Fungus-derived chitosan and glucan mixed wet spinning method

Abstract

The invention relates to the technical field of wet spinning, in particular to a fungus-sourced chitosan and glucan mixed wet spinning method which comprises the following steps: sequentially performing impurity removal and defoaming on a formed raw material solution, and extruding the raw material solution into a coagulating bath through a spinning nozzle to perform fiber shaping so as to output a pre-finished product fiber; obtaining a plurality of extrusion fracture positions in the pre-finished product fiber; determining the fracture frequency of the pre-finished product fiber according to the plurality of extrusion fracture positions and the length of the pre-finished product fiber; and determining an abnormal concentration distribution region type in the raw material solution based on the first dissolution abnormal region and the second dissolution abnormal region, determining an abnormal processing mode, and sequentially processing the chitosan powder and the glucan powder of the next batch according to the abnormal processing mode so as to output pre-finished product fibers of the next batch, sequentially washing and drying the pre-finished product fibers without fractures to output finished product mixed fibers; according to the invention, the efficiency of the chitosan and glucan mixed spinning process is improved.

Description

Technical Field

[0001] The invention relates to the technical field of wet spinning, in particular to a wet spinning method for a mixture of fungus-derived chitosan and glucan. Background Art

[0002] As natural polysaccharides, fungal chitosan and glucan have great application potential in medical dressings, tissue engineering scaffolds, biodegradable materials and other fields due to their excellent biocompatibility, degradability and bioactivity. Wet spinning technology is a common method for preparing polysaccharide fibers because of its gentle operation and minimal damage to the bioactivity of polysaccharides. However, the existing technology for wet spinning mixed chitosan and glucan provides a general analysis of the causes of pre-finished fiber breakage. There is a significant difference in the time distribution of fiber breakage caused by the high concentration area near the stirring paddle and the high concentration area in the dead corner of the cup wall, but the existing technology cannot distinguish them, making the adjustment measures poorly targeted. Therefore, for the wet spinning of mixed fungal chitosan and glucan, there is an urgent need for a technical solution that can accurately identify the type of concentration anomaly, dynamically adjust the stirring parameters, and improve the fiber quality and production efficiency through batch iterative optimization, so as to solve the problems of poor concentration control and insufficient adaptability in the existing technology and promote the practical application of fungal polysaccharide fibers in the biomedical field.

[0003] Chinese Patent Publication No. CN118461230A discloses a plant polysaccharide nanofiber membrane and its preparation method and application, comprising: plant polysaccharides, supramolecular solvents, water, and polyvinyl alcohol fibers. Polysaccharides themselves are not spinnable, and in particular, plant polysaccharides are difficult to attach to electrospinning. The present invention creatively solves the spinnability problem of plant polysaccharides, making it possible to use polysaccharides as nanomaterials and expanding the application of plant polysaccharides in cosmetics and biomedicine. Using electrospinning technology, the nanofiber membrane prepared has high porosity and high specific surface area, enabling more effective utilization of the efficacy of plant polysaccharides. The present invention not only opens up new avenues for the application of plant polysaccharides in nanotechnology and biomedicine, but also provides an important reference for enhancing the practical value of supramolecular solvents and electrospinning technology in related fields. It can be seen that the plant polysaccharide nanofiber membrane and its preparation method and application have the problem that when the raw material solution containing undissolved particles in areas prone to concentration differences during stirring is extruded from the spinneret, the ability to resist stress changes varies, resulting in breakage of some adjacent fiber segments. This, in turn, leads to stress concentration at the aggregation points of different fiber batches, which affects the flexibility of the fiber. Summary of the Invention

[0004] To this end, the present invention provides a wet spinning method for a mixture of fungal-derived chitosan and glucan, so as to overcome the problem in the prior art that, when the raw material solution containing undissolved particles is extruded from the spinneret due to changes in its ability to resist stress changes, some adjacent fiber segments may break, resulting in stress concentration at the aggregation points of fiber particles from different batches, affecting the flexibility of the fibers.

[0005] To achieve the above object, the present invention provides a wet spinning method for a mixture of fungus-derived chitosan and glucan, comprising: A raw material solution formed by mixing and stirring fungal chitosan powder and glucan powder and a base solution in a beaker is sequentially subjected to impurity removal, degassing, and extrusion through a spinneret into a coagulation bath for fiber shaping to output a pre-finished fiber; Obtaining a plurality of extrusion fracture locations in the pre-finished fiber; determining a breakage frequency of the pre-finished fiber based on the plurality of extrusion breakage locations and the length of the pre-finished fiber; If the breakage frequency of the pre-finished fiber is greater than the preset breakage frequency, then the corresponding extrusion breakage positions that meet the preset diameter difference condition are counted; determining a first abnormal dissolution region in the raw material solution based on the corresponding extrusion fracture position; Performing a stretching test on a corresponding pre-finished fiber segment having a diameter within a standard diameter range according to a preset stretching multiple to determine a second abnormal dissolution region in the raw material solution; determining the type of abnormal concentration distribution region in the raw material solution based on the first abnormal dissolution region and the second abnormal dissolution region; Determining an abnormal treatment method according to the type of the abnormal concentration distribution area, including adjusting the stirring height of the raw material solution and / or performing ultrasonic crushing on the stirring dead corner area; According to the abnormal treatment method, the chitosan powder and the glucan powder of the next batch are stirred, impurity-removed, deaerated, and extruded through a spinneret to output the next batch of pre-finished fibers; The next batch of pre-finished fibers without tensile breakage are sequentially surface washed and dried to output finished mixed fibers.

[0006] Furthermore, a first horizontal cylindrical area formed by the first corresponding maximum height intervals in all beakers corresponding to the extrusion fracture positions is determined as the first abnormal dissolution area.

[0007] Further, determining the second abnormal dissolution region in the raw material solution includes: Counting the pre-finished fiber segments within the standard diameter range that have experienced tensile fracture; A second horizontal cylindrical area formed by a second corresponding maximum height interval of the raw material solution in the beaker corresponding to the extrusion time interval corresponding to the pre-finished fiber segment within the standard diameter range is determined as the second abnormal dissolution area.

[0008] Furthermore, the abnormal concentration distribution area type in the raw material solution is determined based on the overlap ratio of the overall abnormal area formed by the first dissolution abnormal area and the second dissolution abnormal area with the stirring range of the stirring paddle and the overlap ratio of the stirring dead angle area.

[0009] Furthermore, if the ratio of the overlapping area between the overall abnormal area and the stirring range of the stirring paddle is greater than a first preset overlapping area ratio, and the ratio of the overlapping area between the overall abnormal area and the stirring dead angle area is greater than a second preset overlapping area ratio, the abnormal concentration distribution area type is determined to be a double abnormal area type; If the overlap ratio of the overall abnormal region and the stirring range of the stirring paddle is greater than the first preset overlap ratio, and the overlap ratio of the overall abnormal region and the stirring dead angle region is less than or equal to the second preset overlap ratio, the abnormal concentration distribution region type is determined as the abnormal concentration region type around the stirring paddle; If the ratio of the overlapping area between the overall abnormal area and the stirring range of the stirring paddle is less than or equal to the first preset overlapping area ratio, and the ratio of the overlapping area between the overall abnormal area and the stirring dead angle area is greater than the second preset overlapping area ratio, the abnormal concentration distribution area type is determined to be the stirring dead angle area type.

[0010] Furthermore, if the ratio of the overlapping area between the overall abnormal area and the stirring range of the agitator is less than or equal to the first preset overlapping area ratio, and the ratio of the overlapping area between the overall abnormal area and the stirring dead angle area is less than or equal to the second preset overlapping area ratio, the abnormal concentration distribution area type is determined to be a conventional abnormal area type.

[0011] Furthermore, the ratio of the overlapping area between the overall abnormal area and the stirring range of the stirring paddle is the ratio of the volume occupied by the same area in the overall abnormal area and the stirring range of the stirring paddle to the volume occupied by the overall abnormal area; the ratio of the overlapping area between the overall abnormal area and the stirring dead angle area is the ratio of the volume occupied by the same area in the overall abnormal area and the stirring dead angle area to the volume occupied by the overall abnormal area.

[0012] Furthermore, the breakage frequency of the pre-finished fiber is a ratio of the total number of the plurality of extrusion breakage positions to the length of the pre-finished fiber.

[0013] Furthermore, if it is determined that the concentration is abnormal around the stirring blade, the stirring height of the raw material solution is adjusted upward; If it is determined to be a stirring dead angle area type, applying ultrasonic vibration to the stirring dead angle area; If it is determined to be a double abnormal area type, the stirring height of the raw material solution is increased and ultrasonic vibration is applied to the stirring dead angle area at the same time.

[0014] Furthermore, the preset diameter difference condition is that the diameter difference between the preceding section of pre-finished product fiber and the succeeding section of adjacent pre-finished product fiber at a single extrusion fracture position is greater than the preset diameter difference, wherein: The difference is the difference in diameter between a preceding section of pre-finished product fiber and a succeeding section of adjacent pre-finished product fiber at a single extrusion break position.

[0015] Compared with the prior art, the beneficial effect of the present invention lies in that the method of the present invention sets a determination process for the first dissolution abnormal area and the second dissolution abnormal area, and determines the abnormal concentration distribution in the raw material solution according to the first dissolution abnormal area and the second dissolution abnormal area. In the process of stirring the fungal chitosan powder and the glucan powder, due to the presence of undissolved solutes in the stirring process or the failure to filter out the solutes with small particle size during the impurity removal process, incompletely dissolved solute particles appear in the raw material solution, which causes some undissolved particles to interfere with or block the extrusion process near the spinneret during extrusion, resulting in differences in the diameters of fiber segments at different positions of the extruded pre-finished fiber. Therefore, different fiber segments have different abilities to resist stress changes, which causes the raw material solution with undissolved particles to become a to-be-formed solution and enter the spinneret for extrusion, which is prone to produce resistance due to resistance. The change in the ability to resist stress changes causes some adjacent fiber segments to break; when undissolved particles appear in the raw material solution, there are two areas where concentration differences are likely to occur. One is that the undissolved particles enter the rotation range of the stirring paddle due to the shear force generated near the stirring paddle, and after a long period of accumulation, they become a relatively stable high concentration area. The other is the stirring dead corner area of ​​the beaker. The stirring dead corner area is an area where the stirring range of the stirring paddle cannot effectively cover or the fluid disturbance intensity is significantly weakened. The stirring paddle is prone to not stirring in place during stirring, causing the undissolved particles to aggregate; by adjusting the stirring height and ultrasonically crushing the second abnormal dissolution area, the concentration aggregation in the beaker was changed, and the influence of undissolved particles on the quality and continuity of the fiber extruded from the spinneret was reduced, thereby improving the integrity of the fiber extrusion in the wet spinning process of the fungal chitosan and glucan mixture.

[0016] Furthermore, the present invention directly associates the extrusion fracture position with the first horizontal cylindrical area in the raw material solution, quantifies the first dissolution abnormality area through the spatial dimension, and determines the second horizontal cylindrical area formed by the extrusion time interval corresponding to the pre-finished fiber segment in the standard diameter range and the second corresponding maximum height interval of the raw material solution in the corresponding beaker as the second dissolution abnormality area, so that subsequent processing can accurately act on the target area, thereby reducing interference with the normal area, reducing energy consumption and raw material loss, and improving the targeting and efficiency of abnormal processing.

[0017] Furthermore, the present invention establishes a quantitative judgment logic for the type of abnormal concentration distribution area by calculating the overlap ratio between the overall abnormal area and the stirring range of the stirring paddle and the stirring dead corner area. The present invention clarifies the relationship between the abnormal area and the equipment disturbance characteristics through the overlap ratio, thereby improving the accuracy of process optimization.

[0018] Furthermore, the present invention distinguishes between paddle circumferential anomalies caused by insufficient disturbance of the agitator paddle, dead angle anomalies caused by sluggish flow, and dual anomalies of the coexistence of the two by setting a specific overlap ratio threshold, providing a clear direction for targeted treatment, improving the efficiency of process adjustment and the improvement of fiber quality. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] Figure 1 This is an overall flow chart of the wet spinning method of a mixture of fungal-derived chitosan and glucan according to an embodiment of the present invention; Figure 2 This is a flow chart of a method for determining the first abnormal dissolution area and the second abnormal dissolution area in a wet spinning method of a mixture of fungus-derived chitosan and glucan according to an embodiment of the present invention; Figure 3 This is a flow chart of a method for handling abnormalities in a wet spinning method of a mixture of fungal-derived chitosan and glucan according to an embodiment of the present invention; Figure 4 A schematic structural diagram of the overall abnormal region and the stirring range of the stirring blade in the wet spinning method of a mixture of fungal-derived chitosan and glucan according to an embodiment of the present invention, in which the abnormal concentration distribution region type is determined to be a double abnormal region type; Explanation of the reference numerals: 1- stirring paddle, 2- overall abnormal area, 3- stirring dead angle area, 4- stirring range. DETAILED DESCRIPTION

[0020] In order to make the objects and advantages of the present invention more clearly understood, the present invention is further described below in conjunction with embodiments; it should be understood that the specific embodiments described herein are merely used to explain the present invention and are not intended to limit the present invention.

[0021] The preferred embodiments of the present invention are described below with reference to the accompanying drawings. It should be understood by those skilled in the art that these embodiments are only used to explain the technical principles of the present invention and are not intended to limit the scope of protection of the present invention.

[0022] It should be noted that, in the description of the present invention, terms such as "up", "down", "left", "right", "inside", and "outside" indicating directions or positional relationships are based on the directions or positional relationships shown in the accompanying drawings. This is only for the convenience of description and does not indicate or imply that the device or element must have a specific orientation, be constructed and operated in a specific orientation. Therefore, it cannot be understood as a limitation on the present invention.

[0023] Furthermore, it should be noted that, in the description of the present invention, unless otherwise expressly specified or limited, the terms "mounted," "connected," and "connected" should be understood in a broad sense. For example, they may refer to fixed connections, detachable connections, or integral connections; mechanical connections or electrical connections; direct connections or indirect connections through an intermediate medium; and internal communication between two components. Those skilled in the art will understand the specific meanings of the above terms in the present invention based on specific circumstances.

[0024] See also Figure 1 、 Figure 2 、 Figure 3 as well as Figure 4 As shown, they are respectively an overall flow chart of the wet spinning method of a mixture of fungal-derived chitosan and glucan according to an embodiment of the present invention, a flow chart of a method for determining a first abnormal dissolution region and a second abnormal dissolution region, a flow chart of a method for handling abnormalities, and a structural schematic diagram of the overall abnormal region and the stirring range of the stirring paddle when the abnormal concentration distribution region type is determined to be a double abnormal region type; the wet spinning method of a mixture of fungal-derived chitosan and glucan according to an embodiment of the present invention comprises: Step S1, removing impurities and degassing the raw material solution formed by mixing and stirring fungal chitosan powder and glucan powder with a base solution in a beaker, and extruding the solution through a spinneret into a coagulation bath for fiber shaping to output a pre-finished fiber; Step S2, obtaining a plurality of extrusion fracture locations in the pre-finished fiber; Step S3, determining the breakage frequency of the pre-finished fiber according to the plurality of extrusion breakage positions and the length of the pre-finished fiber; Step S4, if the breakage frequency of the pre-finished fiber is greater than the preset breakage frequency, then counting the corresponding extrusion breakage positions that meet the preset diameter difference condition; Step S5, determining a first abnormal dissolution region in the raw material solution based on the corresponding extrusion fracture position; Step S6, performing a stretching test on the corresponding pre-finished fiber segment having a diameter within the standard diameter range according to a preset stretching multiple to determine a second abnormal dissolution area in the raw material solution; Step S7, determining the type of abnormal concentration distribution region in the raw material solution based on the first abnormal dissolution region and the second abnormal dissolution region; Step S8, determining an abnormality treatment method according to the type of the abnormal concentration distribution area, including adjusting the stirring height of the raw material solution and / or performing ultrasonic crushing on the stirring dead angle area; Step S9, stirring, removing impurities, degassing, and extruding the chitosan powder and the glucan powder of the next batch in accordance with the abnormality handling method to produce the next batch of pre-finished fibers; Step S10 , sequentially washing and drying the surfaces of the next batch of pre-finished fibers that do not break under tension, to output finished mixed fibers.

[0025] Specifically, the chitosan and glucan are both derived from fungal fermentation products or mycelium extraction.

[0026] Preferably, the chitosan is extracted from the fermented mycelium of filamentous fungi, and its molecular weight range is [100,000 Da, 500,000 Da]; the chitosan is extracted from the mycelium or fruiting body of filamentous fungi, and its molecular weight range is [300,000 Da, 1,000,000 Da].

[0027] Specifically, chitosan can impart good mechanical strength and antibacterial properties to the fiber, and dextran can enhance the biocompatibility and moisture retention of the fiber. A preferred embodiment of the mass ratio of the chitosan powder to the dextran powder is a mass ratio of the chitosan powder to the dextran powder of 2:1.

[0028] Specifically, fungal chitosan and glucan were ground by a planetary ball mill for 2 hours; the base solution was a 2% acetic acid aqueous solution; the impurity removal treatment used a 300-mesh filter to remove insoluble particles, wherein, Based on the solvent capacity of 2% acetic acid aqueous solution, the upper limit of the solubility of chitosan powder in 2% acetic acid aqueous solution is about 3%. In a preferred embodiment, 2.5 g of chitosan powder is added to every 100 mL of base solution. According to the mass ratio of chitosan powder to dextran powder of 2:1, the amount of dextran powder is 0.5 times that of chitosan powder, corresponding to the addition of 1.25 g of dextran powder to every 100 mL of base solution.

[0029] Specifically, the degassing treatment is a process of performing a vacuum degassing treatment on the raw material solution at a vacuum degree of -0.09 MPa for 20 minutes.

[0030] Specifically, the spinneret had an aperture of 0.3 mm and an extrusion speed of 0.5 mL / min; the coagulation bath was a mixed solution of 5% sodium hydroxide solution and 20% ethanol aqueous solution placed in a 500 mL polytetrafluoroethylene flat-bottom container, and the temperature of the coagulation bath was 25°C.

[0031] Those skilled in the art will understand that the operating principle and operating process of the planetary ball mill are conventional technical means well known to those skilled in the art, and therefore the operating principle and operating process of the planetary ball mill will not be described in detail here.

[0032] Specifically, under the conditions that the aperture of the spinneret is 0.3 mm and the extrusion speed is 0.5 mL / min, a preferred embodiment of the standard diameter range is [15 μm, 25 μm].

[0033] Specifically, the stretching test involves fixing the pre-finished fiber on the fixture of a tensile testing machine and performing unidirectional stretching at a constant speed. The preset stretching multiple range is selected based on the molecular properties of fungal chitosan and glucan and fiber application requirements, wherein: The preset stretching ratio is a stretching ratio relative to the initial length of the pre-finished fiber.

[0034] Optionally, the preset stretching ratio range is [1.2 times, 3 times].

[0035] Preferably, the preset stretching ratio is 2 times.

[0036] Specifically, the current batch of pre-finished fibers is used for tensile testing, and then the next batch of pre-finished fibers that do not have tensile fractures are sequentially surface washed and dried, including: Place the pre-finished fiber in a container containing a detergent. Immerse the fiber completely in the detergent and let it stand for 10 minutes. Then replace the detergent and stir at 50 to 100 rpm for 20 minutes. Repeat this operation 4 times until the conductivity of the solution after washing is consistent with that of the initial solution. It is considered clean. The pre-finished fiber after surface washing is spread flat on a breathable mesh rack, placed in a room temperature environment to drain naturally for 30 minutes to remove surface free water, and then transferred to a vacuum drying oven with a vacuum degree of ≥-0.09MPa to dry until the fiber moisture content is ≤5%.

[0037] In practice, the method of the present invention sets a determination process for the first dissolution abnormal area and the second dissolution abnormal area, and determines the abnormal concentration distribution in the raw material solution according to the first dissolution abnormal area and the second dissolution abnormal area. In the process of stirring the fungus-derived chitosan powder and the glucan powder, incompletely dissolved solute particles appear in the raw material solution due to the presence of undissolved solutes in the stirring process or the failure to filter out solutes with small particle size during the impurity removal process, which causes some undissolved particles to interfere with or block the extrusion process near the spinneret during extrusion, resulting in differences in the diameters of fiber segments at different positions of the extruded pre-finished fiber. Therefore, differences in the ability of different fiber segments to resist stress changes occur, which leads to the raw material solution with undissolved particles becoming a to-be-formed solution and entering the spinneret for extrusion, which is prone to the problem of the ability to resist stress changes. The change causes some adjacent fiber segments to break; when undissolved particles appear in the raw material solution, there are two areas where concentration differences are likely to occur. One is that the undissolved particles enter the rotation range of the stirring paddle 1 due to the shear force generated near the stirring paddle 1, and after a long period of accumulation, they become a relatively stable high concentration area. The other is the stirring dead corner area of ​​the beaker. The stirring dead corner area is an area where the stirring range of the stirring paddle 1 cannot effectively cover or the fluid disturbance intensity is significantly weakened. The stirring paddle 1 is prone to not stirring in place during stirring, causing the undissolved particles to aggregate; by adjusting the stirring height and ultrasonically crushing the second dissolution abnormal area, the concentration aggregation situation in the beaker was changed, and the influence of the undissolved particles on the quality and continuity of the fibers extruded from the spinneret was reduced, thereby improving the integrity of the fiber extrusion in the wet spinning process of the fungal-derived chitosan and glucan mixture.

[0038] Please refer to Figure 2 As shown, a first horizontal cylindrical area formed by the first corresponding maximum height intervals in all beakers corresponding to the extrusion fracture positions is determined as the first dissolution abnormality area.

[0039] Please continue to refer to Figure 2 As shown, determining the second dissolution abnormal area in the raw material solution includes, Counting the pre-finished fiber segments within the standard diameter range that have experienced tensile fracture; A second horizontal cylindrical area formed by a second corresponding maximum height interval of the raw material solution in the beaker corresponding to the extrusion time interval corresponding to the pre-finished fiber segment within the standard diameter range is determined as the second abnormal dissolution area.

[0040] In implementation, the present invention directly associates the extrusion fracture position with the first horizontal cylindrical area in the raw material solution, quantifies the first dissolution abnormality area through spatial dimensions, and determines the second horizontal cylindrical area composed of the extrusion time interval corresponding to the pre-finished fiber segment in the standard diameter range and the second corresponding maximum height interval of the raw material solution in the corresponding beaker as the second dissolution abnormality area, so that subsequent processing can accurately act on the target area, thereby reducing interference with normal areas, reducing energy consumption and raw material loss, and improving the targeting and efficiency of abnormal processing.

[0041] Specifically, the abnormal concentration distribution area type in the raw material solution is determined based on the overlap ratio of the overall abnormal area formed by the first dissolution abnormal area and the second dissolution abnormal area with the stirring range of the stirring paddle 1 and the overlap ratio of the stirring dead angle area.

[0042] In practice, the present invention establishes a quantitative judgment logic for the type of abnormal concentration distribution area by calculating the overlap ratio between the overall abnormal area and the stirring range of the stirring paddle 1 and the stirring dead angle area. The present invention clarifies the relationship between the abnormal area and the equipment disturbance characteristics through the overlap ratio, thereby improving the accuracy of process optimization.

[0043] Please refer to Figure 4 As shown, in implementation, if the overlapping area ratio of the overall abnormal area 2 and the stirring range 4 of the stirring paddle 1 is greater than the first preset overlapping area ratio, and the overlapping area ratio of the overall abnormal area 2 and the stirring dead angle area 3 is greater than the second preset overlapping area ratio, then the abnormal concentration distribution area type is determined to be a double abnormal area type; If the overlap ratio of the overall abnormal area and the stirring range 4 of the stirring paddle 1 is greater than the first preset overlap ratio, and the overlap ratio of the overall abnormal area and the stirring dead angle area is less than or equal to the second preset overlap ratio, the abnormal concentration distribution area type is determined to be the abnormal concentration area type around the stirring paddle 1; If the ratio of the overlapping area between the overall abnormal area and the stirring range 4 of the stirring paddle 1 is less than or equal to the first preset overlapping area ratio, and the ratio of the overlapping area between the overall abnormal area and the stirring dead angle area is greater than the second preset overlapping area ratio, the abnormal concentration distribution area type is determined to be the stirring dead angle area type.

[0044] In practice, the present invention distinguishes between the paddle circumference anomaly caused by insufficient disturbance of the agitator paddle 1, the dead angle anomaly caused by sluggish flow, and the dual anomaly of the coexistence of the two by setting a specific overlap ratio threshold, providing a clear direction for targeted treatment, improving the efficiency of process adjustment and the improvement of fiber quality.

[0045] Specifically, the abnormal concentration area around the stirring paddle 1 is a region where the solution has a fast convection speed due to the direct action of the stirring paddle 1, but the improper stirring height causes local turbulence, which prevents the chitosan and glucan powders from being fully dissolved, forming a high-concentration area where the solute is locally agglomerated. The solution in this area is transported to the spinneret in the first time period due to the fast convection speed. The stirring dead corner area is an area with low solution flow rate, such as near the cup wall outside the farthest rotation radius of the stirring paddle 1. This area lacks effective stirring, and the chitosan and glucan powders are easily deposited and form stable solute agglomerates. Moreover, the solution will be transported to the spinneret in the second time period due to the slow flow, wherein the first time period is earlier than the second time period.

[0046] Specifically, a 500 mL beaker with an inner diameter of 8 cm and a three-blade stirring paddle 1 with a diameter of 3 cm is used to mix and stir the fungus-derived chitosan powder and the base solution in the beaker. The stirring paddle 1 has an initial rotation speed of 200 rpm.

[0047] Preferably, according to the parameters of a 500 mL beaker and a stirring paddle 1 with a diameter of 3 cm, the preferred embodiments of the first preset overlap area ratio and the second preset overlap area ratio are both 50%.

[0048] Please continue to refer to Figure 4 As shown, if the ratio of the overlapping area between the overall abnormal area and the stirring range 4 of the stirring paddle 1 is less than or equal to the first preset overlapping area ratio, and the ratio of the overlapping area between the overall abnormal area and the stirring dead angle area is less than or equal to the second preset overlapping area ratio, the abnormal concentration distribution area type is determined to be a conventional abnormal area type.

[0049] Specifically, the treatment method for the conventional abnormal area type is to extend the stirring time by 1 hour based on the original stirring.

[0050] Specifically, the ratio of the overlapping area between the overall abnormal area and the stirring range 4 of the stirring paddle 1 is the ratio of the volume occupied by the same area in the overall abnormal area and the stirring range 4 of the stirring paddle 1 to the volume occupied by the stirring range 4 of the stirring paddle 1; the ratio of the overlapping area between the overall abnormal area and the stirring dead angle area is the ratio of the volume occupied by the same area in the overall abnormal area and the stirring dead angle area to the volume occupied by the stirring dead angle area.

[0051] Specifically, the breakage frequency of the pre-finished fiber is the ratio of the total number of the plurality of extrusion breakage locations to the length of the pre-finished fiber.

[0052] Please refer to Figure 3 As shown, if it is determined that the concentration around the stirring blade 1 is abnormal, the stirring height of the raw material solution is adjusted upward; If it is determined to be a stirring dead angle area type, applying ultrasonic vibration to the stirring dead angle area; If it is determined to be a double abnormal area type, the stirring height of the raw material solution is increased and ultrasonic vibration is applied to the stirring dead angle area at the same time.

[0053] Specifically, the ultrasonic vibration is applied through an immersion ultrasonic processor, which includes an ultrasonic generator arranged on a beaker to provide power for ultrasonic vibration, an immersion ultrasonic probe connected to the ultrasonic processor to apply ultrasonic vibration to the stirring dead corner area of ​​the raw material solution, and a positioning bracket connected to the immersion ultrasonic probe to ensure that the vibrating end of the probe is always aligned with the geometric center of the stirring dead corner.

[0054] Specifically, the preset diameter difference condition is that the diameter difference between the preceding section of pre-finished product fiber and the succeeding section of adjacent pre-finished product fiber at a single extrusion fracture position is greater than the preset diameter difference, wherein, The difference is the difference in diameter between a preceding section of pre-finished product fiber and a succeeding section of adjacent pre-finished product fiber at a single extrusion break position.

[0055] Specifically, the diameter is measured using a laser scanning caliper, which uses the principle of laser diffraction. When a single extrusion break is detected, the diffraction pattern generated by the single extrusion break corresponds to the diameter of the previous section of pre-finished fiber and the next section of adjacent pre-finished fiber. The system calculates and outputs the diameter value in real time. During implementation, a diameter gauge was installed under the spinneret to continuously monitor the diameter change during fiber extrusion, automatically mark the diameter value within 0.5s before and after the break position, and calculate the difference in diameter between the previous section of the pre-finished fiber and the next section of the adjacent pre-finished fiber at a single extrusion break position.

[0056] Working process: Chitosan and glucan, both derived from fungi, are ground separately to form powders of uniform particle size. The chitosan and glucan powders are then added to a base solution in proportion and stirred to form a raw material solution. The raw material solution is filtered to remove undissolved particles or impurities to prevent clogging of the spinneret during the spinning process. Vacuum defoaming is used to remove bubbles from the solution to prevent them from affecting the quality of fiber formation. The purified solution to be shaped is then sprayed through the spinneret into a coagulation bath, where it undergoes physical or chemical changes to form pre-finished fibers. The output pre-finished fibers are monitored, and several extrusion fracture locations are recorded. The fiber fracture frequency is calculated based on these fracture locations and the length of the pre-finished fibers. If the breakage frequency exceeds the preset threshold, the breakage positions that meet the preset conditions for the difference in diameter of adjacent fiber segments are further screened out, and the corresponding first dissolution abnormality area in the raw material solution is inferred based on these positions; pre-finished fiber segments with diameters within the standard range are selected for tensile testing, and the corresponding second dissolution abnormality area in the raw material solution is inferred by counting the fiber segments that are broken during stretching. The type of abnormal concentration distribution area in the raw material solution is determined based on the ratio of the overall abnormal area formed by the first dissolution abnormality area and the second dissolution abnormality area to the overlapping area of ​​the stirring range 4 of the stirring paddle 1 and the overlapping area of ​​the stirring dead angle area. If the abnormality is around the stirring paddle 1, the stirring height is adjusted to optimize the disturbance in the area; if the abnormality is in the stirring dead angle, ultrasonic vibration is applied to the dead angle area to disperse the agglomerates; if it is a double abnormality, the above two methods are combined; if it is a conventional abnormality, measures are taken to optimize the overall dispersion. The above-mentioned treatment strategy is adopted to treat the next batch of chitosan and glucan powders, which are stirred, removed from impurities and degassed in sequence, and then extruded into a coagulation bath through a spinneret to obtain the next batch of pre-finished fibers. Finally, the pre-finished fibers in the next batch that are not stretched and broken are surface washed and dried to finally obtain the finished mixed fibers.

[0057] Thus far, the technical solutions of the present invention have been described in conjunction with the preferred embodiments shown in the accompanying drawings. However, it will be readily understood by those skilled in the art that the scope of protection of the present invention is obviously not limited to these specific embodiments. Without departing from the principles of the present invention, those skilled in the art may make equivalent changes or substitutions to the relevant technical features, and the technical solutions after such changes or substitutions will fall within the scope of protection of the present invention.

Claims

1. A wet spinning method for a mixture of fungal chitosan and glucan, characterized in that: include: The formed raw material solution is sequentially subjected to impurity removal, degassing, and extrusion through a spinneret into a coagulation bath for fiber shaping to output a pre-finished fiber; Obtaining a plurality of extrusion fracture locations in the pre-finished fiber; determining a breakage frequency of the pre-finished fiber based on the plurality of extrusion breakage locations and the length of the pre-finished fiber; If the breakage frequency of the pre-finished fiber is greater than the preset breakage frequency, then the corresponding extrusion breakage positions that meet the preset diameter difference condition are counted; determining a first abnormal dissolution region in the raw material solution based on the corresponding extrusion fracture position; Performing a stretching test on a corresponding pre-finished fiber segment having a diameter within a standard diameter range according to a preset stretching multiple to determine a second abnormal dissolution region in the raw material solution; determining the type of abnormal concentration distribution region in the raw material solution based on the first abnormal dissolution region and the second abnormal dissolution region; Determining an abnormal treatment method according to the type of the abnormal concentration distribution area, including adjusting the stirring height of the raw material solution and / or performing ultrasonic crushing on the stirring dead corner area; According to the abnormal treatment method, the chitosan powder and the glucan powder of the next batch are stirred, impurity-removed, deaerated, and extruded through a spinneret to output the next batch of pre-finished fibers; The next batch of pre-finished fibers without tensile breakage are sequentially surface washed and dried to output finished mixed fibers.

2. The wet spinning method of a mixture of fungus-derived chitosan and glucan according to claim 1, characterized in that: A first horizontal cylindrical area formed by the first corresponding maximum height intervals in all beakers corresponding to the extrusion fracture positions is determined as the first abnormal dissolution area.

3. The wet spinning method of a mixture of fungus-derived chitosan and glucan according to claim 2, characterized in that: Determining a second abnormal dissolution region in the raw material solution includes: Counting the pre-finished fiber segments within the standard diameter range that have experienced tensile fracture; A second horizontal cylindrical area formed by a second corresponding maximum height interval of the raw material solution in the beaker corresponding to the extrusion time interval corresponding to the pre-finished fiber segment within the standard diameter range is determined as the second abnormal dissolution area.

4. The wet spinning method of a mixture of fungus-derived chitosan and glucan according to claim 3, characterized in that: The abnormal concentration distribution region type in the raw material solution is determined based on the overlap ratio of the overall abnormal region formed by the first and second abnormal dissolution regions with the stirring range of the stirring paddle and the overlap ratio of the stirring dead angle region.

5. The wet spinning method of a mixture of fungus-derived chitosan and glucan according to claim 4, characterized in that: If the ratio of the overlapping area between the overall abnormal area and the stirring range of the stirring paddle is greater than a first preset overlapping area ratio, and the ratio of the overlapping area between the overall abnormal area and the stirring dead angle area is greater than a second preset overlapping area ratio, the abnormal concentration distribution area type is determined to be a double abnormal area type; If the overlap ratio of the overall abnormal region and the stirring range of the stirring paddle is greater than the first preset overlap ratio, and the overlap ratio of the overall abnormal region and the stirring dead angle region is less than or equal to the second preset overlap ratio, the abnormal concentration distribution region type is determined as the abnormal concentration region type around the stirring paddle; If the ratio of the overlapping area between the overall abnormal area and the stirring range of the stirring paddle is less than or equal to the first preset overlapping area ratio, and the ratio of the overlapping area between the overall abnormal area and the stirring dead angle area is greater than the second preset overlapping area ratio, the abnormal concentration distribution area type is determined to be the stirring dead angle area type.

6. The wet spinning method of a mixture of fungus-derived chitosan and glucan according to claim 5, characterized in that: If the ratio of the overlapping area between the overall abnormal area and the stirring range of the stirring paddle is less than or equal to the first preset overlapping area ratio, and the ratio of the overlapping area between the overall abnormal area and the stirring dead angle area is less than or equal to the second preset overlapping area ratio, the abnormal concentration distribution area type is determined to be a conventional abnormal area type.

7. The wet spinning method of a mixture of fungus-derived chitosan and glucan according to claim 6, characterized in that: The ratio of the overlapping area between the overall abnormal area and the stirring range of the stirring paddle is the ratio of the volume occupied by the same area in the overall abnormal area and the stirring range of the stirring paddle to the volume occupied by the overall abnormal area; The ratio of the overlapping area between the overall abnormal area and the stirring dead angle area is the ratio of the volume occupied by the same area of ​​the overall abnormal area and the stirring dead angle area to the volume occupied by the overall abnormal area.

8. The wet spinning method of a mixture of fungus-derived chitosan and glucan according to claim 7, characterized in that: The break frequency of the pre-finished fiber is a ratio of the total number of the plurality of extruded break locations to the length of the pre-finished fiber.

9. The wet spinning method of a mixture of fungus-derived chitosan and glucan according to claim 8, characterized in that: If it is determined that the concentration is abnormal around the stirring blade, adjust the stirring height of the raw material solution upward; If it is determined to be a stirring dead angle area type, applying ultrasonic vibration to the stirring dead angle area; If it is determined to be a double abnormal area type, the stirring height of the raw material solution is increased and ultrasonic vibration is applied to the stirring dead angle area at the same time.

10. The wet spinning method of a mixture of fungus-derived chitosan and glucan according to claim 9, characterized in that: The preset diameter difference condition is that the diameter difference between the preceding section of pre-finished product fiber and the succeeding section of adjacent pre-finished product fiber at a single extrusion fracture position is greater than the preset diameter difference, wherein: The difference is the difference in diameter between a preceding section of pre-finished product fiber and a succeeding section of adjacent pre-finished product fiber at a single extrusion break position.

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