A silk fibroin solution purification device and a purification method thereof

Abstract

The application discloses a silk fibroin solution purification device and a purification method thereof, which comprises a dialysate storage tank, a dialysis water tank, a finished product storage tank and a PLC control cabinet; a liquid pumping pump, a self-priming pump and a dialysis cavity are installed in the dialysis water tank, a dialysis bag is hung in the dialysis cavity, and the liquid inlet and the liquid outlet of the dialysis bag are connected to the liquid pumping pump and the self-priming pump through liquid inlet electromagnetic valves and liquid outlet electromagnetic valves respectively; the liquid pumping pump is connected to the liquid pumping electromagnetic valve of the dialysate storage tank, and the self-priming pump is connected to the liquid inlet of the finished product storage tank; water inlet electromagnetic valves and water outlet electromagnetic valves are further installed on the dialysis cavity; and the PLC control cabinet is connected to all electromagnetic valves, the liquid pumping pump and the self-priming pump. The application adopts the PLC to monitor information of each module and control a dialysis process, liberates manual work, reduces cost, improves dialysis precision at the same time, ensures purification quality, improves product purity, automatically monitors a dialysis end point, improves consistency of purification, sets a dialysis circulating flow system and improves dialysis efficiency.

Description

Technical Field

[0001] This invention relates to the field of dialysis technology, specifically to a silk fibroin solution purification device and purification method. Background Technology

[0002] Silk fibroin, as a natural high-molecular biomaterial, has seen rapid development in recent years in fields such as biomedicine (e.g., wound dressings, tissue engineering scaffolds), cosmetics (e.g., high-end skincare ingredients), and food (e.g., functional additives) due to its excellent biocompatibility, biodegradability, and mechanical properties. However, with downstream applications demanding increasingly higher purity levels for silk fibroin (pharmaceutical grade requires ≥98% purity, cosmetic grade requires ≥95%), purification processes have become a core constraint on its industrialization.

[0003] Dialysis, a crucial step in silk fibroin purification, is primarily used to remove salts (such as calcium chloride and lithium bromide), small molecule degradation products, and impurity proteins introduced during dissolution. Early dialysis devices were mainly manually operated static immersion systems, suitable only for small-batch laboratory preparations. With the scaling up of silk fibroin applications, semi-automatic dialysis equipment has gradually emerged, but it still suffers from low efficiency and poor temperature control accuracy. Currently, the industry urgently needs dialysis devices that are highly efficient, precise, intelligent, and highly compatible to meet the production demands of high-purity silk fibroin in various scenarios.

[0004] Patent CN220907407U discloses a silk fibroin purification device, which uses a structure where dialysis bags are statically placed in a dialysis tank, relying on natural diffusion for mass exchange. It is equipped with an ultrafiltration component to pre-treat the filtrate to shorten dialysis time, but the mass transfer efficiency during dialysis is low. Patent CN216472999U discloses a silk fibroin purification device, which uses a stirring shaft in the dialysis tank to accelerate mass transfer by agitating the dialysis solution. However, the dialysis bag fixing method is complex, and it lacks a precise temperature and pH control system, making operation complicated. Patent CN219789906U discloses a silk fibroin solution dialysis device, which uses a structure combining tubular dialysis bags and circulation tubing to achieve dialysis solution circulation. However, manual monitoring is required, and solution residue is easily caused during the collection process.

[0005] Existing static immersion devices suffer from slow migration rates of small molecule impurities, requiring 24-72 hours for a single dialysis session. While stirred and circulating devices offer improvements, they still have limited contact area between the dialysis bag and the dialysate (e.g., a flat dialysis bag has a contact area of ​​only 0.2-0.5 μm). 2The mass transfer efficiency still needs improvement, making it difficult to meet the needs of large-scale production. Furthermore, the purification quality is unstable; silk fibroin is prone to denaturation or precipitation at pH < 6.5 or > 7.5, leading to fluctuations in product quality. Relying solely on manual experience to change the dialysis solution can easily result in incomplete dialysis (impurity residue > 5 ppm) or excessive waste. Moreover, manual operation is cumbersome, has poor compatibility, low automation, increases the cost of manual intervention, and is prone to contamination due to human error. Summary of the Invention

[0006] This invention addresses the shortcomings of existing technologies by providing a silk fibroin solution purification device and method. It employs a PLC control cabinet to monitor information from each module and control the dialysis process, freeing up manual labor, reducing costs, improving dialysis accuracy, ensuring purification quality, preventing silk fibroin denaturation, and increasing product purity. Simultaneously, it automatically monitors the dialysis endpoint, improving purification consistency. A dialysis circulation system is incorporated to enhance dialysis efficiency, shortening the single dialysis session time to 8-12 hours.

[0007] To solve the above-mentioned technical problems, the first aspect of the present invention provides a silk fibroin solution purification device, including a dialysis fluid storage tank, a dialysis water tank, a finished product storage tank, and a PLC control cabinet.

[0008] The dialysis tank is equipped with a liquid pump, a self-priming pump and a dialysis chamber. Several dialysis bags are suspended in the dialysis chamber. The inlet and outlet of the dialysis bags are connected to the liquid pump and the self-priming pump through an inlet solenoid valve and a outlet solenoid valve, respectively.

[0009] The pump is connected to the solenoid valve of the dialysate storage tank, and the self-priming pump is connected to the inlet of the finished product storage tank.

[0010] The dialysis chamber is also equipped with an inlet solenoid valve and an outlet solenoid valve.

[0011] The PLC control cabinet connects all solenoid valves, liquid pumps, and self-priming pumps.

[0012] This invention sets up a dialysis circulation system to improve mass transfer efficiency, thereby improving dialysis efficiency and shortening dialysis time. At the same time, it uses PLC to control the start and stop of each solenoid valve, liquid pump, and self-priming pump, realizing the full automation of the dialysis process, freeing up manual labor, reducing costs, and avoiding contamination caused by human intervention and operational errors.

[0013] Furthermore, a first conductivity sensor and a pH sensor connected to the PLC control cabinet are installed inside the dialysis chamber. Preferably, a temperature sensor, a heating element, and a cooling element are also included. The PLC monitors the conductivity, pH, and temperature parameters inside the dialysis chamber in real time; the pH range is set to 7.0±0.1, and when the pH sensor detects a deviation from 7.0±0.1, the metered infusion pump precisely injects HCl or NaOH to adjust the pH; the temperature range is set to 20±0.5℃, and a heating element and a cooling element are installed inside the dialysis chamber. The heating element is activated when the temperature is below 19.5℃, and the cooling element is activated when the temperature is above 20.5℃.

[0014] Furthermore, a first pressure sensor connected to the PLC control cabinet is installed inside the finished product storage tank.

[0015] Furthermore, a second conductivity sensor and a second pressure sensor are installed inside the dialysis fluid storage tank and connected to the PLC control cabinet.

[0016] Furthermore, the dialysis chamber, finished product storage tank, and dialysate storage tank are all equipped with low-level and high-level gauges connected to the PLC control cabinet.

[0017] Furthermore, both the finished product storage tank and the dialysis fluid storage tank are equipped with pressure relief valves connected to the PLC control cabinet.

[0018] This invention uses a PLC to control various sensors, enabling precise regulation of the dialysis process, improving dialysis accuracy, and ensuring product purity. At the same time, it automatically detects the dialysis endpoint and completes the storage of the finished dialysis product, resulting in high dialysis accuracy and consistency.

[0019] The purification device of this invention can process 5L of crude liquid in only 8 hours, which is 50% faster than traditional devices; the removal rate of small molecule impurities is ≥95%, and the purity of silk fibroin is ≥98%; the recovery rate of the automatic collection system is ≥99%, with no residue; the temperature and pH are precisely controlled (temperature ±0.1℃, pH ±0.01), and the product activity retention rate is ≥97%; the stainless steel, polytetrafluoroethylene and other materials are corrosion resistant, and the equipment life is ≥5 years.

[0020] Furthermore, the surface of the dialysis bag is provided with several hemispherical protrusions to increase the mass transfer area of ​​the dialysis bag.

[0021] A second aspect of the present invention provides a purification method for the silk fibroin solution purification apparatus described in the first aspect, comprising the following steps:

[0022] S1. The equipment is powered on, and the PLC control cabinet collects information on conductivity, pressure, and liquid level in the dialysis fluid storage tank.

[0023] S2, the PLC control cabinet controls the opening of the liquid extraction solenoid valve, the liquid extraction pump, and the liquid inlet solenoid valve. After the dialysate in the dialysate storage tank is quantitatively discharged into the dialysis bag, the liquid extraction solenoid valve, the liquid extraction pump, and the liquid inlet solenoid valve are closed.

[0024] S3, the PLC control cabinet controls the opening of the inlet and outlet solenoid valves to realize the circulation of water in and out of the dialysis chamber. At the same time, the PLC control cabinet collects conductivity and pH information in the dialysis chamber.

[0025] S4. When the rate of change of conductivity and pH value in the dialysis chamber both reach the threshold, stop the water intake and at the same time open the drain solenoid valve and the self-priming pump to drain the dialysate in the dialysis bag into the finished product storage tank.

[0026] Furthermore, the threshold for the rate of change of conductivity is: <0.5 μS / cm / h for 2 consecutive hours; the threshold for pH is 7.0 ± 0.1.

[0027] Furthermore, in S1, when the pressure and liquid level information are within the normal range, the process proceeds to S2; when the pressure exceeds the threshold, the pressure relief valve is opened; and when the liquid level is insufficient, dialysate is added.

[0028] The beneficial effects of this invention are:

[0029] This invention sets up a dialysis circulation system to improve mass transfer efficiency, thereby improving dialysis efficiency and shortening dialysis time. At the same time, it uses PLC to control the start and stop of each solenoid valve, liquid pump, and self-priming pump, realizing the full automation of the dialysis process, freeing up manual labor, reducing costs, and avoiding contamination caused by human intervention and operational errors.

[0030] This invention uses a PLC to control various sensors, enabling precise regulation of the dialysis process, improving dialysis accuracy, and ensuring product purity. At the same time, it automatically detects the dialysis endpoint and completes the storage of the finished dialysis product, resulting in high dialysis accuracy and consistency. Attached Figure Description

[0031] To more clearly illustrate the technical solution of the present invention, the drawings used in the embodiments will be briefly introduced below. Obviously, the drawings described below are only embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0032] Figure 1 This is a schematic diagram of the silk fibroin solution purification device of the present invention;

[0033] Figure 2 This is a schematic diagram of the dialysis tank structure of the present invention;

[0034] Explanation of the labels in the diagram:

[0035] 1. Dialysis fluid storage tank; 101. Liquid extraction solenoid valve; 102. Second conductivity sensor; 103. Second pressure sensor; 104. Pressure relief valve.

[0036] 2. Dialysis water tank, 201. Liquid pump, 202. Self-priming pump, 203. Dialysis chamber, 204. Dialysis bag, 205. Inlet solenoid valve, 206. Outlet solenoid valve, 207. First conductivity sensor, 208. pH sensor, 209. Liquid inlet solenoid valve, 210. Liquid outlet solenoid valve;

[0037] 3. Finished product storage tank; 301. First pressure sensor;

[0038] 4. PLC control cabinet; 5. Low level gauge; 6. High level gauge. Detailed Implementation

[0039] The technical solution of the present invention will be clearly and completely described below with reference to specific embodiments. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0040] In this invention, unless otherwise stated, the terms "center," "upper," "lower," "left," "right," "vertical," "horizontal," "inner," and "outer," indicating orientation or positional relationships, are merely for the convenience of describing the invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation, and therefore should not be construed as a limitation of the invention. The terms "first," "second," and "third" are used for descriptive purposes only and should not be construed as indicating or implying relative importance. Furthermore, unless otherwise explicitly specified and limited, the terms "installed," "connected," and "linked" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral connection; they can refer to a mechanical connection or an electrical connection; they can refer to a direct connection or an indirect connection through an intermediate medium; and they can refer to the internal connection of two components. For those skilled in the art, the specific meaning of the above terms in this patent can be understood according to the specific circumstances.

[0041] Reference Figure 1-2As shown, this embodiment relates to a silk fibroin solution purification device, including a dialysis fluid storage tank 1, a dialysis water tank 2, a finished product storage tank 3, and a PLC control cabinet 4. The dialysis water tank 2 is equipped with a pump 201, a self-priming pump 202, and a dialysis chamber 203. Several dialysis bags 204 are suspended inside the dialysis chamber 203. The inlet and outlet of each dialysis bag 204 are connected to the pump 201 and the self-priming pump 202 respectively via an inlet solenoid valve 209 and a outlet solenoid valve 210. The pump 201 is connected to the pumping solenoid valve 101 of the dialysis fluid storage tank 1, and the self-priming pump 202 is connected to the inlet of the finished product storage tank 3. The dialysis chamber 203 is also equipped with an inlet solenoid valve 205 and an outlet solenoid valve 206. The PLC control cabinet 4 is connected to all solenoid valves, the pump 201, and the self-priming pump 202. This embodiment sets up a dialysis circulation system to improve mass transfer efficiency, thereby improving dialysis efficiency and shortening dialysis time. At the same time, PLC is used to control the start and stop of each solenoid valve, the liquid pump 201, and the self-priming pump 202 to realize the full automation of the dialysis process, freeing up manual labor, reducing costs, and avoiding contamination caused by human intervention and operational errors.

[0042] In a preferred embodiment, a first conductivity sensor 207 and a pH sensor 208 connected to a PLC control cabinet are installed inside the dialysis chamber 203; more preferably, a temperature sensor connected to a PLC control cabinet 4 is installed inside the dialysis chamber 203 to detect the conductivity, pH, and temperature parameters inside the dialysis chamber 203 in real time; the pH range is set to 7.0±0.1, and when the pH sensor 208 detects a deviation from 7.0±0.1, the quantitative infusion pump precisely injects HCl or NaOH to adjust; the temperature range is set to 20±0.5℃, and a heating tube and a cooling plate are installed inside the dialysis chamber 203, with the heating tube activated when the temperature is below 19.5℃ and the cooling plate activated when the temperature is above 20.5℃.

[0043] In a preferred embodiment, the finished product storage tank 3 is equipped with a first pressure sensor 301 connected to the PLC control cabinet; the dialysate storage tank 1 is equipped with a second conductivity sensor 102 and a second pressure sensor 103 connected to the PLC control cabinet; both the finished product storage tank 3 and the dialysate storage tank 1 are equipped with a pressure relief valve 104 connected to the PLC control cabinet. When the first pressure sensor 301 and the second pressure sensor 103 detect that the pressure is too high, the pressure relief valve 104 is opened to release pressure through PLC control.

[0044] This embodiment utilizes PLC-controlled sensors to achieve precise regulation of the dialysis process, improving dialysis accuracy and ensuring product purity. Simultaneously, it automatically detects the dialysis endpoint and stores the finished product, ensuring high dialysis accuracy and consistency. The purification device processes 5L of crude liquid in just 8 hours, 50% faster than traditional devices; small molecule impurity removal rate ≥95%, silk fibroin purity ≥98%; automatic collection system recovery rate ≥99%, no residue; high-precision temperature and pH control (temperature ±0.1℃, pH ±0.01), product activity retention rate ≥97%; corrosion-resistant materials such as stainless steel and PTFE ensure equipment lifespan ≥5 years.

[0045] In a preferred embodiment, the dialysis chamber 203, the finished product storage tank 3, and the dialysis fluid storage tank 1 are all equipped with a low level gauge 5 and a high level gauge 6 connected to the PLC control cabinet.

[0046] In a preferred embodiment, the surface of the dialysis bag 204 is provided with a plurality of hemispherical protrusions.

[0047] Another embodiment relates to a purification method using the silk fibroin solution purification apparatus described in the above embodiments, comprising the following steps:

[0048] S1. The equipment is powered on, and the PLC control cabinet 4 collects the conductivity, pressure, and liquid level information in the dialysate storage tank 1; when the pressure and liquid level information are within the normal range, proceed to S2; when the pressure exceeds the threshold, the pressure relief valve 104 is opened; when the liquid level is insufficient, dialysate is added.

[0049] S2, PLC control cabinet 4 controls the opening of liquid extraction solenoid valve 101, liquid extraction pump 201, and liquid inlet solenoid valve 209. After the dialysate in the dialysate storage tank 1 is quantitatively discharged into the dialysate bag 204, the liquid extraction solenoid valve 101, liquid extraction pump 201, and liquid inlet solenoid valve 209 are closed.

[0050] S3 and PLC control cabinet 4 control the opening of the inlet solenoid valve 205 and the outlet solenoid valve 206 to realize the water inlet and outlet circulation in the dialysis chamber 203. At the same time, PLC control cabinet 4 collects conductivity and pH information in the dialysis chamber 203, and preferably also collects temperature information; the pH range is set to 7.0±0.1. When the pH sensor 208 detects a deviation from 7.0±0.1, the quantitative infusion pump accurately injects HCl or NaOH to adjust; the temperature range is set to 20±0.5℃. A heating tube and a cooling plate are installed in the dialysis chamber 203. The heating tube is activated when the temperature is below 19.5℃ and the cooling plate is activated when the temperature is above 20.5℃.

[0051] S4. When the rate of change of conductivity and pH value in the dialysis chamber 203 both reach the threshold, stop the water intake and at the same time open the drain solenoid valve 210 and the self-priming pump 202 to drain the dialysis fluid in the dialysis bag 204 into the finished product storage tank 3.

[0052] In a preferred embodiment, the threshold for the rate of change of conductivity is: <0.5 μS / cm / h for 2 consecutive hours; and the threshold for pH is 7.0 ± 0.1.

[0053] In summary, this invention features a dialysis circulation system that improves mass transfer efficiency, thereby increasing dialysis efficiency and shortening dialysis time. Simultaneously, the use of a PLC to control the start and stop of various solenoid valves, the pump, and the self-priming pump enables fully automated dialysis, freeing up manual labor, reducing costs, and avoiding contamination caused by human error. Furthermore, PLC-controlled sensors enable precise regulation of the dialysis process, improving dialysis accuracy and ensuring product purity. Finally, the invention automatically detects the dialysis endpoint and stores the finished dialysis product, resulting in high dialysis accuracy and consistency.

[0054] The present invention has been described in detail above with reference to specific embodiments and exemplary examples; however, these descriptions should not be construed as limiting the present invention. Those skilled in the art will understand that various equivalent substitutions, modifications, or improvements can be made to the technical solutions and embodiments of the present invention without departing from the spirit and scope of the invention, and all such modifications and improvements fall within the scope of the present invention. The scope of protection of the present invention is defined by the appended claims.

Claims

1. A silk fibroin solution purification device, characterized in that, Includes dialysis fluid storage tank, dialysis water tank, finished product storage tank, and PLC control cabinet; The dialysis tank is equipped with a liquid pump, a self-priming pump and a dialysis chamber. Several dialysis bags are suspended in the dialysis chamber. The inlet and outlet of the dialysis bags are connected to the liquid pump and the self-priming pump through an inlet solenoid valve and a outlet solenoid valve, respectively. The pump is connected to the solenoid valve of the dialysate storage tank, and the self-priming pump is connected to the inlet of the finished product storage tank. The dialysis chamber is also equipped with an inlet solenoid valve and an outlet solenoid valve. The PLC control cabinet connects all solenoid valves, liquid pumps, and self-priming pumps.

2. The silk fibroin solution purification apparatus as described in claim 1, characterized in that, The dialysis chamber is equipped with a first conductivity sensor and a pH sensor connected to the PLC control cabinet.

3. The silk fibroin solution purification apparatus as described in claim 1, characterized in that, The finished product storage tank is equipped with a first pressure sensor that is connected to the PLC control cabinet.

4. The silk fibroin solution purification apparatus as described in claim 1, characterized in that, The dialysis fluid storage tank is equipped with a second conductivity sensor and a second pressure sensor connected to the PLC control cabinet.

5. The silk fibroin solution purification apparatus as described in claim 1, characterized in that, The dialysis chamber, finished product storage tank, and dialysis fluid storage tank are all equipped with low-level and high-level gauges connected to the PLC control cabinet.

6. The silk fibroin solution purification apparatus as described in claim 1, characterized in that, Both the finished product storage tank and the dialysis fluid storage tank are equipped with pressure relief valves connected to the PLC control cabinet.

7. The silk fibroin solution purification apparatus as described in claim 1, characterized in that, The surface of the dialysis bag is provided with several hemispherical protrusions.

8. A purification method for a silk fibroin solution purification apparatus according to any one of claims 1-7, characterized in that, Includes the following steps: S1. The equipment is powered on, and the PLC control cabinet collects information on conductivity, pressure, and liquid level in the dialysis fluid storage tank. S2, the PLC control cabinet controls the opening of the liquid extraction solenoid valve, the liquid extraction pump, and the liquid inlet solenoid valve. After the dialysate in the dialysate storage tank is quantitatively discharged into the dialysis bag, the liquid extraction solenoid valve, the liquid extraction pump, and the liquid inlet solenoid valve are closed. S3, the PLC control cabinet controls the opening of the inlet and outlet solenoid valves to realize the circulation of water in and out of the dialysis chamber. At the same time, the PLC control cabinet collects conductivity and pH information in the dialysis chamber. S4. When the rate of change of conductivity and pH value in the dialysis chamber both reach the threshold, stop the water intake and at the same time open the drain solenoid valve and the self-priming pump to drain the dialysate in the dialysis bag into the finished product storage tank.

9. The purification method of the silk fibroin solution purification apparatus as described in claim 8, characterized in that, The threshold for the rate of change of conductivity is: <0.5 μS / cm / h for 2 consecutive hours; the threshold for pH is 7.0 ± 0.

1.

10. The purification method of the silk fibroin solution purification apparatus as described in claim 8, characterized in that, In S1, when the pressure and liquid level information are within the normal range, the process proceeds to S2; when the pressure exceeds the threshold, the pressure relief valve is opened; when the liquid level is insufficient, dialysate is added.

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