Device for separating and extracting fibroin and sericin from high-pressure water vapor and extraction method thereof
This method directly extracts sericin using a high-pressure steam separation device and an extrusion drive mechanism, solving the problems of low recovery rate and severe loss in traditional methods. It achieves efficient, green, and environmentally friendly separation of fibroin and sericin, suitable for laboratory and industrial production.
Patent Information
- Application Number
- CN202411682319.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-22
- Publication Date
- 2025-10-21
- Estimated Expiration
- 2044-11-22
AI Technical Summary
Existing high-temperature hydrolysis methods have low recovery rates when extracting sericin, and significant losses occur during water vapor condensation and subsequent separation, resulting in low efficiency and unsuitability for industrial applications.
A high-pressure steam separation device is used, which utilizes a high-pressure outer cylinder and inner cylinder structure, combined with an extrusion drive mechanism and a safety valve, to directly extract sericin protein under high temperature and high pressure, and obtain pure silk fibroin through a solid-liquid separation channel and freeze-drying method.
It improves the extraction rate of sericin, simplifies the operation process, and achieves efficient, green and environmentally friendly separation of fibroin and sericin, which is suitable for laboratory and industrial production.
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Figure CN119771015B_ABST
Abstract
Description
Technical Field
[0001] The present invention belongs to the technical field of separation and extraction, and particularly relates to a device for separating and extracting silk fibroin and sericin using high-pressure steam and an extraction method thereof. Background Art
[0002] During the traditional silk degumming process, sericin is removed, while the silk fibers, primarily composed of fibroin, are retained for textile production. Currently, there are two main methods for extracting sericin: physical and chemical. High-temperature hydrolysis is the most commonly used method. While this method preserves the natural structure of sericin, its recovery rate is low, making it unsuitable for large-scale industrial extraction.
[0003] High-pressure steam extraction involves evaporating water into steam, dissolving the soluble sericin in water. High pressure increases the recovery rate of sericin. This method is environmentally friendly, simple, and effective, while preserving the natural structure of sericin.
[0004] However, the existing high-pressure steam extraction method has the following defects: First, the water vapor will partially condense during the extraction process, reducing the amount of water vapor and lowering the extraction effect; in addition, the sericin protein after steam extraction needs to be manually separated, and the sericin protein will be lost during this process. Summary of the Invention
[0005] Based on the above-mentioned shortcomings and deficiencies in the prior art, one of the objects of the present invention is to at least solve one or more of the above-mentioned problems in the prior art. In other words, one of the objects of the present invention is to provide a device for separating and extracting silk fibroin and sericin with high-pressure water vapor and an extraction method thereof that meet one or more of the above-mentioned needs.
[0006] In order to achieve the above-mentioned object of the invention, the present invention adopts the following technical solutions:
[0007] A device for separating and extracting silk fibroin and sericin by high-pressure steam comprises a high-pressure outer cylinder, an outer cylinder sealing cover disposed above the high-pressure outer cylinder, and an extrusion drive mechanism. An inner cylinder and a heater are disposed within the high-pressure outer cylinder, and the inner cylinder sealing cover is disposed above the inner cylinder. The inner cylinder sealing cover is provided with a safety valve configured to automatically open upon a preset pressure within the high-pressure outer cylinder, thereby connecting the high-pressure outer cylinder and the inner cylinder. The heater is configured to heat water entering the high-pressure outer cylinder to form steam. The inner cylinder comprises a cocoon processing chamber and a sericin storage chamber. The cocoon processing chamber is located above the sericin storage chamber and is connected to the sericin storage chamber via a solid-liquid separation channel. The sericin storage chamber is connected to the exterior of the high-pressure outer cylinder via a drain pipe equipped with an on / off valve. The cocoon processing chamber is provided with an extrusion plate having an array of vent holes. The extrusion drive mechanism extends through the inner cylinder sealing cover to drive the extrusion plate to extrude the steam-treated cocoons within the cocoon processing chamber, causing the extruded liquid to flow into the sericin storage chamber.
[0008] As a preferred solution, a support frame is provided at the bottom of the inner cavity of the high-pressure outer cylinder, and the inner cylinder is provided on the support frame;
[0009] The heater is located in the support frame.
[0010] As a preferred solution, the extrusion drive mechanism is a telescopic air cylinder or a hydraulic telescopic oil cylinder.
[0011] As a preferred solution, the high-pressure outer cylinder is provided with a temperature sensor and a pressure sensor for detecting the temperature and pressure of the water vapor in the inner cavity of the high-pressure outer cylinder.
[0012] As a preferred embodiment, the device for separating and extracting silk fibroin and sericin by high-pressure steam further includes a controller and a touch screen, and the touch screen, heater, extrusion drive mechanism, temperature sensor, and pressure sensor are connected to the controller signal.
[0013] As a preferred solution, the high-pressure outer cylinder has a water inlet and a water outlet;
[0014] The water inlet of the high-pressure outer cylinder is connected to a water inlet pipe, and the water inlet pipe is provided with a water inlet valve;
[0015] The water outlet of the high-pressure outer cylinder is connected to a water outlet pipe, and the water outlet pipe is provided with a water outlet valve.
[0016] As a preferred solution, a sealing ring is provided between the outer cylinder sealing cover and the high-pressure outer cylinder, and a sealing ring is provided between the inner cylinder sealing cover and the inner cylinder.
[0017] As a preferred solution, casters are provided at the bottom of the high-pressure outer cylinder.
[0018] The present invention also provides an extraction method for the device for separating and extracting silk fibroin and sericin using high-pressure steam as described in any of the above schemes, comprising the following steps:
[0019] (1) Place the cocoons into the cocoon processing chamber of the inner cylinder, add water to the high-pressure outer cylinder, and close the inner cylinder sealing cover and the outer cylinder sealing cover;
[0020] (2) The heater heats the water and evaporates it into water vapor. When the inner cavity of the high-pressure outer cylinder reaches the preset pressure, the safety valve automatically opens, and the water vapor enters the inner cylinder. The extrusion drive mechanism drives the extrusion plate up and down to squeeze. The extruded liquid flows into the sericin storage cavity through the solid-liquid separation channel. The separation and extraction time is 0.5 to 1 hour.
[0021] (3) After the sericin extraction is completed, the sericin solution flows out from the drain tube, and freeze-dried sericin is obtained by freeze-drying;
[0022] The sample in the cocoon processing chamber is taken out and rinsed with clean water to obtain silk fibroin.
[0023] As a preferred solution, the preset pressure is 0.1-0.2 MPa, and the heating temperature of the heater is 110-130°C.
[0024] Compared with the prior art, the present invention has the following beneficial effects:
[0025] 1. Traditional high-temperature hydrolysis processes do not apply high pressure, resulting in a low sericin extraction rate and inability to completely separate silk fibroin from sericin. Subsequent degumming of the silk fibroin requires complex steps and low efficiency. However, the present invention utilizes high pressure and a heat-conducting inner cylinder to control the inner cylinder temperature above 100°C. A safety valve allows high-pressure steam to flow directly into the inner cylinder, allowing the sericin to be extracted directly at high temperature and high pressure.
[0026] 2. The traditional high-temperature hydrolysis process cannot directly separate silk fibroin from sericin. After the high-temperature hydrolysis, the sericin solution must be squeezed out, and a large amount of sericin is lost during this process. However, the sericin extracted by steam in the present invention is directly squeezed and separated through an extrusion plate. The sericin liquid flows directly into the sericin storage chamber through the solid-liquid separation channel. After being squeezed, the cocoons can continue to pass through high-pressure steam to continue extracting the remaining sericin, thereby improving the sericin extraction rate. After the extraction is completed, the sericin solution flows out of the drainage pipe and is freeze-dried to obtain freeze-dried sericin. The sample from the cocoon processing chamber is removed and rinsed with clean water to obtain pure silk fibroin.
[0027] 3. The device of the present invention controls the extraction temperature, pressure and time through the parameter settings of the touch screen, and detects the temperature and pressure through the temperature sensor and pressure sensor, so that the temperature, pressure and time can be fully controlled;
[0028] 4. The water inflow and outflow of the high-pressure outer cylinder of the present invention can be controlled by the water inlet valve and the water outlet valve. When cleaning the inner cylinder, it is only necessary to add clean water to the cocoon processing chamber and open the on-off valve of the drain pipe to complete the cleaning, which is simple and easy to operate.
[0029] 5. The device of the present invention is simple to operate, can run continuously, has high efficiency, and the extraction method is green and environmentally friendly, and can be applied to laboratories and industrial production. BRIEF DESCRIPTION OF THE DRAWINGS
[0030] Figure 1 Schematic diagram of the structure of the device for separating and extracting silk fibroin and sericin using high-pressure steam according to Example 1 of the present invention. DETAILED DESCRIPTION
[0031] To more clearly illustrate the embodiments of the present invention, specific embodiments of the present invention will be described below with reference to the accompanying drawings. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings and other embodiments can be obtained based on these drawings without inventive efforts.
[0032] Example 1:
[0033] like Figure 1 As shown, the device for separating and extracting silk fibroin and sericin using high-pressure steam in this embodiment includes a high-pressure outer cylinder 1, an outer cylinder sealing cover 2, an inner cylinder 3, an inner cylinder sealing cover 4, a hydraulic telescopic cylinder 5, an extrusion plate 6, a heater 7 and a support frame 8.
[0034] The high-pressure outer cylinder 1 in this embodiment is a cylindrical structure with an open top, closed by an outer cylinder sealing cover 2. A sealing ring 9 is installed between the high-pressure outer cylinder 1 and the outer cylinder sealing cover 2 to enhance sealing. The outer cylinder sealing cover 2 is equipped with a controller, a touch screen 10, and an integrated temperature and pressure sensor 11. The probe of the integrated temperature and pressure sensor 11 extends into the inner cavity of the high-pressure outer cylinder 1 to detect the temperature and pressure inside the high-pressure outer cylinder 1. The hydraulic telescopic cylinder 5, heater 7, touch screen 10, and integrated temperature and pressure sensor 11 are all connected to the controller for signal transmission, enabling intelligent control.
[0035] The support frame 8 of this embodiment is installed at the bottom of the inner cavity of the high-pressure outer cylinder 1 to support the inner cylinder 3. The support frame 8 is internally installed with a heater 7 for heating the water in the high-pressure outer cylinder 1 to generate water vapor.
[0036] The inner cylinder 3 of this embodiment is a cylindrical structure with an open top. A cocoon processing chamber 3-1, a solid-liquid separation channel 3-3, and a sericin storage chamber 3-2 are arranged in order along its axial direction from top to bottom. The cocoon processing chamber 3-1 and the sericin storage chamber 3-2 are connected through the solid-liquid separation channel 3-3. The top opening of the inner cylinder 3 is covered by an inner cylinder sealing cover 4. A sealing ring is provided between the inner cylinder 3 and the outer cylinder sealing cover 2 to improve sealing performance. Furthermore, the sericin storage chamber 3-2 is connected to the exterior of the high-pressure outer cylinder 1 via a drain pipe 12 equipped with an on / off valve 13. A circular extrusion plate 6 is disposed within the cocoon processing chamber 3-1. The extrusion plate 6 has an array of vent holes 60. A hydraulic telescopic cylinder 5 is mounted in the center of the outer cylinder sealing cover 2. The telescopic rod of the hydraulic telescopic cylinder 5 extends through the outer cylinder sealing cover 2 and the inner cylinder sealing cover 4 and is connected to the extrusion plate 6. This drives the extrusion plate 6 to squeeze the steam-treated cocoons within the cocoon processing chamber 3-1. The extruded liquid then flows through the solid-liquid separation channel 3-3 to the sericin storage chamber 3-2.
[0037] The inner cylinder sealing cover 4 of this embodiment is provided with a safety valve 14 , which is used to automatically open when the inner cavity of the high-pressure outer cylinder reaches a preset pressure to connect the high-pressure outer cylinder 1 with the inner cylinder 3 .
[0038] The water inlet of the high-pressure outer cylinder 1 of this embodiment is connected to an inlet pipe 15, which is equipped with an inlet valve 16 to facilitate external water supply. The water outlet of the high-pressure outer cylinder 1 is connected to an outlet pipe 17, which is equipped with an outlet valve 18 to control the water output. In addition, the bottom of the high-pressure outer cylinder 1 of this embodiment is equipped with casters 19 to facilitate the movement of the entire device.
[0039] The extraction method of the device for separating and extracting silk fibroin and sericin using high-pressure steam in this embodiment includes the following steps:
[0040] Open the outer cylinder sealing cover and the inner cylinder sealing cover;
[0041] Silkworm cocoons are placed in the cocoon processing chamber of the inner cylinder, water is added to the high-pressure outer cylinder, and the inner and outer cylinder sealing covers are closed. The heater heats the water to evaporate it into steam. When the inner chamber of the high-pressure outer cylinder reaches the preset pressure, the safety valve automatically opens, and the steam enters the inner cylinder. The hydraulic telescopic cylinder drives the extrusion plate up and down to squeeze. The extruded liquid flows into the sericin storage chamber through the solid-liquid separation channel. The separation and extraction time is 0.5 to 1 hour. The preset pressure is 0.1 to 0.2 MPa, and the heating temperature of the heater is 110 to 130 degrees Celsius.
[0042] After the sericin protein extraction is completed, the sericin protein solution flows out from the drainage tube, and the sericin protein freeze-dried product is obtained by freeze-drying;
[0043] The sample in the cocoon processing chamber is taken out and rinsed with clean water to obtain silk fibroin;
[0044] The remaining unevaporated water in the high-pressure outer cylinder is discharged from the water outlet pipe.
[0045] The device of this embodiment is used to separate and extract silk fibroin and sericin. The specific process is as follows:
[0046] 50 g of shredded and cleaned silkworm cocoons were placed in a 10 L cocoon processing chamber. The water inlet was opened and 10 L of water was added. The parameters were set at 0.14 MPa, 125°C, and 30 min. The water was evaporated into steam. After reaching the target time and pressure parameters, the safety valve opened, and steam was introduced into the cocoon processing chamber. Simultaneously, the extrusion plate began to squeeze up and down, and the extruded liquid flowed into the sericin storage chamber through the solid-liquid separation channel. After the sericin extraction was completed, the sericin solution flowed out of the drainage pipe and was centrifuged at 6000 rpm for 10 min. The supernatant was then freeze-dried to obtain freeze-dried sericin. The sample from the cocoon processing chamber was removed, rinsed with clean water, and dried to obtain pure silk fibroin. The remaining water flowed out of the water outlet.
[0047] The recommended parameter settings for the green separation and extraction of silk fibroin and sericin by high-pressure steam are shown in Table 1.
[0048] Table 1 Recommended parameters for separation and extraction of silk fibroin and sericin
[0049]
[0050] Higher temperatures increase extraction efficiency, but excessively high temperatures may lead to degradation of sericin. Increasing pressure helps accelerate the dissolution and diffusion of sericin, but it should be kept within an appropriate range to prevent thermal degradation. Extraction time is closely related to temperature and pressure, with higher temperatures and pressures generally shortening extraction time.
[0051] Example 2:
[0052] The device for separating and extracting silk fibroin and sericin with high-pressure steam in this embodiment differs from that in Example 1 in that:
[0053] The hydraulic telescopic cylinder is replaced with a telescopic cylinder to meet the needs of different applications;
[0054] For other structures, please refer to Example 1.
[0055] Example 3:
[0056] The device for separating and extracting silk fibroin and sericin with high-pressure steam in this embodiment differs from that in Example 1 in that:
[0057] The cocoon processing chamber and sericin storage chamber can be designed as a split type, and the two can be connected by a solid-liquid separation pipeline to meet the needs of different applications;
[0058] For other structures, please refer to Example 1.
[0059] The above description is only a detailed description of the preferred embodiments and principles of the present invention. For ordinary technicians in this field, based on the ideas provided by the present invention, there may be changes in the specific implementation methods, and these changes should also be considered as the scope of protection of the present invention.
Claims
1. A device for separating and extracting silk fibroin and sericin using high-pressure steam, characterized in that: The invention comprises a high-pressure outer cylinder, an outer cylinder sealing cover disposed on the high-pressure outer cylinder, and an extrusion drive mechanism. The high-pressure outer cylinder houses an inner cylinder and a heater, and the inner cylinder sealing cover is disposed on the inner cylinder. The inner cylinder sealing cover is provided with a safety valve, which automatically opens when the inner cavity of the high-pressure outer cylinder reaches a preset pressure, thereby connecting the high-pressure outer cylinder and the inner cylinder. The heater is configured to heat water entering the high-pressure outer cylinder to form steam. The inner cylinder comprises a cocoon processing chamber and a sericin storage chamber. The cocoon processing chamber is located above the sericin storage chamber and is connected via a solid-liquid separation channel. The sericin storage chamber is connected to the exterior of the high-pressure outer cylinder via a drainage pipe, which is provided with an on-off valve. The cocoon processing chamber is provided with an extrusion plate having an array of vent holes. The extrusion drive mechanism extends through the inner cylinder sealing cover to drive the extrusion plate to extrude the steam-treated cocoons in the cocoon processing chamber, causing the extruded liquid to flow into the sericin storage chamber.
2. The device for separating and extracting silk fibroin and sericin using high-pressure steam according to claim 1, characterized in that: A support frame is provided at the bottom of the inner cavity of the high-pressure outer cylinder, and the inner cylinder is provided on the support frame; The heater is located in the support frame.
3. The device for separating and extracting silk fibroin and sericin using high-pressure steam according to claim 1, characterized in that: The extrusion drive mechanism is a telescopic air cylinder or a hydraulic telescopic oil cylinder.
4. The device for separating and extracting silk fibroin and sericin using high-pressure steam according to claim 1, characterized in that: The high-pressure outer cylinder is provided with a temperature sensor and a pressure sensor for detecting the temperature and pressure of water vapor in the inner cavity of the high-pressure outer cylinder.
5. The device for separating and extracting silk fibroin and sericin using high-pressure steam according to claim 4, characterized in that: It also includes a controller and a touch screen, and the touch screen, heater, extrusion drive mechanism, temperature sensor, and pressure sensor are connected to the controller signal.
6. The device for separating and extracting silk fibroin and sericin using high-pressure steam according to claim 1, characterized in that: The high-pressure outer cylinder has a water inlet and a water outlet; The water inlet of the high-pressure outer cylinder is connected to a water inlet pipe, and the water inlet pipe is provided with a water inlet valve; The water outlet of the high-pressure outer cylinder is connected to a water outlet pipe, and the water outlet pipe is provided with a water outlet valve.
7. The device for separating and extracting silk fibroin and sericin using high-pressure steam according to claim 1, characterized in that: A sealing ring is provided between the outer cylinder sealing cover and the high-pressure outer cylinder, and a sealing ring is provided between the inner cylinder sealing cover and the inner cylinder.
8. The device for separating and extracting silk fibroin and sericin using high-pressure steam according to claim 1, characterized in that: Casters are provided at the bottom of the high-pressure outer cylinder.
9. The extraction method of the device for separating and extracting silk fibroin and sericin with high-pressure steam according to any one of claims 1 to 8, characterized in that: The following steps are involved: (1) Place the cocoons into the cocoon processing chamber of the inner cylinder, add water to the high-pressure outer cylinder, and close the inner cylinder sealing cover and the outer cylinder sealing cover; (2) The heater heats the water and evaporates it into water vapor. When the inner cavity of the high-pressure outer cylinder reaches the preset pressure, the safety valve automatically opens, and the water vapor enters the inner cylinder. The extrusion drive mechanism drives the extrusion plate up and down to squeeze. The extruded liquid flows into the sericin storage cavity through the solid-liquid separation channel. The separation and extraction time is 0.5 to 1 hour. (3) After the sericin extraction is completed, the sericin solution flows out from the drain tube, and freeze-dried sericin is obtained by freeze-drying; The sample in the cocoon processing chamber is taken out and rinsed with clean water to obtain silk fibroin.
10. The extraction method according to claim 9, characterized in that The preset pressure is 0.1-0.2 MPa, and the heating temperature of the heater is 110-130°C.
Citation Information
Patent Citations
Multi-layer extrusion type supercritical extraction kettle
CN110404289A
Method for rapidly preparing regenerated fibroin solution
CN117143355A