A device and method for the integrated preparation of chitin micro- and nanofibers from crustaceans

Abstract

The application relates to a crustacean chitin micro-nano fiber preparation integrated equipment and method, and belongs to the technical field of micro-nano fiber preparation. The crustacean chitin micro-nano fiber preparation integrated equipment and method comprises an equipment rack, an alkaline hydrothermal oxidation reaction zone, a bleaching reaction zone and an acid pickling density sorting reaction zone which are installed on the equipment rack and are sequentially arranged along a material conveying direction, the alkaline hydrothermal oxidation reaction zone, the bleaching reaction zone and the acid pickling density sorting reaction zone are sequentially arranged on the equipment rack along the material conveying direction and are communicated through a joint device, a pretreatment process is continuously completed in the same equipment, process interruption and material loss caused by repeated filtration, washing, transportation and re-feeding of materials between processes are avoided, and the large-scale preparation efficiency of crustacean chitin micro-nano fibers is improved.

Description

Technical Field

[0001] This invention relates to the field of micro / nanofiber preparation technology, and in particular to an integrated device and method for preparing chitin micro / nanofibers from crustaceans. Background Technology

[0002] Chitin is an important natural polymer component in crustacean waste such as crab and shrimp shells. Chitin micro / nanofibers can be prepared after pretreatment processes including deproteinization, bleaching, decalcification, and mechanical dissociation. These chitin micro / nanofibers possess biodegradability, antibacterial activity, high specific surface area, and excellent mechanical properties, showing broad application prospects in fields such as biomedicine, food packaging, and functional composite materials. They provide an effective way to achieve high-value utilization of crustacean biomass resources.

[0003] Existing pretreatment processes typically employ multiple reaction devices to complete each processing step separately. Inter-step operations such as filtration, washing, transfer, and refeeding are required, forcing interruptions in the overall preparation process. Repeated material transfers increase material losses and make continuous production difficult, hindering the improvement of efficiency in large-scale preparation. Summary of the Invention

[0004] Therefore, it is necessary to provide an integrated equipment and method for preparing chitin micro / nanofibers from crustaceans, addressing the problem that existing pretreatment processes, which involve the use of multiple independent devices operating in segments and require material transfer between processes, lead to interruptions in the preparation process, increased material losses, and difficulty in achieving continuous and large-scale production.

[0005] An integrated device for the preparation of chitin micro / nanofibers from crustaceans, comprising: Equipment rack; The alkaline hydrothermal oxidation reaction zone, bleaching reaction zone, and pickling density sorting reaction zone are installed on the equipment frame, and are arranged sequentially along the material conveying direction. The alkaline hydrothermal oxidation reaction zone includes a sealed pressure tank and a mechanical crushing and stirring shaft, with the mechanical crushing and stirring shaft installed in the center of the sealed pressure tank. The bleaching reaction zone includes a first atmospheric pressure tank and a low-speed rotating blade agitator, wherein the low-speed rotating blade agitator is installed in the center of the first atmospheric pressure tank. The pickling density sorting reaction zone includes a second atmospheric pressure tank, an umbrella-shaped guide plate, a central shaft, an elliptical flipping plate, and an external drive mechanism. The umbrella-shaped guide plate is fixed inside the second atmospheric pressure tank. The central shaft passes through the second atmospheric pressure tank and one end of the central shaft extends out of the tank. The elliptical flipping plate is mounted on the arc surface of the central shaft. The external drive mechanism is fixed to the end of the central shaft that extends out of the second atmospheric pressure tank. The top of the sealed pressure tank, the first atmospheric pressure tank, and the second atmospheric pressure tank are all provided with inlets, the lower side of the sealed pressure tank, the first atmospheric pressure tank, and the second atmospheric pressure tank are all provided with outlets, and the bottom of the sealed pressure tank, the first atmospheric pressure tank, and the second atmospheric pressure tank are all provided with outlets. Three circumferential coarse screening and drainage components are respectively installed on the inner circumferential walls of the sealed pressure tank, the first atmospheric pressure tank, and the second atmospheric pressure tank. The quantity is three connector devices. The top connector device is installed between the outlet of the sealed pressure tank and the inlet of the first atmospheric pressure tank. The middle connector device is installed between the outlet of the first atmospheric pressure tank and the inlet of the second atmospheric pressure tank. The bottom connector device is installed at the outlet of the second atmospheric pressure tank. The topmost connector device includes a hollow short spiral feeder and an openable isolation valve. The inlet of the hollow short spiral feeder is connected to the outlet of the sealed pressure tank, and the outlet of the hollow short spiral feeder is connected to the inlet of the first atmospheric pressure tank. The openable isolation valve is installed on the outlet pipeline of the hollow short spiral feeder.

[0006] In one embodiment, the uppermost circumferential coarse screening and drainage assembly includes a screen that is fixedly connected to the inner wall of a sealed pressure tank, and the bottom of the screen has an annular liquid collection chamber that communicates with the discharge port.

[0007] In one embodiment, the screen installed in the sealed pressure tank has a mesh size of 20-40 mesh, the screen installed in the first atmospheric pressure tank has a mesh size of 60-100 mesh, and the screen installed in the second atmospheric pressure tank has a mesh size of 120-200 mesh.

[0008] In one embodiment, the surface of the alkaline hydrothermal oxidation reaction zone is provided with an oxygen inlet / outlet port and a pressure gauge.

[0009] In one embodiment, a washing water pipe is installed on the equipment frame, and a clean water sprayer is installed on the inner top of the sealed pressure tank, the first atmospheric pressure tank, and the second atmospheric pressure tank. The clean water sprayer is connected to the washing water pipe through a three-way solenoid valve.

[0010] In one embodiment, the outer walls of the sealed pressure tank, the first atmospheric pressure tank, and the second atmospheric pressure tank are all covered with a jacketed heating device.

[0011] In one embodiment, infrared detection systems are installed on the outer walls of the sealed pressure tank, the first atmospheric pressure tank, and the second atmospheric pressure tank.

[0012] In one embodiment, the infrared detection system includes an infrared temperature measurement module and a near-infrared spectroscopy detection module, with the detection ends of both the uppermost infrared temperature measurement module and the near-infrared spectroscopy detection module penetrating into the first atmospheric pressure tank.

[0013] In one embodiment, the uppermost openable isolation valve is installed via a flange between the hollow short spiral feeder and the feed inlet of the first atmospheric pressure tank.

[0014] A method of using an integrated device for preparing chitin micro / nanofibers from crustaceans, comprising the integrated device for preparing chitin micro / nanofibers from any one of claims 1-9, characterized in that the specific method of use is as follows: Step 1: Feeding and Zone Isolation: The crustacean raw materials are fed into the sealed pressure tank, the first atmospheric pressure tank and the second atmospheric pressure tank through the top feed port respectively. The feed port is closed and the three reaction zones are isolated into independent reaction spaces through the openable isolation valve. Step 2: Alkaline hydrothermal oxidation reaction: Turn on the jacket heating device to heat, turn on the mechanical crushing and stirring shaft to stir, and fill the sealed pressure tank with oxygen through the oxygen inlet and outlet ports until the pressure is 0.35-0.50 MPa. Monitor the pressure with a pressure gauge, and react at 108-118℃ for 80-110 minutes. After the reaction, release the pressure to atmospheric pressure through the oxygen inlet and outlet ports. Step 3: First-stage drainage and spray washing: Turn on the top circumferential coarse screen drainage component. After the waste liquid is filtered by the screen, it enters the annular collection chamber along the inner wall of the tank and is then discharged through the water outlet pipe. At the same time, turn on the top clean water sprayer for spray washing. Step 4: First-stage material conveying: Close the top circumferential coarse screen drain assembly and the clean water sprayer, open the top openable isolation valve, and start the top hollow short spiral feeder. Convey the material through the discharge port to the feed port of the first atmospheric pressure tank at a speed of 20-60 r / min. During conveying, open the top clean water sprayer to rinse the residual material. The rinsing water is discharged through the water outlet pipe. After all the material has entered, close the hollow short spiral feeder, the openable isolation valve, and the clean water sprayer. Step 5: Bleaching reaction: Turn on the jacket heating device to heat, turn on the low-speed rotating blade agitator to stir, and react for 20 to 30 minutes at 45 to 75°C. Step 6: Second-stage drainage and spray washing: After the reaction, turn off the jacket heating device and the low-speed rotating blade agitator, turn on the intermediate circumferential coarse screen drainage component, and the waste liquid enters the annular collection chamber along the inner wall of the tank after being filtered by the screen, and then is discharged through the water outlet pipe. At the same time, turn on the intermediate clean water sprayer for spray washing. Step 7: Second-stage material conveying: Close the intermediate circumferential coarse screen drain assembly and the clean water sprayer, open the intermediate openable isolation valve, start the intermediate hollow short spiral feeder, and convey the material through the discharge port to the feed port of the second atmospheric pressure tank at a speed of 20-60 r / min. During conveying, open the intermediate clean water sprayer to rinse the residual material. The rinsing water is discharged through the water outlet pipe. After all the material has entered, close the hollow short spiral feeder, the openable isolation valve and the clean water sprayer. Step 8: Pickling density sorting reaction: Add acid solution into the second atmospheric pressure tank through the feed port, start the external drive mechanism to drive the central shaft to rotate, drive the elliptical flipping plate to rotate relative to the umbrella-shaped guide plate, form a low-shear internal circulation flow, and react for 3 to 5 hours at room temperature to 40°C. Step Nine: Third-stage drainage, spray washing and discharge: After the reaction, turn off the external drive mechanism, turn on the bottom circumferential coarse screen drainage component, the waste liquid is filtered through the screen and enters the annular collection chamber along the inner wall of the tank, and then discharged through the water outlet pipe. Turn on the bottom clean water sprayer for spray washing, turn off the circumferential coarse screen drainage component and the clean water sprayer, start the bottom hollow short spiral feeder, and continuously discharge the chitin fiber slurry through the discharge port.

[0015] 1. The above-mentioned integrated equipment and method for preparing chitin micro / nanofibers of crustaceans involves setting up an alkaline hydrothermal oxidation reaction zone, a bleaching reaction zone, and an acid washing density sorting reaction zone sequentially on the equipment frame along the material conveying direction and connecting them through a connector device. This allows the pretreatment process to be completed continuously within the same equipment, avoiding process interruptions and material losses caused by repeated filtration, washing, transfer, and refeeding of materials between processes, thereby improving the efficiency of large-scale preparation of chitin micro / nanofibers of crustaceans. 2. A circumferential coarse screen drainage assembly and a clean water sprayer are installed in the alkaline hydrothermal oxidation reaction zone, the bleaching reaction zone, and the pickling density sorting reaction zone. After the reaction, waste liquid can be separated and discharged and clean water spray washing can be completed inside the reaction zone. The screen aperture of the circumferential coarse screen drainage assembly decreases along the material conveying direction to adapt to the gradual decrease in material particle size, realizing gradient drainage and online spray washing. Attached Figure Description

[0016] To more clearly illustrate the technical solutions in this invention or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are some embodiments of this invention. For those skilled in the art, other drawings can be obtained from these drawings without creative effort.

[0017] Figure 1 This is a schematic diagram of the overall structure of the present invention; Figure 2 This is a cross-sectional schematic diagram of the alkaline hydrothermal oxidation reaction zone in this invention; Figure 3 This is a cross-sectional schematic diagram of the bleaching reaction zone in this invention; Figure 4 This is a cross-sectional schematic diagram of the acid washing density sorting reaction zone in this invention; Figure 5 This is a schematic diagram of the connector device in this invention; Figure 6 This is a schematic diagram showing the connection between the washing water pipe and the clean water sprayer in this invention; Figure 7 This is a schematic diagram of the infrared detection system in this invention.

[0018] Figure label: 100. Equipment frame; 200. Alkaline hydrothermal oxidation reaction zone; 210. Sealed pressure tank; 220. Mechanical crushing and stirring shaft; 230. Oxygen inlet and outlet; 240. Pressure gauge; 300. Bleaching reaction zone; 310. First atmospheric pressure tank; 320. Low-speed rotating blade agitator; 400. Acid washing density sorting reaction zone; 410. Second atmospheric pressure tank; 420. Umbrella-shaped guide plate; 430. Central shaft; 440. Elliptical tilting plate; 450. External drive motor Structure; 500, Inlet; 600, Outlet pipe; 700, Outlet; 800, Connector; 810, Hollow short spiral feeder; 820, Openable isolation valve; 900, Circumferential coarse screen drainage assembly; 910, Screen; 920, Annular liquid collection chamber; 1000, Washing water pipe; 1100, Clean water sprayer; 1200, Jacketed heating device; 1300, Infrared detection system; 1310, Infrared temperature measurement module; 1320, Near-infrared spectral detection module. Detailed Implementation

[0019] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, 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.

[0020] It should be noted that when a component is referred to as being "fixed to" or "set on" another component, it can be directly on the other component or there may be an intermediate component. When a component is considered to be "connected to" another component, it can be directly connected to the other component or there may be an intermediate component present. The terms "vertical," "horizontal," "upper," "lower," "left," "right," and similar expressions used in this specification are for illustrative purposes only and do not represent the only possible implementation.

[0021] Furthermore, the terms "first" and "second" are used for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one of that feature. In the description of this invention, "a plurality of" means at least two, such as two, three, etc., unless otherwise explicitly specified.

[0022] In this invention, unless otherwise explicitly specified and limited, "above" or "below" the second feature can mean that the first feature is in direct contact with the second feature, or that the first feature and the second feature are in indirect contact through an intermediate medium. Furthermore, "above," "over," and "on top" the second feature can mean that the first feature is directly above or diagonally above the second feature, or simply indicates that the first feature is at a higher horizontal level than the second feature. "Below," "below," and "under" the second feature can mean that the first feature is directly below or diagonally below the second feature, or simply indicates that the first feature is at a lower horizontal level than the second feature.

[0023] Unless otherwise defined, all technical and scientific terms used in this specification have the same meaning as commonly understood by one of ordinary skill in the art to which this invention pertains. The terminology used in this specification is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. The term "and / or" as used in this specification includes any and all combinations of one or more of the associated listed items.

[0024] The following is combined with Figures 1-7 This invention describes an integrated apparatus and method for preparing chitin micro / nanofibers from crustaceans.

[0025] In one embodiment, an integrated apparatus for preparing chitin micro / nanofibers from crustaceans includes: Equipment rack 100; The alkaline hydrothermal oxidation reaction zone 200, bleaching reaction zone 300, and pickling density sorting reaction zone 400 are installed on the equipment frame 100, and are arranged sequentially along the material conveying direction. The alkaline hydrothermal oxidation reaction zone 200 includes a sealed pressure tank 210 and a mechanical crushing and stirring shaft 220. The sealed pressure tank 210 is a titanium alloy-lined pressure-bearing structure. The mechanical crushing and stirring shaft 220 is installed in the center of the sealed pressure tank 210. The sealed pressure tank 210 creates a high temperature and high pressure environment. Combined with the strong crushing and stirring of the mechanical crushing and stirring shaft 220, the oxygen-alkali reaction and mechanical dissociation are carried out in a coordinated manner, which can improve the protein removal efficiency. The bleaching reaction zone 300 includes a first atmospheric pressure tank 310 and a low-speed rotating blade agitator 320. The inner lining of the first atmospheric pressure tank 310 is polypropylene or polytetrafluoroethylene. The low-speed rotating blade agitator 320 is installed in the center of the inside of the first atmospheric pressure tank 310. The service life of the tank is extended by the anti-corrosion lining material. The low-speed rotating blade agitator 320 achieves gentle and uniform mixing of bleaching liquid with low shear force, which reduces fiber damage while ensuring bleaching effect. The pickling density sorting reaction zone 400 includes a second atmospheric pressure tank 410, an umbrella-shaped guide plate 420, a central shaft 430, an elliptical tilting plate 440, and an external drive mechanism 450. The lining of the second atmospheric pressure tank 410 is polypropylene or polytetrafluoroethylene. The umbrella-shaped guide plate 420 is fixed inside the second atmospheric pressure tank 410. The central shaft 430 passes through the second atmospheric pressure tank 410, with one end extending out of the tank. The elliptical tilting plate 440 is mounted on the arc surface of the central shaft 430. The external drive mechanism 450 is fixed. The umbrella-shaped guide plate 420 is used to guide the acid solution to diffuse evenly in the radial direction through one end of the second atmospheric pressure tank 410 through the central axis 430. The elliptical flip plate 440 is used to drive the fiber slurry to circulate in an overall tumbling manner. The umbrella-shaped guide plate 420 and the elliptical flip plate 440 cooperate to form a low-shear internal circulation slurry flow field. The umbrella-shaped guide plate 420 guides the acid solution to diffuse evenly, and the elliptical flip plate 440 drives the fiber slurry to circulate in an overall tumbling manner. The low-shear internal circulation flow field replaces the local high-speed shear stirring, reduces the mechanical damage to long fibers, and improves the uniformity of decalcification. The top of each of the sealed pressure tank 210, the first atmospheric pressure tank 310, and the second atmospheric pressure tank 410 is provided with a feed inlet 500. The bottom of each of the sealed pressure tank 210, the first atmospheric pressure tank 310, and the second atmospheric pressure tank 410 is provided with a water outlet 600. The bottom of each of the sealed pressure tank 210, the first atmospheric pressure tank 310, and the second atmospheric pressure tank 410 is provided with a discharge outlet 700. Through the feed inlet 500, the water outlet 600, and the discharge outlet 700 respectively provided at the top, bottom, and sides of each tank, the feeding, draining, and discharging operations in each reaction zone are realized in a pipeline manner, reducing the exposure of materials between processes and manual transfer. Three circumferential coarse screening and drainage components 900 are respectively installed on the inner circumferential walls of the sealed pressure tank 210, the first atmospheric pressure tank 310, and the second atmospheric pressure tank 410. By setting the drainage components on the inner circumferential walls of the tanks, the waste liquid is filtered by the screen and then enters the annular collection chamber along the inner wall of the tank before being discharged, thereby achieving solid-liquid separation and continuous drainage, while avoiding material blockage during the drainage process. There are three connector devices 800. The uppermost connector device 800 is installed between the discharge port 700 of the sealed pressure tank 210 and the inlet 500 of the first atmospheric pressure tank 310. The middle connector device 800 is installed between the discharge port 700 of the first atmospheric pressure tank 310 and the inlet 500 of the second atmospheric pressure tank 410. The lowermost connector device 800 is installed at the discharge port 700 of the second atmospheric pressure tank 410. The continuous material transport between the reaction zones is achieved through the three connector devices 800, so that the preparation process can be operated continuously. The uppermost connector device 800 includes a hollow short spiral feeder 810 and an openable isolation valve 820. The spiral shaft of the hollow short spiral feeder 810 is hollow. The inlet of the hollow short spiral feeder 810 is connected to the outlet 700 of the sealed pressure tank 210, and the outlet of the hollow short spiral feeder 810 is connected to the inlet 500 of the first atmospheric pressure tank 310. The openable isolation valve 820 is installed in the outlet pipeline of the hollow short spiral feeder 810. The middle connector device 800 is connected to the uppermost... The joint device 800 described above has the same structure. The joint device 800 described at the bottom only includes a hollow short spiral feeder 810. The inlet of the hollow short spiral feeder 810 of the joint device 800 is connected to the outlet 700 of the second atmospheric pressure tank 410. The hollow short spiral feeder 810 realizes the stable conveying of materials and reduces the pulling damage to fibers. The openable isolation valve 820 switches the connection or isolation state of each reaction zone as needed, which not only ensures the establishment of independent reaction space, but also realizes the connection between processes. The uppermost circumferential coarse screening and drainage assembly 900 includes a screen 910, which is fixedly connected to the inner wall of the sealed pressure tank 210. The bottom of the screen 910 is provided with an annular liquid collection chamber 920 that communicates with the discharge port 700. The screen 910 of the circumferential coarse screening and drainage assembly 900 installed in the first atmospheric pressure tank 310 is connected to the water outlet pipe 600 of the first atmospheric pressure tank 310 through the annular liquid collection chamber 920. The screen 910 of the circumferential coarse screening and drainage assembly 900 installed in the second atmospheric pressure tank 410 is connected to the water outlet pipe 600 of the second atmospheric pressure tank 410 through the annular liquid collection chamber 920. The screen 910 installed in the sealed pressure tank 210 has a mesh size of 20-40 mesh, the screen 910 installed in the first atmospheric pressure tank 310 has a mesh size of 60-100 mesh, and the screen 910 installed in the second atmospheric pressure tank 410 has a mesh size of 120-200 mesh. The mesh size of the screens in each reaction zone decreases sequentially along the material conveying direction to adapt to the gradual decrease in material particle size and to achieve gradient drainage. This can balance the drainage efficiency and fiber retention rate at each stage and reduce the risk of clogging. The surface of the alkaline hydrothermal oxidation reaction zone 200 is provided with an oxygen inlet / outlet port 230 and a pressure gauge 240. Both the oxygen inlet / outlet port 230 and the pressure gauge 240 are connected to the inside of the sealed pressure tank 210. The pressure gauge 240 monitors the pressure inside the tank in real time and controls the reaction pressure in conjunction with the oxygen inlet / outlet port 230 to ensure the safety of the reaction process. The equipment frame 100 is equipped with a washing water pipe 1000. The top inner side of the sealed pressure tank 210, the first atmospheric pressure tank 310 and the second atmospheric pressure tank 410 are all equipped with a clean water sprayer 1100. The clean water sprayer 1100 is connected to the washing water pipe 1000 through a three-way solenoid valve, so that online spray washing can be carried out directly after the reaction is completed in each reaction zone, without the need to transfer the material to an external washing device. The outer walls of the sealed pressure tank 210, the first atmospheric pressure tank 310, and the second atmospheric pressure tank 410 are all wrapped with jacketed heating devices 1200, which can make each tank heat evenly through outer wall wrapping heating, and achieve temperature control of each reaction zone in conjunction with temperature feedback. Infrared detection systems 1300 are installed on the outer walls of the sealed pressure tank 210, the first atmospheric pressure tank 310, and the second atmospheric pressure tank 410. The infrared detection system 1300 includes a temperature measurement module and a near-infrared spectroscopy detection module. The infrared detection system 1300 is connected to each jacket heating device 1200 for real-time monitoring of the material temperature in each reaction zone and temperature control in conjunction with the jacket heating device, as well as online detection of material composition changes, which can improve the accuracy of process control and the consistency of the reaction. The infrared detection system 1300 includes an infrared temperature measurement module 1310 and a near-infrared spectroscopy detection module 1320. The detection ends of the uppermost infrared temperature measurement module 1310 and near-infrared spectroscopy detection module 1320 are both inserted into the first atmospheric pressure tank 310, which can simultaneously realize real-time monitoring of reaction temperature and online detection of material components. The uppermost openable isolation valve 820 is installed between the hollow short spiral feeder 810 and the feed inlet 500 of the first atmospheric pressure tank 310 via a flange; The mechanical crushing and stirring shaft 220, the circumferential coarse screen drainage assembly 900, the low-speed rotating blade stirring paddle 320, the umbrella-shaped guide plate 420, the elliptical tilting plate 440, and the hollow short spiral feeder 810 are all polytetrafluoroethylene-coated stainless steel anti-corrosion structures. The stainless steel core material can be used to ensure structural strength, and the polytetrafluoroethylene coating layer can isolate the corrosion of the metal by acid and alkali media, thus extending the service life of the equipment.

[0026] like Figure 1-7As shown, a method of using an integrated device for preparing chitin micro / nanofibers from crustaceans, comprising the integrated device for preparing chitin micro / nanofibers from any one of claims 1-9, is characterized in that the specific method of use is as follows: Step 1: Feeding and Zone Isolation: The crustacean raw materials are added to the sealed pressure tank 210 of the alkaline hydrothermal oxidation reaction zone 200 through the feed port 500 at the top of the equipment frame 100. At this time, no raw materials are added to the first atmospheric pressure tank 310 of the bleaching reaction zone 300 and the second atmospheric pressure tank 410 of the pickling density sorting reaction zone 400. The feed port 500 is closed, and the three reaction zones are isolated into independent reaction spaces through the openable isolation valve 820. Step 2: Alkaline hydrothermal oxidation reaction: The jacketed heating device 1200 of the alkaline hydrothermal oxidation reaction zone 200 is turned on for heating, and the mechanical crushing and stirring shaft 220 is turned on for stirring. Oxygen is introduced into the sealed pressure tank 210 through the oxygen inlet and outlet port 230 to a pressure of 0.35-0.50 MPa. The internal pressure of the sealed pressure tank 210 is monitored by the pressure gauge 240. The reaction is carried out at 108-118℃ for 80-110 minutes, so that the crushing and stirring of the mechanical crushing and stirring shaft 220 and the oxygen-alkali reaction are carried out in a coordinated manner. After the reaction is completed, the internal pressure of the sealed pressure tank 210 is released to atmospheric pressure through the oxygen inlet and outlet port 230. This alkaline hydrothermal oxidation reaction corresponds to the particle crushing and oxidative depolymerization stage of chitin raw materials, so that the macromolecular chains are degraded while the fiber skeleton is preserved, laying the foundation for subsequent low-damage treatment. Step 3: First-stage drainage and spray washing: Turn on the circumferential coarse screen drainage assembly 900 installed on the inner wall of the sealed pressure tank 210. The reaction waste liquid in the sealed pressure tank 210 is filtered by the screen 910 and enters the annular collection chamber 920 along the inner wall of the tank. Then it is discharged through the water outlet pipe 600 on the lower side of the sealed pressure tank 210. At the same time, turn on the clean water sprayer 1100 installed on the inner side of the top of the sealed pressure tank 210. Clean water is sprayed into the sealed pressure tank 210 through the washing water pipe 1000 for online washing. The washing waste liquid is discharged through the water outlet pipe 600. Step 4: First-stage material conveying: Close the circumferential coarse screen drainage assembly 900 installed on the inner wall of the sealed pressure tank 210, close the clean water sprayer 1100, open the openable isolation valve 820 of the uppermost connector device 800, and start the hollow short spiral feeder 810 of the uppermost connector device 800 to convey the material in the sealed pressure tank 210 through the discharge port 700 at the bottom of the sealed pressure tank 210 at a speed of 20-60 r / min. The material is fed into the inlet 500 at the top of the first atmospheric pressure tank 310. During the conveying process, the clean water sprayer 1100 is turned on to spray clean water into the sealed pressure tank 210, flushing the residual material into the first atmospheric pressure tank 310. The flushing water is discharged through the outlet pipe 600 at the bottom side of the sealed pressure tank 210. After all the material has entered the first atmospheric pressure tank 310, the hollow short spiral discharger 810 is turned off, the openable isolation valve 820 is turned off, and the clean water sprayer 1100 is turned off. Step 5: Bleaching reaction: Turn on the jacket heating device 1200 of the bleaching reaction zone 300 for heating, turn on the low-speed rotating blade agitator 320 for stirring, and react for 20 to 30 minutes at 45 to 75°C to carry out the bleaching reaction; this bleaching reaction corresponds to the fiber decolorization and purification stage, removes pigments and impurities, improves fiber whiteness, and avoids excessive fiber degradation under mild conditions. Step Six: Second-stage drainage and spray washing: After the reaction is completed, the jacket heating device 1200 and the low-speed rotating blade agitator 320 are turned off. The circumferential coarse screen drainage assembly 900 installed on the inner wall of the first atmospheric pressure tank 310 is turned on. The reaction waste liquid in the first atmospheric pressure tank 310 is filtered by the screen 910 and enters the annular collection chamber 920 along the inner wall of the tank. Then it is discharged through the water outlet pipe 600 on the lower side of the first atmospheric pressure tank 310. At the same time, the clean water sprayer 1100 installed on the inner side of the top of the first atmospheric pressure tank 310 is turned on. Clean water is sprayed into the first atmospheric pressure tank 310 through the washing water pipe 1000 for online washing. The washing waste liquid is discharged through the water outlet pipe 600. Step 7: Second-stage material conveying: Close the circumferential coarse screen drainage assembly 900 installed on the inner wall of the first atmospheric pressure tank 310, close the clean water sprayer 1100, open the openable isolation valve 820 of the intermediate joint device 800, and start the hollow short spiral feeder 810 of the intermediate joint device 800 to convey the material in the first atmospheric pressure tank 310 through the discharge port 700 at the bottom of the first atmospheric pressure tank 310 at a speed of 20-60 r / min. The feed inlet 500 at the top of the second atmospheric pressure tank 410 is opened during the conveying process. The clean water sprayer 1100 is turned on to spray clean water into the first atmospheric pressure tank 310, and the residual material is flushed into the second atmospheric pressure tank 410. The flushing water is discharged through the water outlet pipe 600 at the lower side of the first atmospheric pressure tank 310. After all the material has entered the second atmospheric pressure tank 410, the hollow short spiral discharger 810 is closed, the openable isolation valve 820 is closed, and the clean water sprayer 1100 is turned off. Step 8: Acid washing and density sorting reaction: Acid solution is added to the second atmospheric pressure tank 410 through the feed inlet 500. The feed inlet 500 is then closed, and the external drive mechanism 450 is activated. The external drive mechanism 450 drives the central shaft 430 to rotate, which in turn drives the elliptical tilting plate 440 to rotate relative to the umbrella-shaped guide plate 420. This causes the fiber slurry in the second atmospheric pressure tank 410 to form a low-shear internal circulation flow. The acid solution is guided by the umbrella-shaped guide plate 420 to diffuse evenly in the radial direction. The elliptical tilting plate 440 drives the fiber slurry to rotate and circulate as a whole. The reaction is carried out at room temperature to 40°C for 3-5 hours to perform acid washing and decalcification reaction. This acid washing and density sorting reaction corresponds to the acid washing and decalcification and density sorting stages, effectively removing calcium and achieving fiber grading. The entire three-stage treatment system follows the deconstruction law of raw materials from particles to fiber networks, achieving gradual and gentle treatment and avoiding excessive damage to the fiber structure. Step Nine: Third-stage drainage, spray washing, and discharge: After the reaction is completed, the external drive mechanism 450 is turned off, and the circumferential coarse screen drainage assembly 900 installed on the inner wall of the second atmospheric pressure tank 410 is turned on. The reaction waste liquid in the second atmospheric pressure tank 410 is filtered by the screen 910 and enters the annular collection chamber 920 along the inner wall of the tank, and then discharged through the water outlet pipe 600 on the lower side of the second atmospheric pressure tank 410. At the same time, the system installed on the inner side of the top of the second atmospheric pressure tank 410 is turned on. The clean water sprayer 1100 sprays clean water into the second atmospheric pressure tank 410 through the washing water pipe 1000 for online washing. The washing waste liquid is discharged through the outlet pipe 600. The circumferential coarse screen drain assembly 900 is closed, the clean water sprayer 1100 is closed, and the hollow short spiral discharger 810 of the bottom connector device 800 is started to continuously discharge the chitin fiber slurry in the second atmospheric pressure tank 410 through the discharge port 700 at the bottom of the second atmospheric pressure tank 410.

[0027] It should be noted that the actual model number of the variable frequency motor 220 is Wuhan Weite's YZLPWT-160L-8 water-cooled, high-temperature resistant, variable frequency speed-regulating, corrosion-resistant special motor; the actual model number of the variable frequency motor 320 is Wuhan Weite's YZLPWT series water-cooled, high-temperature resistant, variable frequency speed-regulating, corrosion-resistant special motor; the actual model number of the external drive mechanism 450 is Wuhan Weite's YGLPWT series water-cooled, high-temperature resistant, variable frequency speed-regulating roller conveyor motor; and the actual model number of the screw conveyor drive motor 810 is Wuhan Weite's YZL... PWT series water-cooled high-temperature resistant variable frequency speed control corrosion-resistant special motors; the actual model of the frequency converter is ABB's ACS580-01-018A-4 general-purpose frequency converter; the actual model of the openable isolation valve 820 is Masonland's D671F46 pneumatic fluoropolymer-lined butterfly valve; the actual model of the pressure gauge 240 is Xi'an Instrument Factory's YTH-100 corrosion-resistant and high-temperature resistant pressure gauge; the actual model of the infrared temperature measurement module 1310 is Raytek's CI-B type Compact CI series infrared thermometer; the actual model of the near-infrared spectroscopy detection module 1320 is Crystalma's JGM NIR type probe-type online near-infrared spectrometer; the actual model of the PLC controller is Siemens' S7-1200CPU 1214C programmable controller; the actual model of the high-temperature resistant sealing ring is FZ Fuzhao's FKM70 type fluororubber O-ring.

[0028] The technical features of the above embodiments can be combined in any way. For the sake of brevity, not all possible combinations of the technical features in the above embodiments are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.

[0029] The embodiments described above are merely illustrative of several implementations of the present invention, and while the descriptions are specific and detailed, they should not be construed as limiting the scope of the invention. It should be noted that those skilled in the art can make various modifications and improvements without departing from the concept of the present invention, and these modifications and improvements all fall within the scope of protection of the present invention. Therefore, the scope of protection of the present invention should be determined by the appended claims.

Claims

1. An integrated device for preparing chitin micro / nanofibers from crustaceans, characterized in that, include: Equipment rack (100); The alkaline hydrothermal oxidation reaction zone (200), bleaching reaction zone (300) and pickling density sorting reaction zone (400) are installed on the equipment frame (100), and the alkaline hydrothermal oxidation reaction zone (200), bleaching reaction zone (300) and pickling density sorting reaction zone (400) are arranged sequentially along the material conveying direction; The alkaline hydrothermal oxidation reaction zone (200) includes a sealed pressure tank (210) and a mechanical crushing and stirring shaft (220), wherein the mechanical crushing and stirring shaft (220) is installed in the center inside the sealed pressure tank (210); The bleaching reaction zone (300) includes a first atmospheric pressure tank (310) and a low-speed rotating blade agitator (320), wherein the low-speed rotating blade agitator (320) is installed in the center inside the first atmospheric pressure tank (310); The pickling density sorting reaction zone (400) includes a second atmospheric pressure tank (410), an umbrella-shaped guide plate (420), a central shaft (430), an elliptical flipping plate (440), and an external drive mechanism (450). The umbrella-shaped guide plate (420) is fixed inside the second atmospheric pressure tank (410). The central shaft (430) passes through the second atmospheric pressure tank (410) and one end of the central shaft (430) extends out of the second atmospheric pressure tank (410). The elliptical flipping plate (440) is installed on the arc surface of the central shaft (430). The external drive mechanism (450) is fixed to one end of the central shaft (430) that extends out of the second atmospheric pressure tank (410). The top of the sealed pressure tank (210), the first atmospheric pressure tank (310), and the second atmospheric pressure tank (410) are all provided with inlets (500), the bottom of the sealed pressure tank (210), the first atmospheric pressure tank (310), and the second atmospheric pressure tank (410) are all provided with outlet pipes (600), and the bottom of the sealed pressure tank (210), the first atmospheric pressure tank (310), and the second atmospheric pressure tank (410) are all provided with outlets (700). Three circumferential coarse screening drainage components (900) are respectively installed on the inner circumferential side of the sealed pressure tank (210), the inner circumferential side of the first atmospheric pressure tank (310), and the inner circumferential side of the second atmospheric pressure tank (410); The quantity is three connector devices (800). The uppermost connector device (800) is installed between the outlet (700) of the sealed pressure tank (210) and the inlet (500) of the first atmospheric pressure tank (310). The middle connector device (800) is installed between the outlet (700) of the first atmospheric pressure tank (310) and the inlet (500) of the second atmospheric pressure tank (410). The lowermost connector device (800) is installed at the outlet (700) of the second atmospheric pressure tank (410). The uppermost connector device (800) includes a hollow short spiral feeder (810) and an openable isolation valve (820). The inlet of the hollow short spiral feeder (810) is connected to the outlet (700) of the sealed pressure tank (210), and the outlet of the hollow short spiral feeder (810) is connected to the inlet (500) of the first atmospheric pressure tank (310). The openable isolation valve (820) is installed on the outlet pipeline of the hollow short spiral feeder (810).

2. The device according to claim 1, characterized in that, The uppermost circumferential coarse screening and drainage assembly (900) includes a screen (910), which is fixedly connected to the inner wall of the sealed pressure tank (210). The bottom of the screen (910) is provided with an annular liquid collection chamber (920) that communicates with the discharge port (700).

3. The device according to claim 2, characterized in that, The screen (910) installed in the sealed pressure tank (210) has a mesh size of 20 to 40 mesh, the screen (910) installed in the first atmospheric pressure tank (310) has a mesh size of 60 to 100 mesh, and the screen (910) installed in the second atmospheric pressure tank (410) has a mesh size of 120 to 200 mesh.

4. The device according to claim 1, characterized in that, The surface of the alkaline hydrothermal oxidation reaction zone (200) is provided with an oxygen inlet / outlet port (230) and a pressure gauge (240).

5. The device according to claim 1, characterized in that, The equipment frame (100) is equipped with a washing water pipe (1000). The top inner side of the sealed pressure tank (210), the first atmospheric pressure tank (310) and the second atmospheric pressure tank (410) are all equipped with a clean water sprayer (1100). The clean water sprayer (1100) is connected to the washing water pipe (1000) through a three-way solenoid valve.

6. The device according to claim 1, characterized in that, The outer walls of the sealed pressure tank (210), the first atmospheric pressure tank (310), and the second atmospheric pressure tank (410) are all covered with jacketed heating devices (1200).

7. The device according to claim 1, characterized in that, Infrared detection systems (1300) are installed on the outer walls of the sealed pressure tank (210), the first atmospheric pressure tank (310), and the second atmospheric pressure tank (410).

8. The device according to claim 7, characterized in that, The infrared detection system (1300) includes an infrared temperature measurement module (1310) and a near-infrared spectral detection module (1320). The detection ends of the uppermost infrared temperature measurement module (1310) and near-infrared spectral detection module (1320) are inserted into the first atmospheric pressure tank (310).

9. The device according to claim 1, characterized in that, The uppermost openable isolation valve (820) is installed via a flange between the hollow short spiral feeder (810) and the feed inlet (500) of the first atmospheric pressure tank (310).

10. A method of using an integrated apparatus for preparing chitin micro / nanofibers of crustaceans, comprising the integrated apparatus for preparing chitin micro / nanofibers of crustaceans as described in any one of claims 1-9, characterized in that, The specific usage method is as follows: Step 1: Feeding and Zone Isolation: The crustacean raw materials are fed into the sealed pressure tank (210), the first atmospheric pressure tank (310) and the second atmospheric pressure tank (410) through the top feed port (500) respectively. The feed port (500) is closed, and the three reaction zones are isolated into independent reaction spaces through the openable isolation valve (820). Step 2: Alkaline hydrothermal oxidation reaction: Turn on the jacket heating device (1200) to heat, turn on the mechanical crushing and stirring shaft (220) to stir, and fill the sealed pressure tank (210) with oxygen to 0.35-0.50 MPa through the oxygen inlet and outlet port (230). Monitor the pressure through the pressure gauge (240), and react at 108-118℃ for 80-110 min. After the reaction, release the pressure to atmospheric pressure through the oxygen inlet and outlet port (230). Step 3: First-stage drainage and spray washing: Turn on the top circumferential coarse screen drainage component (900). After the waste liquid is filtered through the screen (910), it enters the annular collection chamber (920) along the inner wall of the tank and is then discharged through the water outlet pipe (600). At the same time, turn on the top clean water sprayer (1100) for spray washing. Step 4: First-stage material conveying: Close the top circumferential coarse screen drain assembly (900) and the clean water sprayer (1100), open the top openable isolation valve (820), start the top hollow short spiral feeder (810), and convey the material through the discharge port (700) to the feed port (500) of the first atmospheric pressure tank (310) at a speed of 20-60 r / min. During conveying, open the top clean water sprayer (1100) to rinse the residual material. The rinsing water is discharged through the water outlet pipe (600). After all the material has entered, close the hollow short spiral feeder (810), the openable isolation valve (820), and the clean water sprayer (1100). Step 5: Bleaching reaction: Turn on the jacket heating device (1200) to heat, turn on the low-speed rotating blade agitator (320) to stir, and react at 45-75℃ for 20-30 minutes; Step 6: Second-stage drainage and spray washing: After the reaction, the jacket heating device (1200) and the low-speed rotating blade agitator (320) are turned off, and the intermediate circumferential coarse screen drainage assembly (900) is turned on. The waste liquid is filtered through the screen (910) and enters the annular collection chamber (920) along the inner wall of the tank, and then is discharged through the water outlet pipe (600). At the same time, the intermediate clean water sprayer (1100) is turned on for spray washing. Step 7: Second-stage material conveying: Close the intermediate circumferential coarse screen drain assembly (900) and the clean water sprayer (1100), open the intermediate openable isolation valve (820), start the intermediate hollow short spiral feeder (810), and convey the material through the discharge port (700) to the feed port (500) of the second atmospheric pressure tank (410) at a speed of 20-60 r / min. During conveying, open the intermediate clean water sprayer (1100) to rinse the residual material. The rinsing water is discharged through the water outlet pipe (600). After all the material has entered, close the hollow short spiral feeder (810), the openable isolation valve (820), and the clean water sprayer (1100). Step 8: Pickling density sorting reaction: Add acid solution to the second atmospheric pressure tank (410) through the feed port (500), start the external drive mechanism (450) to drive the central shaft (430) to rotate, drive the elliptical flip plate (440) to rotate relative to the umbrella-shaped guide plate (420) to form a low-shear internal circulation flow, and react at room temperature to 40°C for 3 to 5 hours; Step Nine: Third-stage drainage, spray washing and discharge: After the reaction, the external drive mechanism (450) is turned off, the bottom circumferential coarse screen drainage component (900) is turned on, the waste liquid is filtered through the screen (910) and enters the annular collection chamber (920) along the inner wall of the tank, and then discharged through the water outlet pipe (600). The bottom clear water sprayer (1100) is turned on for spray washing, the circumferential coarse screen drainage component (900) and the clear water sprayer (1100) are turned off, and the bottom hollow short spiral feeder (810) is started to continuously discharge the chitin fiber slurry through the discharge port (700).

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