complex working conditions through dynamic normalization regulation and multi-parameter collaborative response, and is suitable for automated production scenarios.
[0029] 2. When the visual detector detects an increase in the bubble density in the concentration tank, the regulation system can also control the drainage component, the stirring mechanism, the diversion component, and the shunt component to perform defoaming treatment, which not only improves the defoaming rate but also avoids thermal denaturation of the silk fibroin aqueous solution.
[0030] 3. The stirring mechanism in the concentration tank heats the silk fibroin aqueous solution at a low temperature, while in the drainage component, the silk fibroin aqueous solution is heated by a hydrothermal component to achieve a water bath temperature rise. The combination of the two heating methods realizes a gradient temperature rise; on the one hand, the method of heating the flowing silk fibroin aqueous solution by a water bath can improve the heating rate of the silk fibroin aqueous solution and also improve the heating uniformity. Further, when it is detected that the temperature of the silk fibroin aqueous solution rises too fast in the concentration tank, the flow of the silk fibroin aqueous solution in the drainage component can be cut off at this time, and the silk fibroin aqueous solution can be concentrated in the concentration tank to quickly reduce the heating rate of the silk fibroin aqueous solution, thereby further avoiding the deformation of the silk fibroin aqueous solution due to too fast temperature rise; on the other hand, it is convenient to centrally observe the bubbles in the silk fibroin aqueous solution in the concentration tank, which is convenient for subsequent rapid defoaming treatment of the bubbles in the silk fibroin aqueous solution.
[0031] 4. After adding defoaming agent particles into the concentration barrel, the filter plate can collect the defoaming agent particles at this time. Under the push of the filter plate, the defoaming agent particles move and dissolve rapidly relative to the aqueous solution of fibroin, thereby eliminating the bubbles in the aqueous solution of fibroin above the baffle. During this process, under the guiding action of the filter plate, the bubbles gather and merge upward, increasing the bubble elimination rate. Further, since the filter plate is reticular, the control system controls the deflector plate to rotate and tend to be horizontal, so that the aqueous solution of fibroin is less disturbed, preventing the aqueous solution of fibroin on both sides of the baffle from mixing with each other and reducing the bubble elimination rate. At the same time, the filter mesh on the baffle is arranged vertically, which can also reduce the flow exchange rate of the aqueous solution of fibroin on both sides of the baffle during defoaming. BRIEF DESCRIPTION OF THE DRAWINGS
[0032] Figure 1 is a schematic structural diagram of the present invention;
[0033] Figure 2 is a schematic internal structure diagram of the concentration barrel of the present invention;
[0034] Figure 3 is a schematic structural diagram of the flow splitting component in the present invention;
[0035] Figure 4 is a schematic structural diagram of the stirring mechanism in the present invention;
[0036] Figure 5 is a schematic structural diagram of the deflector component in the present invention;
[0037] Figure 6 is a schematic flow chart of the method for concentrating the aqueous solution of fibroin in the present invention.
[0038] In the drawings: 1, workbench; 2, concentration barrel; 3, drainage component; 31, spiral water pipe; 32, first water pump; 4, hydrothermal component; 41, hydrothermal sleeve; 42, water tank; 5, stirring mechanism; 51, sleeve; 52, electric heating tube; 53, stirring rod; 54, driving component; 6, deflector component; 61, support frame; 62, deflector plate; 63, filter plate; 7, flow splitting component; 71, baffle; 72, diversion groove; 73, filter mesh; 8, cavity; 9, first solenoid valve; 10, material box; 11, vacuum pump; 12, mechanism box; 13, cover plate; 14, electric rod. DETAILED DESCRIPTION OF THE EMBODIMENTS
[0039] In order to make the objectives, technical solutions and advantages of the present invention clearer, the present invention will be further described in detail below with reference to the drawings and embodiments. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not used to limit the present invention.
[0040] The following describes the specific implementation of the present invention in detail with reference to specific embodiments.
[0041] As Figures 1 - 6 shown, a concentration device for preparing a silk fibroin aqueous solution provided by an embodiment of the present invention includes a workbench 1, the workbench 1 is fixedly connected with a concentration barrel 2, a drainage assembly 3 is arranged outside the concentration barrel 2, the drainage assembly 3 can drive the silk fibroin aqueous solution in the concentration barrel 2 to circulate, and a hydrothermal assembly 4 is arranged outside the drainage assembly 3, and the hydrothermal assembly 4 can perform water bath heating on the silk fibroin aqueous solution in the drainage assembly 3;
[0042] A motorized rod 14 is fixedly connected to the bottom of the concentration barrel 2, and the telescopic part of the motorized rod 14 is connected with a stirring mechanism 5 and a flow splitting assembly 7. The flow splitting assembly 7 is below the stirring mechanism 5. The stirring mechanism 5 can mix and stir the silk fibroin aqueous solution and heat it. The stirring mechanism 5 can also add a stabilizer to the silk fibroin aqueous solution. The flow splitting assembly 7 can filter the bubbles in it. The stirring mechanism 5 is also connected with a diversion assembly 6. The diversion assembly 6 can drive the vertical mixing of the silk fibroin aqueous solution, and the diversion assembly 6 can also drive the defoaming agent particles to dissolve faster;
[0043] The upper part of the concentration barrel 2 is sealed with a cover plate 13. The cover plate 13 is connected with a material box 10 and a vacuum pump 11. The material box 10 is provided with a second solenoid valve at the discharge pipe in the concentration barrel 2. A condensation and drying system (usually including an evaporation flask, a low-temperature cold trap, a condensation receiving flask, and a drying tower) is arranged between the vacuum pump 11 and the concentration barrel 2 for collecting water vapor in a low-pressure environment, and at the same time ensuring the safety and repeatability of the silk fibroin concentration process;
[0044] A regulation system, which can generate a regulation model based on the heating rate of the silk fibroin aqueous solution, the vacuum degree increase rate in the concentration barrel 2, the stirring rate of the stirring mechanism 5, and the stabilizer feeding rate, and improve the stability during the concentration process of the silk fibroin aqueous solution through the regulation model;
[0045] A visual detector is arranged on the inner end face of the cover plate 13. When the bubble density in the concentration barrel 2 increases, the regulation system can also control the drainage assembly 3, the stirring mechanism 5, the diversion assembly 6, and the flow splitting assembly 7 to perform defoaming treatment.
[0046] A method for concentrating a silk fibroin aqueous solution includes the following steps:
[0047] S1: Pour the silk fibroin aqueous solution into the concentration barrel 2, and then close the concentration barrel 2; First, start the vacuum pump 11 to gradually reduce the air pressure in the concentration barrel 2, so that the vacuum degree in the concentration barrel 2 rises, thereby reducing the boiling point temperature of water;
[0048] S2: First, start the stirring mechanism 5 to mix and stir the aqueous solution of silk fibroin in the concentration barrel 2 and heat it. Then, start the drainage component 3, and the drainage component 3 drives the aqueous solution of silk fibroin to circulate. At this time, the hydrothermal component 4 can perform water bath heating on the aqueous solution of silk fibroin in the drainage component 3, and during this process, keep the water bath temperature of the hydrothermal component 4 higher than the heating temperature of the stirring mechanism 5 in the concentration barrel 2;
[0049] S3: In the concentration barrel 2, the stirring mechanism 5 can also add a stabilizer to the aqueous solution of silk fibroin, and the diversion component 6 can drive the vertical mixing of the aqueous solution of silk fibroin, improving the uniformity of heat absorption of the aqueous solution of silk fibroin in the concentration barrel 2;
[0050] S4: During this process, the control system generates a control model based on the heating rate of the aqueous solution of silk fibroin, the vacuum degree increase rate in the concentration barrel 2, the stirring rate of the stirring mechanism 5, and the stabilizer feeding rate, and improves the stability during the concentration process of the aqueous solution of silk fibroin through the control model;
[0051] S5: When the visual detector detects an increase in the bubble density in the concentration barrel 2, at this time, the control system can also control the drainage component 3, the stirring mechanism 5, the diversion component 6, and the shunt component 7 to perform defoaming treatment.
[0052] During this process, in the concentration barrel 2, the stirring mechanism 5 heats the aqueous solution of silk fibroin at a low temperature, while in the drainage component 3, the hydrothermal component 4 performs water bath heating to increase the temperature of the aqueous solution of silk fibroin. The cooperation of the two heating methods realizes gradient heating; on the one hand, the method of heating the flowing aqueous solution of silk fibroin through the water bath can not only improve the heating rate of the aqueous solution of silk fibroin, but also, since the aqueous solution of silk fibroin is constantly flowing in the drainage component 3, it can also improve the heating uniformity. Further, due to gradient heating, when it is detected that the temperature of the aqueous solution of silk fibroin rises too fast in the concentration barrel 2, at this time, the flow of the aqueous solution of silk fibroin in the drainage component 3 can be cut off, and the aqueous solution of silk fibroin can be concentrated in the concentration barrel 2 to quickly reduce the heating rate of the aqueous solution of silk fibroin, thereby further avoiding the deformation of the aqueous solution of silk fibroin due to too fast temperature rise;
[0053] On the other hand, in the concentration barrel 2, it is convenient to centrally observe the bubbles in the aqueous solution of silk fibroin (foam easily causes protein denaturation at the gas-liquid interface and destroys the protein structure), facilitating subsequent rapid defoaming treatment of the bubbles in the aqueous solution of silk fibroin.
[0054] Such as Figure 1As shown, as a preferred embodiment of the present invention, the drainage assembly 3 includes a spiral water pipe 31 and a first water pump 32. The spiral water pipe 31 is spirally arranged around the outer wall of the concentration barrel 2. The lower end of the spiral water pipe 31 is connected to the concentration barrel 2 through the first water pump 32, and the upper end of the spiral water pipe 31 is directly connected to the concentration barrel 2. A semi-permeable membrane for filtering air bubbles is provided at the upper end of the spiral water pipe 31, and electromagnetic cut-off valves are provided at both ends of the spiral water pipe 31.
[0055] In this embodiment, the first water pump 32 is started, and the first water pump 32 drives the fibroin aqueous solution to circulate between the concentration barrel 2 and the spiral water pipe 31. During this process, the hydrothermal assembly 4 is started, and the hydrothermal assembly 4 performs water bath heating on the fibroin aqueous solution flowing through the spiral water pipe 31.
[0056] As Figure 1 shown, as a preferred embodiment of the present invention, the hydrothermal assembly 4 includes a hydrothermal sleeve 41 and a water tank 42. The hydrothermal sleeve 41 and the water tank 42 are both fixedly connected to the workbench 1. The hydrothermal sleeve 41 is attached to the spiral water pipe 31. Both ends of the hydrothermal sleeve 41 are connected to the water tank 42, and a second water pump is provided at one end of the hydrothermal sleeve 41. An electric heater and a first temperature sensor are provided in the water tank 42.
[0057] In this embodiment, the heater in the water tank 42 is started for heating, and then the second water pump is started to make the water flow circulate between the hydrothermal sleeve 41 and the water tank 42. When the fibroin aqueous solution in the concentration barrel 2 flows through the spiral water pipe 31, at this time, the fibroin aqueous solution in the spiral water pipe 31 exchanges heat with the water flow in the concentration barrel 2. By means of water bath heating, while increasing the heating rate of the fibroin aqueous solution, the uniformity and stability of the heating temperature during the heating process can be ensured.
[0058] As Figure 4 shown, as a preferred embodiment of the present invention, the stirring mechanism 5 includes a sleeve 51, an electric heating tube 52, a stirring rod 53, and a driving assembly 54;
[0059] The sleeve 51 is rotationally connected to the telescopic part of the electric rod 14. A mechanism box 12 is fixedly connected to the telescopic part of the electric rod 14. A driving assembly 54 capable of driving the sleeve 51 to rotate is provided in the mechanism box 12. The sleeve 51 is connected with a plurality of electric heating tubes 52, and the electric heating tubes 52 are connected with a plurality of stirring rods 53. An electric heater is provided in the electric heating tube 52. The driving assembly 54 is composed of a motor and a gear transmission pair, and the motor drives the sleeve 51 to rotate through the gear transmission pair.
[0060] In this embodiment, the driving component 54 drives the sleeve 51 to rotate. The sleeve 51 drives the electric heating tube 52 and the stirring rod 53 to stir and heat the aqueous solution of fibroin in the concentration barrel 2. During this process, the electric heater in the electric heating tube 52 is started to heat the electric heating tube 52 and the stirring rod 53, so that the electric heating tube 52 and the electric heating tube 52 carry out low-temperature heating and stirring on the aqueous solution of fibroin.
[0061] As Figure 6 shown, as a preferred embodiment of the present invention, the diversion component 6 includes a support frame 61, a diversion plate 62 and a filter plate 63;
[0062] The support frame 61 is fixedly connected to the sleeve 51. The two ends of the support frame 61 are respectively rotatably connected with a diversion plate 62 and a filter plate 63. The diversion plate 62 and the filter plate 63 are inclined and abutted against both sides of the support frame 61. Electromagnets are arranged on both sides of the support frame 61. A button battery for supplying power to the electromagnets is arranged in the support frame 61. The button battery is electrically connected to the control system.
[0063] In this embodiment, when the aqueous solution of fibroin is heated and raised in temperature in the concentration barrel 2, at this time, the control system controls the electromagnets on both sides of the support frame 61 to adsorb the diversion plate 62 and the filter plate 63, so that the diversion plate 62 and the filter plate 63 on both sides of the support frame 61 are kept stably inclined. The sleeve 51 drives the support frame 61 to rotate. At this time, all the diversion plates 62 are in the water-facing surface. The aqueous solution of fibroin is diverted through the diversion plate 62, so that the aqueous solution of fibroin in the concentration barrel 2 is vertically mixed, thereby improving the uniformity of the temperature rise of the aqueous solution of fibroin in the concentration barrel 2. And the diversion plate 62 can protect the filter plate 63 on the back, avoiding the blockage of the mesh holes of the filter plate 63 by fibroin fibers or impurities during the mixing process.
[0064] As Figure 3 shown, as a preferred embodiment of the present invention, the shunt component 7 includes a baffle 71, a diversion groove 72 and a filter net 73;
[0065] The baffle 71 is fixedly connected to the telescopic part of the electric rod 14. A plurality of diversion grooves 72 are obliquely arranged on the baffle 71. A filter net 73 is arranged perpendicular to the end face of the baffle 71 in the diversion groove 72.
[0066] In this embodiment, when the visual detector detects that there are too many bubbles in the concentration barrel 2, at this time, the control system controls the first water pump 32 to reversely pump out the aqueous solution of fibroin in the spiral water pipe 31 (the upper end opening of the spiral water pipe 31 is slightly higher than the liquid level of the aqueous solution of fibroin), and then starts the electromagnetic cut-off valve at the end of the spiral water pipe 31 to close the spiral water pipe 31, and starts the hydrothermal component 4 to stop heating the spiral water pipe 31 by water bath;
[0067] In the concentration barrel 2, the control system controls the telescopic part of the electric rod 14 to drive the baffle 71 to rise. The baffle 71 filters and collects the bubbles in the aqueous solution of fibroin from bottom to top until most of the bubbles are collected by the baffle 71 near the liquid level of the aqueous solution of fibroin. At this time, the electric heating tube 52 and the stirring rod 53 on the sleeve 51 are separated from the aqueous solution of fibroin to prevent the aqueous solution of fibroin from being continuously heated and denatured during the defoaming process.
[0068] Start the drive assembly 54 to drive the support frame 61 to reverse. After adding defoaming agent particles to the concentration barrel 2, the filter plate 63 can collect the defoaming agent particles at this time. Under the push of the filter plate 63, the defoaming agent particles move and dissolve rapidly relative to the aqueous solution of fibroin, thereby eliminating the bubbles in the aqueous solution of fibroin above the baffle 71. During this process, the filter plate 63 can collect the bubbles. Since the filter plate 63 is inclined, under the guiding action of the filter plate 63, the bubbles gather and merge upward, improving the bubble elimination rate.
[0069] Furthermore, since the filter plate 63 is reticular, the control system controls the electromagnet on one side of the guide plate 62 to change the electrode direction. Under the magnetic force, the guide plate 62 rotates and tends to be horizontal. Therefore, when the filter plate 63 dissolves the defoaming agent particles in the aqueous solution of fibroin, the aqueous solution of fibroin can be less disturbed at this time, preventing the aqueous solution of fibroin on both sides of the baffle 71 from mixing with each other and rapidly reducing the concentration of the defoaming agent on the upper side of the baffle 71, thereby reducing the bubble elimination rate. At the same time, the filter net 73 on the baffle 71 is vertically arranged, which can also reduce the flow exchange rate of the aqueous solution of fibroin on both sides of the baffle 71 during defoaming.
[0070] As Figure 4 shown, as a preferred embodiment of the present invention, a cavity 8 is formed between the middle section of the telescopic part of the electric rod 14 and the sleeve 51. Defoaming agent particles are stored in the cavity 8. One-way solenoid valves 9 are provided at one end of the electric heating tube 52 connected to the cavity 8, and a number of material dropping holes are provided on the electric heating tube 52.
[0071] In this embodiment, when the electric heating tube 52 on the sleeve 51 and the electric heating tube 52 heat the aqueous solution of fibroin at a low temperature, the stirring rod 53 can dry the defoaming agent particles in the cavity 8 at a low temperature, thereby preventing the defoaming agent particles from being affected by moisture and reducing their defoaming effect.
[0072] As a preferred embodiment of the present invention, the control system includes:
[0073] A monitoring module, which includes a second temperature sensor. The second temperature sensor is arranged in the concentration barrel 2. It also includes a pressure vacuum gauge arranged in the concentration barrel 2 and an encoder electrically connected to the stirring mechanism 5.
[0074] A processing module, which is used to record the temperature rising speed of the temperature sensor, the vacuum degree rising speed shown by the pressure vacuum gauge, the stirring speed value of the stirring mechanism 5 measured by the encoder, and the feeding speed of the stabilizer in the material tank 10 calculated by the opening size of the first solenoid valve 9, and generate a regulation coefficient according to the measured temperature rising speed, vacuum degree rising speed, stirring speed and stabilizer feeding speed. When the regulation coefficient exceeds the preset threshold range, judgment information is generated at this time;
[0075] A control module, which is used to control the hydrothermal component 4, the stirring mechanism 5, the first solenoid valve 9 and the vacuum pump 11.
[0076] The generation method of the regulation coefficient is as follows:
[0077] The measured temperature rising speed, vacuum degree rising speed, stirring speed and stabilizer feeding speed are processed by maximum-minimum normalization and then weighted to finally generate a regulation coefficient:
[0078] SCI = w1V T + w2V w + w3V P + w4V s
[0079] Among them, w1, w2, w3, and w4 are the weights of the temperature rising speed, vacuum degree rising speed, stirring speed, and stabilizer feeding speed on the stability during the concentration process of the silk fibroin aqueous solution. (In the actual production process, the change of the secondary structure of silk fibroin (β-sheet content) can be monitored by FTIR to dynamically optimize the weights of w1, w2, w3, and w4), w1 + w2 + w3 + w4 = 1; V T is the temperature rising speed of the silk fibroin aqueous solution in the concentration tank 2 after normalization processing, V w is the vacuum degree rising speed in the concentration tank 2, V P the stirring speed of the stirring mechanism 5, V s is the stabilizer feeding speed; SCI is the regulation coefficient.
[0080] In this embodiment, the regulation system can maintain the stability of silk fibroin under complex working conditions through dynamic normalization regulation and multi-parameter collaborative response, and is applicable to automated production scenarios. Data is collected at regular intervals on the temperature rise rate of the temperature sensor, the vacuum degree displayed by the pressure vacuum gauge, the stirring speed value of the stirring mechanism 5, and the feeding speed of the stabilizer. When the regulation coefficient calculated by the processing module exceeds the preset threshold in the processing module, the control module then controls the heating speed, mixing speed, the vacuum degree rise rate in the concentration barrel 2, and the feeding speed of the stabilizer of the silk fibroin aqueous solution by means of the hydrothermal component 4, the stirring mechanism 5, the first solenoid valve 9, and the vacuum pump 11 (reducing the heating speed of the silk fibroin aqueous solution can prevent the silk fibroin from overheating and denaturing; increasing the mixing speed of the stirring mechanism 5 and the pumping speed of the drainage component 3 can enhance the heat transfer uniformity of the silk fibroin aqueous solution; reducing the vacuum degree rise rate in the concentration barrel 2 can slow down the evaporation rate of the silk fibroin aqueous solution; increasing the feeding speed of the stabilizer can improve the thermal stability of the silk fibroin aqueous solution), thereby enhancing the stability during the concentration process of the silk fibroin aqueous solution.
[0081] The foregoing are only preferred embodiments of the present invention and are not intended to limit the present invention. Any modifications, equivalent substitutions, and improvements made within the spirit and principle of the present invention shall be included within the protection scope of the present invention.
Claims
1. A concentration device for preparing a silk fibroin aqueous solution, comprising a workbench (1), wherein the workbench (1) is fixedly connected with a concentration barrel (2), and is characterized in that, An external drainage component (3) is provided outside the concentration barrel (2). The drainage component (3) can drive the fibroin aqueous solution in the concentration barrel (2) to circulate. An external hydrothermal component (4) is provided outside the drainage component (3). The hydrothermal component (4) can perform water bath heating on the fibroin aqueous solution in the drainage component (3). The bottom of the concentration barrel (2) is fixedly connected with an electric rod (14). The telescopic part of the electric rod (14) is connected with a stirring mechanism (5) and a shunt component (7). The stirring mechanism (5) can mix, stir and heat the fibroin aqueous solution. The stirring mechanism (5) can also add a stabilizer to the fibroin aqueous solution. The shunt component (7) can filter the bubbles in it. The stirring mechanism (5) is also connected with a diversion component (6). The diversion component (6) can drive the vertical mixing of the fibroin aqueous solution, and the diversion component (6) can also drive the defoaming agent particles to dissolve faster. The upper part of the concentration barrel (2) is sealed with a cover plate (13). The cover plate (13) is connected with a material box (10) and a vacuum pump (11). The material box (10) is provided with a second solenoid valve at the discharge pipe in the concentration barrel (2). The inner end face of the cover plate (13) is provided with a vision detector for detecting the bubble density. A control system, which can generate a control model based on the heating rate of the fibroin aqueous solution, the vacuum degree increasing rate in the concentration barrel (2), the stirring rate of the stirring mechanism (5) and the stabilizer feeding rate, and improve the stability during the concentration process of the fibroin aqueous solution through the control model.
2. The concentration device for preparing aqueous fibroin solution according to claim 1, characterized in that, The drainage component (3) includes a spiral water pipe (31) and a first water pump (32). The spiral water pipe (31) is spirally arranged around the outer wall of the concentration barrel (2). The lower end of the spiral water pipe (31) is connected to the concentration barrel (2) through the first water pump (32). The upper end of the spiral water pipe (31) is directly connected to the concentration barrel (2). A semi-permeable membrane for filtering bubbles is provided at the upper end of the spiral water pipe (31), and electromagnetic cut-off valves are provided at both ends of the spiral water pipe (31).
3. The concentration device for preparing the aqueous solution of silk fibroin according to claim 2, wherein, The hydrothermal component (4) includes a hydrothermal sleeve (41) and a water tank (42). The hydrothermal sleeve (41) and the water tank (42) are both fixedly connected to the workbench (1). The hydrothermal sleeve (41) fits the spiral water pipe (31). Both ends of the hydrothermal sleeve (41) are connected to the water tank (42), and a second water pump is provided at one end of the hydrothermal sleeve (41). An electric heater and a first temperature sensor are provided in the water tank (42).
4. The concentration device for preparing the aqueous solution of silk fibroin according to claim 1, characterized in that, The stirring mechanism (5) includes a sleeve (51), an electric heating tube (52), a stirring rod (53) and a driving component (54). The sleeve (51) is rotationally connected to the telescopic part of the electric rod (14). A mechanism box (12) is fixedly connected to the telescopic part of the electric rod (14). A driving component (54) capable of driving the sleeve (51) to rotate is arranged in the mechanism box (12). The sleeve (51) is connected with a plurality of electric heating tubes (52). The electric heating tubes (52) are connected with a plurality of stirring rods (53). An electric heater is arranged in the electric heating tubes (52). The driving component (54) is composed of a motor and a gear transmission pair, and the motor drives the sleeve (51) to rotate through the gear transmission pair.
5. The concentration device for preparing the aqueous solution of silk fibroin according to claim 4, characterized in that, The diversion component (6) includes a support frame (61), a diversion plate (62) and a filter plate (63); The support frame (61) is fixedly connected with the sleeve (51). The two ends of the support frame (61) are respectively rotationally connected with a diversion plate (62) and a filter plate (63). The diversion plate (62) and the filter plate (63) are inclined and abutted against both sides of the support frame (61). Electromagnets are arranged on both sides of the support frame (61). A button battery for supplying power to the electromagnets is arranged in the support frame (61). The button battery is electrically connected with the control system.
6. The concentration device for preparing the aqueous solution of silk fibroin according to claim 1, characterized in that, The flow splitting component (7) includes a baffle (71), a diversion groove (72) and a filter net (73); The baffle (71) is fixedly connected with the telescopic part of the electric rod (14). A plurality of diversion grooves (72) are obliquely arranged on the baffle (71). A filter net (73) is arranged perpendicular to the end face of the baffle (71) in the diversion groove (72).
7. The concentration device for preparing aqueous fibroin solution according to claim 4, characterized in that, A cavity (8) is formed between the middle section of the telescopic part of the electric rod (14) and the sleeve (51). Antifoaming agent particles are stored in the cavity (8). One-way solenoid valves (9) are arranged at one ends of the electric heating tubes (52) communicated with the cavity (8). A plurality of material dropping holes are arranged on the electric heating tubes (52).
8. The concentration device for preparing the aqueous fibroin solution according to claim 1, characterized in that, The control system includes: A monitoring module, which includes a second temperature sensor arranged in the concentration barrel (2), a pressure vacuum gauge arranged in the concentration barrel (2), and an encoder electrically connected with the stirring mechanism (5); A processing module, which is used for recording the temperature rising speed of the temperature sensor, the vacuum degree rising speed shown by the pressure vacuum gauge, the stirring speed value of the stirring mechanism (5) measured by the encoder, and the feeding speed of the stabilizer in the material box (10) calculated by the opening size of the one-way solenoid valve (9), and generating a control coefficient according to the calculated temperature rising speed, vacuum degree rising speed, stirring speed and stabilizer feeding speed. When the control coefficient exceeds the preset threshold range, judgment information is generated at this time; A control module, which is used for controlling the hydrothermal component (4), the stirring mechanism (5), the one-way solenoid valve (9) and the vacuum pump (11).
9. A method for concentrating an aqueous solution of silk fibroin, which is applied to the concentration equipment for preparing an aqueous solution of silk fibroin described in claims 1-8, and is characterized in that, Including the following steps: S1: Pour the silk fibroin aqueous solution into the concentration barrel (2), and then seal the concentration barrel (2); First, start the vacuum pump (11) to gradually reduce the air pressure in the concentration barrel (2), so that the vacuum degree in the concentration barrel (2) rises, thereby reducing the boiling point temperature of water; S2: In the concentration barrel (2), the stirring mechanism (5) heats the aqueous solution of silk fibroin at a low temperature, while in the drainage assembly (3), the aqueous solution of silk fibroin is heated by the hydrothermal assembly (4) to increase the temperature of the water bath. The combination of the two heating methods achieves a gradient temperature increase; S3: During the stirring process of the stirring mechanism (5), a stabilizer is added to the aqueous solution of silk fibroin; S4: The control system generates a control model based on the heating rate of the aqueous solution of silk fibroin, the vacuum degree increase rate in the concentration barrel (2), the stirring rate of the stirring mechanism (5), and the stabilizer feeding rate, and improves the stability during the concentration process of the aqueous solution of silk fibroin through the control model; S5: When the visual detector detects an increase in the bubble density in the concentration barrel (2), the control system can also control the drainage assembly (3), the stirring mechanism (5), the diversion assembly (6), and the shunt assembly (7) to perform defoaming treatment.