Wet spinning method for mixing fungus-derived chitosan and glucan

Abstract

The present application relates to the technical field of wet spinning, and particularly relates to a mixed wet spinning method of chitosan and dextran from fungi, which comprises the following steps: a formed raw material solution is sequentially subjected to impurity removal, defoaming and extrusion through a spinneret into a coagulation bath for fiber setting to output a pre-product fiber; a plurality of extrusion fracture positions in the pre-product fiber are obtained; a fracture frequency of the pre-product fiber is determined according to the plurality of extrusion fracture positions and the length of the pre-product fiber; a type of abnormal concentration distribution area in the raw material solution is determined based on a first dissolution abnormal area and a second dissolution abnormal area, and an abnormal treatment mode is determined, the chitosan powder and the dextran powder of the next batch are sequentially treated according to the abnormal treatment mode to output a pre-product fiber of the next batch, and the pre-product fiber without fracture is sequentially subjected to washing and drying to output a finished product mixed fiber; and the present application improves the efficiency of the mixed spinning process of chitosan and dextran.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of wet spinning, in particular to a mixed wet spinning method of fungus-derived chitosan and dextran. BACKGROUND

[0002] Fungus-derived chitosan and dextran, as natural polysaccharides, have important application potential in the fields of medical dressings, tissue engineering scaffolds, and biodegradable materials due to their excellent biocompatibility, degradability, and biological activity. Wet spinning technology is a common method for preparing polysaccharide fibers because it is gentle and causes little damage to the biological activity of polysaccharides. However, the existing technology for mixed wet spinning of chitosan and dextran is generally analyzed in terms of the causes of pre-product fiber breakage. The high concentration areas near the stirring paddle and the high concentration areas in the dead corners of the cup lead to significant differences in the time distribution of fiber breakage, but the existing technology cannot distinguish between them, resulting in poor targetedness of adjustment measures. Therefore, for mixed wet spinning of fungus-derived chitosan and dextran, there is an urgent need for a technical solution that can accurately identify the type of concentration anomaly, dynamically adjust the stirring parameters, and iteratively optimize the batch to improve fiber quality and production efficiency, in order to solve the problems of poor concentration control and insufficient adaptability in the existing technology and promote the practical application of fungus polysaccharide fibers in the field of biomedical materials.

[0003] Chinese Patent Publication No. CN118461230A discloses a plant polysaccharide nanofiber membrane and its preparation method and application, which comprises plant polysaccharide, supramolecular solvent, water, and polyvinyl alcohol fiber. Polysaccharides themselves do not have spinnability, especially plant polysaccharides are difficult to adhere to electrospinning. The present application creatively solves the problem of spinnability of plant polysaccharides, making it possible for polysaccharides to be used as nanomaterials, and expanding the application of plant polysaccharides in the fields of cosmetics and biological medicines. The nanofiber membrane prepared by electrospinning technology has high porosity and high specific surface area, which can more effectively exert the efficacy of plant polysaccharides. The present application not only opens up a new way for the application of plant polysaccharides in the fields of nanotechnology and biological medicines, but also provides an important reference for improving the practical value of supramolecular solvents and electrospinning technology in related fields. As can be seen, the plant polysaccharide nanofiber membrane and its preparation method and application have the problem that some adjacent fiber segments are broken due to the change in the ability to resist stress changes when the raw material solution containing undissolved particles in the area where concentration differences are easily generated during stirring is extruded from the spinneret, which further causes stress concentration at the fiber particle aggregation site of different batches, affecting the flexibility of the fiber. SUMMARY

[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:

[0006] 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;

[0007] Obtaining a plurality of extrusion fracture locations in the pre-finished fiber;

[0008] 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;

[0009] 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;

[0010] determining a first abnormal dissolution region in the raw material solution based on the corresponding extrusion fracture position;

[0011] 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;

[0012] 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;

[0013] 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;

[0014] 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;

[0015] The next batch of pre-finished fibers without tensile breakage are sequentially surface washed and dried to output finished mixed fibers.

[0016] 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.

[0017] Further, determining the second abnormal dissolution region in the raw material solution includes:

[0018] Counting the pre-finished fiber segments within the standard diameter range that have experienced tensile fracture;

[0019] 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.

[0020] 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.

[0021] 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;

[0022] 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;

[0023] 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.

[0024] 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.

[0025] 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.

[0026] 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.

[0027] 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;

[0028] If it is determined to be a stirring dead angle area type, applying ultrasonic vibration to the stirring dead angle area;

[0029] 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.

[0030] 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:

[0031] 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.

[0032] Compared with the prior art, the method has the beneficial effects that: the method determines the abnormal concentration distribution in the raw material solution according to the first and second abnormal dissolution areas, and in the process of stirring the fungus-derived chitosan powder and the dextran powder, due to the presence of unsolved solutes in the stirring process or the presence of small-particle solutes that are not filtered in the impurity removal process, the raw material solution contains unsolved solute particles, which causes some interference or blockage of the extrusion process near the spinneret when the spinneret is extruded, resulting in differences in the diameters of the fiber segments at different positions of the extruded pre-product fiber, and thus the ability of different fiber segments to resist stress changes differs, which causes the raw material solution containing unsolved particles to become a solution to be shaped when entering the spinneret for extrusion, and thus some adjacent fiber segments may break due to changes in the ability to resist stress changes; when unsolved particles are present in the raw material solution, two areas are prone to concentration differences, one is the area where the unsolved particles enter the rotation range of the stirring paddle due to the shear force generated near the stirring paddle, and the other is the stirring dead angle area of the beaker, which is an area that cannot be effectively covered by the stirring paddle or where the fluid disturbance intensity is significantly weakened, and the stirring paddle may not stir properly, causing the unsolved particles to aggregate; by adjusting the stirring height and ultrasonic crushing of the second abnormal dissolution area, the concentration aggregation in the beaker is changed, and the influence of the unsolved particles on the quality and continuity of the extruded fiber of the spinneret is reduced, thereby improving the integrity of the fiber extrusion in the fungus-derived chitosan and dextran mixed wet spinning process.

[0033] Further, the present application directly associates the extrusion breakage position with the first horizontal cylindrical area in the raw material solution, quantifies the first abnormal dissolution area by spatial dimension, determines the second horizontal cylindrical area formed by the extrusion time interval of the pre-product fiber segment within the standard diameter range and the corresponding second corresponding maximum height interval of the raw material solution in the beaker as the second abnormal dissolution area, so that the subsequent processing can accurately act on the target area, thereby reducing the interference with the normal area, reducing energy consumption and raw material loss, and improving the targeting and efficiency of abnormal processing.

[0034] Further, the present application establishes a quantitative determination logic of the abnormal concentration distribution area type by calculating the overlap ratio of the overall abnormal area and the stirring range of the stirring paddle and the stirring dead angle area, and the present application clearly associates the abnormal area with the disturbance characteristics of the equipment by the overlap ratio, thereby improving the accuracy of process optimization.

[0035] 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

[0036] 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;

[0037] 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;

[0038] 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;

[0039] 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;

[0040] Explanation of the reference numerals: 1- stirring paddle, 2- overall abnormal area, 3- stirring dead angle area, 4- stirring range. DETAILED DESCRIPTION

[0041] 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.

[0042] 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.

[0043] 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.

[0044] Moreover, it needs to be explained that in the description of the present application, unless otherwise explicitly specified and limited, the terms "mounting", "connection", "connecting" should be understood in a broad sense and for example, can be fixed connection, can also be detachable connection, or integrally connected; can be mechanical connection, can also be electrical connection; can be directly connected, can also be indirectly connected through intermediate medium, can be internal communication of two elements. For those skilled in the art, the specific meaning of the above terms in the present application can be understood according to the specific circumstances.

[0045] Please refer to Figure 1 、 Figure 2 、 Figure 3 and Figure 4 , which are respectively the overall flowchart of the mixed wet spinning method of fungal-derived chitosan and dextran, the method flowchart of determining the first and second dissolution abnormal regions, the method flowchart of abnormal processing mode, and the structural schematic diagram of the overall abnormal region and the stirring range of the stirring paddle when the type of the abnormal concentration distribution region is determined as the double abnormal region type; the mixed wet spinning method of fungal-derived chitosan and dextran in the embodiment of the present application, comprising:

[0046] Step S1, the raw material solution formed by mixing and stirring the fungal-derived chitosan powder and dextran powder and the base solution in the beaker is successively subjected to impurity removal, defoaming, and extruded to the coagulation bath through the spinneret for fiber setting to output the pre-product fiber;

[0047] Step S2, a plurality of extrusion fracture positions in the pre-product fiber are obtained;

[0048] Step S3, the fracture frequency of the pre-product fiber is determined according to the plurality of extrusion fracture positions and the length of the pre-product fiber;

[0049] Step S4, if the fracture frequency of the pre-product fiber is greater than the preset fracture frequency, the corresponding extrusion fracture position meeting the preset diameter difference condition is counted;

[0050] Step S5, the first dissolution abnormal region in the raw material solution is determined based on the corresponding extrusion fracture position;

[0051] Step S6, the corresponding pre-product fiber segment with a diameter meeting the standard diameter range is subjected to stretching test according to the preset stretching multiple to determine the second dissolution abnormal region in the raw material solution;

[0052] Step S7, the type of the abnormal concentration distribution region in the raw material solution is determined based on the first and second dissolution abnormal regions;

[0053] Step S8, determining an abnormality processing mode according to the abnormal concentration distribution area type, including adjusting the stirring height of the raw material solution and / or performing ultrasonic crushing on the stirring dead angle area;

[0054] Step S9, stirring, impurity removal, defoaming and extruding through the spinneret to output the next batch of pre-product fibers according to the abnormality processing mode for the next batch of chitosan powder and dextran powder in sequence;

[0055] Step S10, sequentially performing surface washing and drying on the next batch of pre-product fibers without tensile fracture to output the finished mixed fibers.

[0056] Specifically, the chitosan and dextran are derived from fungal fermentation products or mycelium extraction.

[0057] Preferably, the chitosan is extracted from the fermentation mycelium of filamentous fungi, and the molecular weight range is [100000 Da, 500000 Da]; the chitosan is extracted from the mycelium or fruiting body of filamentous fungi, and the molecular weight range is [300000 Da, 1000000 Da].

[0058] Specifically, chitosan can impart good mechanical strength and antibacterial properties to the fibers, and dextran can enhance the biocompatibility and moisturizing properties of the fibers. In preferred embodiments, the mass ratio of chitosan powder to dextran powder is 2:1.

[0059] Specifically, the fungal-derived chitosan and dextran are ground by a planetary ball mill for 2 hours; the base solution is a 2% acetic acid aqueous solution; the impurity removal process uses a 300-mesh filter to remove insoluble particles, wherein,

[0060] Based on the solvent capacity of 2% acetic acid aqueous solution, the solubility limit of chitosan powder in 2% acetic acid aqueous solution is about 3%, and in preferred embodiments, 2.5g of chitosan powder is added to every 100mL 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, so 1.25g of dextran powder is added to every 100mL of base solution.

[0061] Specifically, the defoaming treatment is a process of vacuum defoaming the raw material solution for 20 minutes under a vacuum degree of -0.09MPa.

[0062] Specifically, the pore size of the spinneret is 0.3mm, and the extrusion speed is 0.5mL / min; the coagulation bath is a mixed solution of 5% sodium hydroxide solution and 20% ethanol aqueous solution placed in a 500mL polytetrafluoroethylene flat-bottom container, and the temperature of the coagulation bath is 25℃.

[0063] It is understood by those skilled in the art that the operation principle and operation process of the planetary ball mill are conventional technical means known to those skilled in the art, and thus the operation principle and operation process of the planetary ball mill are not described herein.

[0064] Specifically, under the conditions that the aperture of the spinneret is 0.3 mm and the extrusion speed is 0.5 mL / min, the preferred embodiment of the standard diameter range is [15 μm, 25 μm].

[0065] Specifically, the stretching treatment test is to fix the pre-product fiber on the clamps of a stretching testing machine for unidirectional stretching at a constant speed, and the preset stretching multiple range is selected based on the molecular properties of the fungus-derived chitosan and dextran and the fiber application requirements, wherein,

[0066] The preset stretching multiple is the stretching multiple relative to the initial length of the pre-product fiber.

[0067] Optionally, the preset stretching multiple range is [1.2 times, 3 times].

[0068] Preferably, the preferred embodiment of the preset stretching multiple is 2 times.

[0069] Specifically, the pre-product fiber of the current batch is used for stretching test, and then the pre-product fiber of the next batch without stretching breakage is sequentially subjected to surface washing and drying, including:

[0070] The pre-product fiber is placed in a container containing a washing reagent, the fiber is completely immersed in the reagent and stands for 10 minutes, then the washing reagent is replaced, and the fiber is stirred at a speed of 50 to 100 rpm for 20 minutes, the operation is repeated 4 times, until the conductivity of the solution after washing is consistent with that of the initial reagent, then it is determined that the washing is complete.

[0071] The pre-product fiber after surface washing is laid on a breathable mesh rack, and is naturally drained for 30 minutes in a room temperature environment to remove free water on the surface, and is then transferred to a vacuum drying box with a vacuum degree of ≥-0.09 MPa for drying until the moisture content of the fiber is ≤5%.

[0072] In the implementation, the method provided by the present application determines the abnormal concentration distribution in the raw material solution according to the first and second dissolution abnormal areas, and in the process of stirring the fungus-derived chitosan powder and the dextran powder, due to the presence of unsolved solutes in the stirring process or the failure to filter the solutes with small particle sizes in the impurity removal process, the raw material solution contains unsolved solute particles, which causes some interference or blockage of the extrusion process of the spinneret when the spinneret is extruded, resulting in differences in the diameters of the fiber segments at different positions of the extruded pre-product fibers, and thus the ability of the different fiber segments to resist stress changes is different. Therefore, when the raw material solution containing unsolved particles enters the spinneret for extrusion to become a solution to be shaped, the change in the ability to resist stress changes can easily cause some adjacent fiber segments to break. When unsolved particles are present in the raw material solution, two areas are prone to concentration differences. One is the area where the unsolved 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, it becomes a relatively stable high-concentration area. The other is the stirring dead angle area of the beaker, which is an area that cannot be effectively covered by the stirring paddle 1 or where the fluid disturbance intensity is significantly weakened. The stirring paddle 1 is prone to incomplete stirring, causing the unsolved particles to aggregate. By adjusting the stirring height and performing ultrasonic crushing on the second dissolution abnormal area, the concentration aggregation in the beaker is changed, the influence of the unsolved particles on the quality and continuity of the extruded fiber of the spinneret is reduced, and the integrity of the fiber extrusion in the mixed wet spinning process of the fungus-derived chitosan and dextran is improved.

[0073] Please refer to Figure 2 The first horizontal cylindrical area formed by all the first corresponding maximum height intervals in the beaker corresponding to the extrusion fracture position is determined as the first dissolution abnormal area.

[0074] Please continue to refer to Figure 2 The second dissolution abnormal area in the raw material solution is determined, including,

[0075] The pre-product fiber segments in the standard diameter range that occur tensile fracture are counted.

[0076] The second horizontal cylindrical area formed by the second corresponding maximum height intervals of the raw material solution in the beaker corresponding to the extrusion time interval of the pre-product fiber segments in the standard diameter range is determined as the second dissolution abnormal area.

[0077] 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.

[0078] 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.

[0079] 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.

[0080] 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;

[0081] 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;

[0082] 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.

[0083] 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.

[0084] 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.

[0085] 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.

[0086] 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.

[0087] 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%.

[0088] 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.

[0089] Specifically, the treatment method for the conventional abnormal area type is to extend the stirring time by 1 hour based on the original stirring.

[0090] 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.

[0091] 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.

[0092] Please refer to Figure 3If the abnormal region type around the stirring blade 1 is determined, the stirring height of the raw material solution is adjusted upward;

[0093] If the stirring dead angle region type is determined, the stirring dead angle region is subjected to ultrasonic vibration;

[0094] If the double abnormal region type is determined, the stirring height of the raw material solution is increased and the stirring dead angle region is subjected to ultrasonic vibration at the same time.

[0095] Specifically, the ultrasonic vibration is applied by an immersion ultrasonic processor, which includes an ultrasonic generator provided on a beaker to provide power for ultrasonic vibration, and an immersion ultrasonic probe connected to the ultrasonic processor to apply ultrasonic vibration to the stirring dead angle region of the raw material solution, and a positioning support connected to the immersion ultrasonic probe to ensure that the vibration end of the probe is always aligned with the geometric center of the stirring dead angle.

[0096] Specifically, the preset diameter difference condition is that the difference between the diameters of the front section of the pre-product fiber and the rear section of the adjacent pre-product fiber at the single extrusion fracture position is greater than the preset diameter difference amount, wherein,

[0097] The difference amount is the difference between the diameters of the front section of the pre-product fiber and the rear section of the adjacent pre-product fiber at the single extrusion fracture position.

[0098] Specifically, the diameter is measured by a laser scanning diameter gauge, which uses the principle of laser diffraction. When the single extrusion fracture position is detected, the diffraction pattern generated by the single extrusion fracture position corresponds to the diameters of the front section of the pre-product fiber and the rear section of the adjacent pre-product fiber. The system calculates and outputs the diameter value in real time.

[0099] In implementation, a diameter gauge is installed below the spinneret to continuously monitor the diameter change during the fiber extrusion process, automatically mark the diameter values within 0.5s before and after the fracture position, and calculate the difference between the diameters of the front section of the pre-product fiber and the rear section of the adjacent pre-product fiber at the single extrusion fracture position.

[0100] 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.

[0101] 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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