Method for producing silkworm protein viscose fibers by utilizing matured silkworms

Abstract

The invention relates to the technical field of biological materials, in particular to a method for producing silkworm protein viscose fibers by using matured silkworms, which comprises the following steps: S1, selecting matured silkworms in the mature period of silkworms, and peeling the matured silkworms; s2, mixing the peeled matured silkworm raw material with an acid solution to carry out an acid hydrolysis reaction; s3, carrying out preliminary filtering; s4, carrying out enzymolysis treatment on the hydrolysate filtered in the step S3; s5, mixing the silkworm protein solution subjected to enzymolysis with a polyvinyl alcohol solution; s6, spinning is conducted through a spinning nozzle; s7, carrying out hot stretching treatment; and S8, carrying out water washing and drying treatment to obtain a silkworm protein viscose fiber finished product. According to the method disclosed by the invention, acid hydrolysis and enzymolysis treatment are combined, so that the extraction efficiency of the silkworm protein is improved, spinning and hot drawing processes are optimized, the strength, elasticity and degradability of the silkworm protein viscose fiber are remarkably improved, and the method has relatively high production efficiency and wide industrial application prospects.

Description

Technical Field

[0001] The present invention relates to the technical field of biomaterials, and particularly to a method for producing silkworm protein viscose fiber by using mature silkworms of Bombyx mori. Background Art

[0002] In recent years, mature silkworm protein viscose fiber, as a new type of environmentally friendly material, has gradually attracted wide attention in the academic and industrial fields due to its good biodegradability and excellent mechanical properties; mature silkworm protein has natural hydrophilicity and biocompatibility and can be applied in the fields of textiles, medicine, environmental protection, etc.; however, the existing production process of mature silkworm protein viscose fiber still faces some technical challenges, especially in terms of how to efficiently extract mature silkworm protein, optimize fiber properties, and improve production efficiency, etc., there are still certain difficulties.

[0003] Traditional methods for producing mature silkworm protein fibers mostly rely on chemical dissolution and physical spinning processes. Although fibers of a certain quality can be obtained, there are still some problems to be solved in the extraction and processing of mature silkworm protein; for example, in the extraction process of mature silkworm protein by traditional acid hydrolysis or enzymatic hydrolysis methods, relatively long reaction times and high temperatures are often required, resulting in low reaction efficiency and possible destruction of the protein structure, affecting the properties of the final fiber; in addition, the existing spinning process is still not fine enough in the regulation of fiber strength, elasticity, etc., resulting in the comprehensive properties of mature silkworm protein viscose fiber being difficult to meet the needs of the high-end market. Summary of the Invention

[0004] Based on the above purposes, the present invention provides a method for producing silkworm protein viscose fiber by using mature silkworms of Bombyx mori.

[0005] A method for producing silkworm protein viscose fiber by using mature silkworms of Bombyx mori, comprising the following steps:

[0006] S1: Select mature silkworms at the mature stage of Bombyx mori, and perform molting treatment on them to obtain the molted mature silkworm raw materials;

[0007] S2: Mix the molted mature silkworm raw materials with an acidic solution, and perform acid hydrolysis reaction at a predetermined temperature to obtain a hydrolysis solution;

[0008] S3: Perform preliminary filtration on the hydrolysis solution to remove the solid impurities generated during the hydrolysis process, and obtain a liquid containing silkworm protein;

[0009] S4: Perform enzymatic hydrolysis treatment on the hydrolysis solution filtered in S3 to degrade silkworm protein and improve its fibrillation performance;

[0010] S5: Mix the enzymatically hydrolyzed silkworm protein solution with a polyvinyl alcohol solution to form a mixed solution;

[0011] S6: Spinning the mixed solution formed in S5 through a spinneret and solidifying it with a coolant to form a preliminary silkworm protein viscose fiber;

[0012] S7: Performing a hot stretching treatment on the cooled silkworm protein viscose fiber to improve the strength and elasticity of the fiber;

[0013] S8: Washing the stretched silkworm protein viscose fiber and removing excess moisture by drying to finally obtain the finished product of silkworm protein viscose fiber.

[0014] Optionally, S1 specifically includes:

[0015] S11: Selecting ripe silkworms at the mature stage of silkworms, and the weight range of the selected ripe silkworms is 0.2 g to 0.5 g;

[0016] S12: Performing a preliminary cleaning on the selected ripe silkworms to remove surface impurities and dirt, and the cleaning solution is deionized water;

[0017] S13: Immersing the cleaned ripe silkworms in a skin-removing solvent, the skin-removing solvent is chloroform or an alcohol solvent, the immersion time is 30 minutes to 60 minutes, and the immersion temperature is 20°C to 30°C. Removing the outer shell of the ripe silkworms through the action of the solvent to obtain the raw material of the skinned ripe silkworms.

[0018] Optionally, S2 specifically includes:

[0019] S21: Mixing the raw material of the skinned ripe silkworms with an acidic solution, the acidic solution is hydrochloric acid solution, sulfuric acid solution or acetic acid solution, the concentration of the acid is 0.5 mol / L to 2 mol / L, and the mixing ratio is that the mass ratio of the skinned ripe silkworm raw material to the acidic solution is 1:2 to 1:4;

[0020] S22: Heating the mixed raw material of the skinned ripe silkworms and the acidic solution in a reactor, setting the reaction temperature to 40°C to 60°C, and the reaction time to 2 hours to 4 hours;

[0021] S23: After the reaction ends, cooling the hydrolysis solution to room temperature.

[0022] Optionally, S3 specifically includes:

[0023] S31: Transferring the hydrolysis solution formed in S2 to a filtering device, and the filtering device is a filter with a filter mesh aperture of 50 μm to 100 μm;

[0024] S32: Performing a preliminary filtration by pressure filtration, the filtration pressure is 0.05 MPa to 0.2 MPa, and the filtration time is 10 minutes to 30 minutes to remove the solid impurities generated during the hydrolysis process.

[0025] Optionally, S4 specifically includes:

[0026] S41: Transfer the hydrolyzate filtered in S3 to an enzymatic hydrolysis reactor, and add cellulase or protease. The addition amount of the enzyme is 0.5% to 2% of the mass of the hydrolyzate.

[0027] S42: Adjust the reaction temperature to 45°C to 55°C, and maintain a constant temperature reaction for 4 to 6 hours to ensure that the enzymatic hydrolysis reaction proceeds fully.

[0028] S43: After the reaction ends, cool the enzymatic hydrolysate to room temperature to obtain a silkworm protein solution that has undergone enzymatic hydrolysis treatment.

[0029] Optionally, S5 specifically includes:

[0030] S51: Mix the silkworm protein solution after enzymatic hydrolysis with a polyvinyl alcohol solution at a mass ratio of 1:2. The concentration of the polyvinyl alcohol solution is 5 wt% to 10 wt%.

[0031] S52: Adjust the temperature of the mixed solution to 20°C to 30°C, and under stirring conditions, use a mechanical stirrer to stir at a speed of 200 rpm to 500 rpm for 30 to 60 minutes to obtain a mixed solution.

[0032] Optionally, S6 specifically includes:

[0033] S61: Spun the mixed solution formed in S5 through a spinneret. The pore diameter of the spinneret is 0.2 mm to 0.5 mm, and the spinning rate is 5 m / min to 20 m / min.

[0034] S62: Solidify the mixed solution after spinning through a coolant. The coolant is water, and the temperature of the coolant is controlled at 5°C to 15°C, and the cooling time is 1 second to 5 seconds. Form a preliminary silkworm protein viscose fiber.

[0035] Optionally, S7 specifically includes:

[0036] S71: Perform a hot stretching treatment on the cooled silkworm protein viscose fiber. The hot stretching treatment includes placing the fiber in a heating device and setting the stretching temperature to 60°C to 80°C.

[0037] S72: At the set stretching temperature, stretch the fiber at a stretching speed of 1 times / minute to 5 times / minute.

[0038] S73: Stretch the fiber along its length direction to 2 to 4 times its original length.

[0039] S74: During the stretching process, maintain a constant stretching tension, and the stretching tension is controlled at 10 N to 30 N.

[0040] S75: After stretching is completed, remove the fiber from the heating device and let it cool naturally to room temperature.

[0041] Optionally, the specific steps of S8 are as follows:

[0042] S81: Place the stretched mulberry silk protein viscose fiber in a water-washing device, add deionized water, and set the water-washing temperature to 20°C to 30°C.

[0043] S82: In the water-washing device, circulate deionized water through the mulberry silk protein viscose fiber at a constant flow rate, control the constant flow rate at 0.5 L / min to 2 L / min, and the circulation time is 15 minutes to 30 minutes to fully remove the excess solvent and impurities in the fiber.

[0044] Optionally, S8 further includes:

[0045] S84: Place the water-washed mulberry silk protein viscose fiber in a drying device and set the drying temperature to 60°C to 80°C.

[0046] S85: In the drying device, blow hot air over the mulberry silk protein viscose fiber at a constant wind speed, control the constant wind speed at 2 m / s to 5 m / s, and the drying time is 2 hours to 4 hours to remove the excess moisture in the fiber.

[0047] S86: After drying is completed, take out the dried mulberry silk protein viscose fiber from the drying device to finally obtain the finished product of mulberry silk protein viscose fiber.

[0048] Advantages of the present invention:

[0049] In the present invention, by adopting the combined method of acid hydrolysis and enzymatic hydrolysis, the extraction efficiency of mulberry silk protein is significantly improved, and the performance of the fiber is effectively improved; by reasonably controlling the conditions of the acid hydrolysis reaction and enzymatic hydrolysis treatment, mulberry silk protein can be efficiently extracted in a short time, while avoiding the problem of protein structure damage caused by high-temperature and long-time reactions in traditional methods, ensuring the strength, elasticity and degradability of the final fiber.

[0050] In the present invention, by optimizing the spinning process and hot stretching treatment, the physical properties of the mulberry silk protein viscose fiber are further improved; by adopting the combined method of spinneret spinning and coolant solidification, the diameter and morphology of the fiber can be precisely controlled, and the hot stretching process effectively improves the strength and toughness of the fiber; the combination of water washing and drying treatments also ensures the purity and dryness of the fiber. Description of the Drawings

[0051] In order to more clearly illustrate the technical solutions in the present invention or the prior art, the following will briefly introduce the accompanying drawings required for the description of the embodiments or the prior art. Obviously, the accompanying drawings in the following description are only those of the present invention. For those of ordinary skill in the art, without creative efforts, other accompanying drawings can also be obtained based on these drawings.

[0052] Figure 1 Schematic diagram of the method for producing silkworm protein viscose fiber according to an embodiment of the present invention;

[0053] Figure 2 Schematic diagram of the process for performing hot stretching treatment according to an embodiment of the present invention. Detailed implementation manners

[0054] The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments. At the same time, it should be noted here that in order to make the embodiments more detailed, the following embodiments are the best and preferred embodiments. For some well-known technologies, those skilled in the art can also adopt other alternative methods for implementation; moreover, the accompanying drawings are only for more specifically describing the embodiments, and are not intended to specifically limit the present invention.

[0055] It should be noted that in the specification, when referring to "an embodiment", "embodiments", "exemplary embodiments", "some embodiments", etc., it indicates that the described embodiments may include specific features, structures or characteristics, but not necessarily every embodiment includes such specific features, structures or characteristics. Additionally, when combining embodiments to describe specific features, structures or characteristics, implementing such features, structures or characteristics in combination with other embodiments (whether explicitly described or not) should be within the knowledge scope of those skilled in the relevant art.

[0056] Generally, terms can be understood at least in part from their use in the context. For example, at least in part depending on the context, the term "one or more" used herein can be used to describe any feature, structure or characteristic in a singular sense, or can be used to describe a combination of features, structures or characteristics in a plural sense. Additionally, the term "based on" can be understood as not necessarily aiming to convey a set of exclusive factors, but rather, at least in part depending on the context, allowing for the existence of other factors that may not be explicitly described.

[0057] Embodiment 1

[0058] As Figure 1 - Figure 2 shown, a method for producing silkworm protein viscose fiber using mature silkworms includes the following steps:

[0059] S1: Select mature silkworms at the maturity stage of silkworms, and perform molting treatment on them to obtain the molted mature silkworm raw materials;

[0060] S2: Mix the cooked silkworm raw materials after molting with an acidic solution and conduct an acid hydrolysis reaction at a predetermined temperature to obtain a hydrolysis solution;

[0061] S3: Conduct a preliminary filtration on the hydrolysis solution to remove the solid impurities generated during the hydrolysis process to obtain a liquid containing silkworm protein;

[0062] S4: Conduct an enzymatic hydrolysis treatment on the hydrolysis solution filtered in S3 to degrade the silkworm protein and improve its fibrillation performance;

[0063] S5: Mix the silkworm protein solution after enzymatic hydrolysis with a polyvinyl alcohol (PVA) solution to form a mixed solution;

[0064] S6: Spin the mixed solution formed in S5 through a spinneret and solidify it through a coolant to form a preliminary silkworm protein viscose fiber;

[0065] S7: Conduct a thermal stretching treatment on the cooled silkworm protein viscose fiber to improve the strength and elasticity of the fiber, enabling the fiber to possess the required physical properties for subsequent applications;

[0066] S8: Conduct a water washing treatment on the stretched silkworm protein viscose fiber and remove the excess moisture through drying to finally obtain the finished product of silkworm protein viscose fiber.

[0067] S1 specifically includes:

[0068] S11: Select cooked silkworms at the mature stage of the silkworm, and the weight of the selected cooked silkworms is 0.3 g;

[0069] S12: Conduct a preliminary cleaning on the selected cooked silkworms to remove the surface impurities and dirt, and the cleaning solution is deionized water;

[0070] S13: Immerse the cleaned cooked silkworms in a molting solvent. The molting solvent is a chloroform solvent, the immersion time is 45 minutes, and the immersion temperature is 25 °C. Remove the outer shell of the cooked silkworms through the action of the solvent to obtain the cooked silkworm raw materials after molting.

[0071] S2 specifically includes:

[0072] S21: Mix the cooked silkworm raw materials after molting with an acidic solution. The acidic solution is a sulfuric acid solution, the concentration of the acid is 1 mol / L, and the mixing ratio is that the mass ratio of the cooked silkworm raw materials after molting to the acidic solution is 1:3;

[0073] S22: Heat the mixed cooked silkworm raw materials after molting and the acidic solution in a reactor, set the reaction temperature to 50 °C, and the reaction time to 3 hours to ensure the full progress of the acid hydrolysis reaction;

[0074] S23: After the reaction ends, cool the hydrolysis solution to room temperature and prepare for subsequent filtration and treatment.

[0075] S3 specifically includes:

[0076] S31: Transfer the hydrolyzate formed in S2 to a filtering device, where the filtering device is a filter with a filter mesh aperture of 75 μm;

[0077] S32: Conduct preliminary filtration by means of pressure filtration, with a filtration pressure of 0.1 MPa and a filtration time of 20 minutes, to remove the solid impurities generated during the hydrolysis process.

[0078] S4 specifically includes:

[0079] S41: Transfer the hydrolyzate after filtration in S3 to an enzymatic hydrolysis reactor, and add cellulase, with the addition amount of the enzyme being 1% of the mass of the hydrolyzate;

[0080] S42: Adjust the reaction temperature to 50 °C and maintain a constant-temperature reaction for 5 hours to ensure the full progress of the enzymatic hydrolysis reaction;

[0081] S43: After the reaction ends, cool the enzymatic hydrolysate to room temperature to obtain the silkworm protein solution after enzymatic hydrolysis treatment.

[0082] S5 specifically includes:

[0083] S51: Mix the silkworm protein solution after enzymatic hydrolysis with a polyvinyl alcohol solution at a mass ratio of 1:2, and the concentration of the polyvinyl alcohol solution is 7 wt%;

[0084] S52: Adjust the temperature of the mixed solution to 25 °C, and under stirring conditions, use a mechanical stirrer to stir at a speed of 300 rpm for 45 minutes to ensure the full mixing of the silkworm protein solution and the polyvinyl alcohol solution, obtaining a mixed solution for subsequent spinning treatment.

[0085] S6 specifically includes:

[0086] S61: Spin the mixed solution formed in S5 through a spinneret, where the aperture of the spinneret is 0.4 mm and the spinning rate is 10 m / min;

[0087] S62: Solidify the mixed solution after spinning through a coolant, where the coolant is water, the temperature of the coolant is controlled at 10 °C, and the cooling time is 3 seconds. Form a preliminary silkworm protein viscose fiber for subsequent hot stretching treatment.

[0088] S7 specifically includes:

[0089] S71: Conduct hot stretching treatment on the cooled silkworm protein viscose fiber. The hot stretching treatment includes placing the fiber in a heating device and setting the stretching temperature to 70 °C;

[0090] S72: At the set stretching temperature, stretch the fiber at a stretching speed of 3 times per minute;

[0091] S73: Stretch the fiber along its length direction to 3 times its original length;

[0092] S74: During the stretching process, maintain a constant stretching tension, and control the stretching tension to 20 N;

[0093] S75: After completing the stretching, remove the fiber from the heating device and let it cool naturally to room temperature, preparing for the subsequent water washing treatment.

[0094] The specific steps of the water washing treatment in S8 include:

[0095] S81: Place the stretched mulberry silk fibroin viscose fiber in a water washing device, add deionized water, and set the water washing temperature to 25 °C;

[0096] S82: In the water washing device, circulate deionized water through the mulberry silk fibroin viscose fiber at a constant flow rate. Control the constant flow rate at 1 L / min, and the circulation time is 20 minutes to fully remove the excess solvent and impurities in the fiber.

[0097] S8 also includes:

[0098] S84: Place the water-washed mulberry silk fibroin viscose fiber in a drying device, and set the drying temperature to 70 °C;

[0099] S85: In the drying device, blow hot air over the mulberry silk fibroin viscose fiber at a constant wind speed. Control the constant wind speed at 3 m / s, and the drying time is 3 hours to remove the excess moisture in the fiber;

[0100] S86: After completing the drying, take out the dried mulberry silk fibroin viscose fiber from the drying device to finally obtain the finished product of mulberry silk fibroin viscose fiber.

[0101] Example 2

[0102] S1: First, select mature silkworms with a body weight of 0.2 grams; the selected mature silkworms are preliminarily cleaned, and the impurities and dirt on the surface are removed using deionized water; subsequently, soak the cleaned mature silkworms in a peeling solvent. Select an alcohol solvent, set the soaking time to 30 minutes, and maintain the soaking temperature at 20 °C; through the action of the solvent, effectively remove the outer shell of the mature silkworms to finally obtain the peeled mature silkworm raw material, preparing for the subsequent acid hydrolysis step;

[0103] S2: Mix the cooked silkworm raw materials after skinning with an acidic solution at a mass ratio of 1:2. The selected acidic solution is 0.5 mol / L hydrochloric acid solution. Heat the mixed mixture in a reactor to 40°C and keep the reaction at this temperature for 2 hours to ensure that the acid hydrolysis reaction proceeds fully. After the reaction, cool the hydrolysis solution to room temperature to prepare for the subsequent filtration step.

[0104] S3: Transfer the cooled hydrolysis solution to a filter with a filter mesh aperture of 50 microns and conduct preliminary filtration by means of pressure filtration. During the filtration process, control the filtration pressure at 0.05 MPa and set the filtration time to 10 minutes to effectively remove the solid impurities generated during the hydrolysis process. After filtration, obtain a clear liquid containing silkworm protein to provide a pure basic liquid for the subsequent enzymatic hydrolysis treatment.

[0105] S4: Transfer the filtered hydrolysis solution to an enzymatic hydrolysis reactor and add protease at 0.5% of the mass of the hydrolysis solution. Adjust the reaction temperature to 45°C and keep the reaction at this constant temperature for 4 hours to fully degrade the silkworm protein and improve its fibrillation performance. After the reaction, cool the enzymatic hydrolysis solution to room temperature to obtain the silkworm protein solution after enzymatic hydrolysis treatment.

[0106] S5: Mix the silkworm protein solution after enzymatic hydrolysis with a 5wt% polyvinyl alcohol solution at a mass ratio of 1:2. Adjust the temperature of the mixed solution to 20°C and stir it on a mechanical stirrer at a speed of 200 revolutions per minute for 30 minutes to ensure that the two solutions are fully mixed evenly to form a stable mixed solution, providing a suitable fiber-forming medium for the spinning step.

[0107] S6: Spin the prepared mixed solution through a spinneret with an aperture of 0.2 mm, and control the spinning rate at 5 m / min. The spun solution is solidified by a coolant with a temperature controlled at 5°C, and the cooling time is set to 1 second. Through this process, form preliminary silkworm protein viscose fibers to prepare for the subsequent physical property improvement step.

[0108] S7: Place the cooled and solidified silkworm protein viscose fibers in a heating device, and set the heating temperature at 60°C. At this temperature, stretch the fibers at a stretching speed of 1 times / minute along the fiber length direction to stretch them to 2 times their original length while maintaining a constant stretching tension, and control the tension at 10 Newtons. After stretching, remove the fibers from the heating device and let them cool naturally to room temperature.

[0109] S8: Place the thermally stretched silkworm protein viscose fiber in a water washing device, add deionized water, and set the water washing temperature at 20°C. During the water washing process, circulate the deionized water through the fiber at a constant flow rate of 0.5 liters per minute, and control the circulation time at 15 minutes to fully remove the excess solvent and impurities in the fiber. Subsequently, place the water-washed fiber in a drying device, set the drying temperature at 60°C, and blow hot air over the fiber at a constant wind speed of 2 meters per second. Set the drying time at 2 hours to completely remove the moisture in the fiber. After drying is completed, take out the fiber from the drying device to finally obtain a high-quality finished product of silkworm protein viscose fiber.

[0110] Example 3

[0111] S1: First, select mature silkworms with a body weight of 0.5 grams. The selected mature silkworms are preliminarily cleaned, and the impurities and dirt on the surface are removed using deionized water. Subsequently, soak the cleaned mature silkworms in a skin-removing solvent. Select chloroform as the solvent, set the soaking time at 60 minutes, and maintain the soaking temperature at 30°C. Through the action of the solvent, effectively remove the outer shell of the mature silkworms to finally obtain the raw material of skinned mature silkworms, preparing for the subsequent acid hydrolysis step.

[0112] S2: Mix the raw material of skinned mature silkworms with an acidic solution at a mass ratio of 1:4. The selected acidic solution is a 2-molar per liter acetic acid solution. Heat the mixed mixture in a reactor to 60°C and maintain the reaction at this temperature for 4 hours to ensure that the acid hydrolysis reaction proceeds fully. After the reaction ends, cool the hydrolysis solution to room temperature to prepare for the subsequent filtration step.

[0113] S3: Transfer the cooled hydrolysis solution to a filter with a filter mesh aperture of 100 microns and perform preliminary filtration using the pressure filtration method. During the filtration process, control the filtration pressure at 0.2 MPa and set the filtration time at 30 minutes to effectively remove the solid impurities generated during the hydrolysis process. After filtration is completed, obtain a clear liquid containing silkworm protein, providing a pure basic liquid for the subsequent enzymatic hydrolysis treatment.

[0114] S4: Transfer the filtered hydrolysis solution to an enzymatic hydrolysis reactor and add cellulase at 2% of the mass of the hydrolysis solution. Adjust the reaction temperature to 55°C and maintain the reaction at this constant temperature for 6 hours to fully degrade the silkworm protein and improve its fibrillation performance. After the reaction ends, cool the enzymatic hydrolysis solution to room temperature to obtain the silkworm protein solution after enzymatic hydrolysis treatment.

[0115] S5: Mix the hydrolyzed silkworm protein solution with a 10 wt% polyvinyl alcohol solution at a mass ratio of 1:2. Adjust the temperature of the mixed solution to 30 °C and stir it on a mechanical stirrer at a speed of 500 revolutions per minute for 60 minutes to ensure that the two solutions are fully and evenly mixed, forming a stable mixed solution to provide a suitable fiber-forming medium for the spinning step.

[0116] S6: Spin the prepared mixed solution through a spinneret with a pore size of 0.5 mm, and control the spinning rate at 20 m / min. The spun solution is solidified by a coolant with a temperature controlled at 15 °C, and the cooling time is set at 5 seconds. Through this process, preliminary silkworm protein viscose fibers are formed, preparing for the subsequent physical property improvement steps.

[0117] S7: Place the cooled and solidified silkworm protein viscose fibers in a heating device, and set the heating temperature at 80 °C. At this temperature, stretch the fibers at a stretching speed of 5 times per minute along the fiber length direction to 4 times their original length while maintaining a constant stretching tension, with the tension controlled at 30 Newtons. After stretching, remove the fibers from the heating device and let them cool naturally to room temperature.

[0118] S8: Place the silkworm protein viscose fibers after thermal stretching treatment in a water washing device, add deionized water, and set the water washing temperature at 30 °C. During the water washing process, circulate the deionized water through the fibers at a constant flow rate of 2 liters per minute, and control the circulation time at 30 minutes to fully remove the excess solvent and impurities in the fibers. Subsequently, place the washed fibers in a drying device, set the drying temperature at 80 °C, and blow hot air through the fibers at a constant wind speed of 5 meters per second, with the drying time set at 4 hours to completely remove the moisture in the fibers. After drying, take out the fibers from the drying device to finally obtain high-quality silkworm protein viscose fiber products.

[0119] Comparative Example 1

[0120] Step 1: First, select high-quality silkworm cocoons as raw materials. Treat the collected cocoons in a steam environment at 80 °C for 30 minutes to soften the cocoons. Subsequently, place the softened cocoons in a 0.02 mol / L sodium carbonate solution and boil for 45 minutes to remove sericin (the sticky substance on the outer layer of fibroin), obtaining degummed fibroin.

[0121] Step 2: After thoroughly washing the degummed fibroin with deionized water, transfer it to a solution containing 9 mol / L ammonium sulfate. Stir the mixed solution at 60 °C for 4 hours to ensure that the fibroin is completely dissolved, forming a uniform fibroin solution.

[0122] Step 3: Pass the dissolved silk fibroin solution through a molecular sieve or membrane filtration device to remove undissolved impurities and macromolecular substances. This process is usually carried out at room temperature, with the filtration pressure controlled at 0.1 MPa and the filtration time about 30 minutes to obtain a pure silk fibroin solution;

[0123] Step 4: Extrude the purified silk fibroin solution through a spinneret with a diameter of 0.3 mm at a spinning rate of 10 m / min to form preliminary silk fibroin fibers;

[0124] Step 5: Place the preliminarily formed silk fibroin fibers in a drying device, set the drying temperature at 70 °C, and control the drying time within 2 hours to completely remove moisture and obtain the finished product of silkworm protein viscose fiber.

[0125] Table 1 Comparison of performance parameters of the finished product

[0126]

[0127]

[0128] Table 1 Explanation of performance indicators:

[0129] Tensile strength (MPa), the maximum stress that the fiber withstands during the stretching process. The higher the tensile strength, the stronger the durability and load-bearing capacity of the fiber;

[0130] Elongation at break (%), the maximum elongation percentage of the fiber before fracture. The higher the elongation at break, the better the ductility and toughness of the fiber;

[0131] Fiber diameter (μm), the average diameter of the fiber. A smaller diameter usually means a finer fiber texture;

[0132] Elastic modulus (GPa), an index of the rigidity of the fiber. The higher the elastic modulus, the better the elasticity of the fiber;

[0133] Moisture absorption rate (%), the ability of the fiber to absorb moisture. A moderate moisture absorption rate helps improve the comfort and breathability of the fiber;

[0134] Thermal stability (°C), the temperature at which the fiber maintains stable performance at high temperatures. The higher the thermal stability, the wider the applicability of the fiber in high-temperature environments;

[0135] Surface smoothness (score), a subjective score (1 - 10 points) for the smoothness of the fiber surface. The higher the score, the smoother the surface and the better the handfeel.

[0136] By comparing the performance of Example 1, Example 2, Example 3 and Comparative Example 1 in the seven performance indicators in Table 1 above, it can be seen that Example 1 is superior to other examples and Comparative Example 1 in terms of tensile strength, elongation at break, fiber diameter, elastic modulus, moisture absorption rate, thermal stability and surface smoothness, etc. This indicates that the process parameters and conditions adopted in Example 1 effectively improve the overall performance of the silkworm protein viscose fiber, making it have higher practical value and market competitiveness in textile and industrial applications.

[0137] Comparison of Other Performance Aspects of the Finished Product

[0138]

[0139]

[0140] Description of Performance Indicators in Table 2

[0141] Oil absorption rate (%), the ability of the fiber to absorb oil. The lower the oil absorption rate, the better the anti-pollution performance of the fiber in an oily environment.

[0142] Antibacterial activity (colony reduction rate %), the inhibitory effect of the fiber on bacteria, indicating the percentage reduction in the number of bacteria. The higher the antibacterial activity, the greater the application potential of the fiber in medical and hygienic products.

[0143] Air permeability (cm 3 / cm 2 ·s), the ability of the fiber to allow air to pass through, with the unit of cubic centimeters per square centimeter per second. The higher the air permeability, the better the comfort and breathability of the fiber.

[0144] Thermal conductivity (W / m·K), the ability of the fiber to conduct heat, with the unit of watts per meter kelvin. The lower the thermal conductivity, the better the heat insulation performance of the fiber.

[0145] Wear resistance (number of frictions), the number of times the fiber can withstand during the friction process, indicating its wear resistance. The higher the wear resistance, the longer the service life of the fiber.

[0146] Moisture retention rate (%), the ability of the fiber to retain moisture, indicating the percentage of moisture absorbed and retained by the fiber under certain conditions. An appropriate moisture retention rate helps to improve the comfort of the fiber.

[0147] Chromaticity (CIEL*a*b*), a quantitative representation of the color of the fiber, where L* represents brightness, a* represents the axis from green to red, and b* represents the axis from blue to yellow. The higher the chromaticity value, the more vivid the color, and the lower the value, the lighter the color.

[0148] By comparing the performance of Example 1, Example 2, Example 3 and Comparative Example 1 in the performance indicators through Table 2 above, especially in the seven performance indicators in Table 2, Example 1 performed excellently in terms of oil absorption rate, antibacterial activity, air permeability, thermal conductivity, abrasion resistance, moisture retention rate and chromaticity, etc., significantly better than other examples and Comparative Example 1; this indicates that the process parameters and conditions adopted in Example 1 not only improved the basic mechanical properties of the silkworm protein viscose fiber, but also demonstrated higher comprehensive performance in many aspects such as antibacterial property, air permeability and heat preservation property. Therefore, Example 1 was selected as the best example of the present invention, and the silkworm protein viscose fiber produced by it has excellent performance, is suitable for high-end textile, medical and health and other industrial fields, and has broad application prospects and market competitiveness.

[0149] The present invention covers any alternatives, modifications, equivalent methods and solutions made on the essence and scope of the present invention. In order to enable the public to have a thorough understanding of the present invention, specific details are described in detail in the following preferred embodiments of the present invention, and those skilled in the art can fully understand the present invention without the description of these details. In addition, well-known methods, processes, procedures, components and circuits, etc. are not described in detail in order to avoid unnecessary confusion to the essence of the present invention.

[0150] The above are only the preferred embodiments of the present invention. It should be pointed out that for those of ordinary skill in the art, without departing from the principle of the present invention, several improvements and refinements can be made, and these improvements and refinements should also be regarded as the protection scope of the present invention.

Claims

1. A method for producing silkworm protein viscose fiber using mature silkworms of the silkworm, characterized in that, It includes the following steps: S1: Select mature silkworms at the mature stage and perform molting treatment on them to obtain the molted mature silkworm raw materials; S2: Mix the molted mature silkworm raw materials with an acidic solution and carry out acid hydrolysis reaction at a predetermined temperature to obtain a hydrolysis solution; S3: Conduct preliminary filtration on the hydrolysis solution to remove the solid impurities generated during the hydrolysis process and obtain a liquid containing silkworm protein; S4: Carry out enzymatic hydrolysis treatment on the hydrolysis solution filtered in S3 to degrade the silkworm protein and improve its fibrillation performance; S5: Mix the enzymatically hydrolyzed silkworm protein solution with a polyvinyl alcohol solution to form a mixed solution; S6: Spin the mixed solution formed in S5 through a spinneret and solidify it through a coolant to form a preliminary silkworm protein viscose fiber; S7: Carry out hot stretching treatment on the cooled silkworm protein viscose fiber to improve the strength and elasticity of the fiber; S8: Wash the stretched silkworm protein viscose fiber and remove the excess moisture through drying to finally obtain the finished product of silkworm protein viscose fiber.

2. The method for producing silkworm protein viscose fiber using mature silkworms according to claim 1, characterized in that, The specific content of S1 includes: S11: Select mature silkworms at the mature stage, and the weight range of the selected mature silkworms is 0.2 g to 0.5 g; S12: Conduct preliminary cleaning on the selected mature silkworms to remove the surface impurities and dirt, and the cleaning solution is deionized water; S13: Immerse the cleaned mature silkworms in a molting solvent, and the molting solvent is chloroform or an alcohol solvent. The immersion time is 30 minutes to 60 minutes, and the immersion temperature is 20°C to 30°C. Remove the outer shell of the mature silkworms through the action of the solvent to obtain the molted mature silkworm raw materials.

3. A method for producing silkworm protein viscose fiber using mature silkworms according to claim 1, characterized in that, The specific content of S2 includes: S21: Mix the molted mature silkworm raw materials with an acidic solution. The acidic solution is hydrochloric acid solution, sulfuric acid solution or acetic acid solution, the concentration of the acid is 0.5 mol / L to 2 mol / L, and the mixing ratio is that the mass ratio of the molted mature silkworm raw materials to the acidic solution is 1:2 to 1:4; S22: Heat the mixed molted mature silkworm raw materials and acidic solution in a reactor, set the reaction temperature to 40°C to 60°C, and the reaction time to 2 hours to 4 hours; S23: After the reaction is completed, cool the hydrolysis solution to room temperature.

4. A method for producing silkworm protein viscose fiber using mature silkworms according to claim 1, characterized in that, The specific content of S3 includes: S31: Transfer the hydrolysis solution formed in S2 to a filtration device, and the filtration device is a filter with a filter mesh aperture of 50 μm to 100 μm; S32: Conduct preliminary filtration through the method of pressure filtration, the filtration pressure is 0.05 MPa to 0.2 MPa, and the filtration time is 10 minutes to 30 minutes to remove the solid impurities generated during the hydrolysis process.

5. A method for producing silkworm protein viscose fiber using mature silkworms according to claim 1, characterized in that, The specific content of S4 includes: S41: Transfer the hydrolysis solution filtered in S3 to an enzymatic hydrolysis reactor and add cellulase or protease, and the addition amount of the enzyme is 0.5% to 2% of the mass of the hydrolysis solution; S42: Adjust the reaction temperature to 45°C to 55°C and maintain a constant temperature reaction, and the reaction time is 4 hours to 6 hours to ensure that the enzymatic hydrolysis reaction proceeds fully; S43: After the reaction is completed, cool the enzymatic hydrolysis solution to room temperature to obtain the silkworm protein solution after enzymatic hydrolysis treatment.

6. The method for producing silkworm protein viscose fiber using mature silkworms according to claim 1, characterized in that, The specific content of S5 includes: S51: Mix the hydrolyzed silkworm protein solution with the polyvinyl alcohol solution at a mass ratio of 1:

2. The concentration of the polyvinyl alcohol solution is 5wt% to 10wt%. S52: Adjust the temperature of the mixture to 20°C to 30°C. Under stirring conditions, use a mechanical stirrer to stir at a speed of 200 rpm to 500 rpm for 30 minutes to 60 minutes to obtain a mixed solution.

7. A method for producing silkworm protein viscose fiber using mature silkworms according to claim 1, characterized in that, The specific steps of S6 are as follows: S61: Spin the mixed solution formed in S5 through a spinneret. The pore diameter of the spinneret is 0.2 mm to 0.5 mm, and the spinning rate is 5 m / min to 20 m / min. S62: Solidify the spun mixed solution with a coolant. The coolant is water, and the temperature of the coolant is controlled at 5°C to 15°C, and the cooling time is 1 second to 5 seconds. A preliminary silkworm protein viscose fiber is formed.

8. A method for producing silkworm protein viscose fiber using mature silkworms according to claim 1, characterized in that, The specific steps of S7 are as follows: S71: Conduct a hot stretching treatment on the cooled silkworm protein viscose fiber. The hot stretching treatment includes placing the fiber in a heating device and setting the stretching temperature at 60°C to 80°C. S72: At the set stretching temperature, stretch the fiber at a stretching speed of 1 times / minute to 5 times / minute. S73: Stretch the fiber along its length direction to 2 times to 4 times its original length. S74: During the stretching process, maintain a constant stretching tension, and the stretching tension is controlled at 10 N to 30 N. S75: After the stretching is completed, remove the fiber from the heating device and let it cool naturally to room temperature.

9. A method for producing silkworm protein viscose fiber using mature silkworms according to claim 1, characterized in that, The specific steps of S8 are as follows: S81: Place the stretched silkworm protein viscose fiber in a water washing device, add deionized water, and set the water washing temperature at 20°C to 30°C. S82: In the water washing device, circulate the deionized water through the silkworm protein viscose fiber at a constant flow rate. The constant flow rate is controlled at 0.5 L / min to 2 L / min, and the circulation time is 15 minutes to 30 minutes to fully remove the excess solvent and impurities in the fiber.

10. A method for producing silkworm protein viscose fiber using ripe silkworms of Bombyx mori, characterized in that, S8 also includes: S84: Place the water-washed silkworm protein viscose fiber in a drying device and set the drying temperature at 60°C to 80°C. S85: In the drying device, blow hot air over the silkworm protein viscose fiber at a constant wind speed. The constant wind speed is controlled at 2 m / s to 5 m / s, and the drying time is 2 hours to 4 hours to remove the excess moisture in the fiber. S86: After the drying is completed, take out the dried silkworm protein viscose fiber from the drying device to finally obtain the finished product of silkworm protein viscose fiber.

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