A kind of cordyceps protein fiber and preparation method thereof

Abstract

The present invention provides a cordyceps protein fiber and a preparation method thereof, belonging to the field of functional cellulose fiber preparation. Cordyceps protein liquid and viscose liquid are used as raw materials, and are prepared by blending, spinning, coagulation, curing and post-treatment; wherein, when blending, the mass proportion of protein in the cordyceps protein liquid is 1-40%, and the mass proportion of cellulose fiber in the viscose liquid is 60-99%; the finished product indicators of the cordyceps protein fiber are: dry breaking strength ≥2.06cN / dtex, wet breaking strength ≥1.00cN / dtex, dry breaking elongation 17±2.5%, protein content ≥2.3%. The cordyceps protein fiber involved has a soft and delicate feel, giving people a warm feeling; the fiber textile has good resilience, and the dimensional stability is significantly better than that of regenerated cellulose fiber, and has no sense of oppression on the skin, is skin-friendly and non-sticky, and can bring more functional product choices to consumers.

Description

Technical Field

[0001] The invention relates to cordyceps militaris protein fiber and a preparation method thereof, and belongs to the field of functional cellulose fiber preparation. Background Art

[0002] Regenerated cellulose fiber is a biodegradable material made from natural cellulose (such as cotton, linen, bamboo, trees, shrubs, etc.). The active hydroxyl groups in natural cellulose molecules are grafted and copolymerized with many functional molecules in different production links to achieve modification. Among them, without changing its chemical structure, only changing the physical structure of natural cellulose can produce regenerated cellulose fibers with better performance, such as good air permeability, good moisture absorption, good elasticity, soft, smooth and cool fabric feel, not easy to generate static electricity, with the softness of cotton, the luster of silk, and the smoothness of linen; easier to color, good color fastness and other characteristics.

[0003] Silkworm pupae are rich in protein and trace elements, and are important nutrients. They are mostly used to make feed or as the main raw material for nutrients. Silkworm pupa protein powder is made from silkworm pupa shells, which are obtained after crushing, impurity removal, dissolution, extraction, purification, drying and other processes. The fat content of the protein powder is ≤5%, and the protein content is ≥60%. Cordyceps militaris is rich in adenosine, cordycepin, cordyceps polysaccharides, etc., and is mixed with viscose spinning solution to prepare a new type of fiber. It is rich in amino acids and has antibacterial, anti-mite, anti-inflammatory, antiviral and other effects. This new fiber is a new functional fiber that can be completely degraded and is suitable for underwear, bedding, medical and sanitary materials, etc.

[0004] The prior art CN106381543A discloses the following main ingredients: viscose fiber, silkworm pupa powder, shell powder, aromatic polyamide, surfactant, adding aromatic polyamide as the main modifier to enhance fiber strength; adding shell powder and silkworm pupa powder allows the fabric to emit fragrance for a long time, and after washing 100 times, it can still emit a strong fragrance when worn close to the body for exercise, but its purpose is to obtain a high-strength viscose fiber. CN108867056A discloses that protein is firmly bound to cellulose through a cross-linking reaction, and bio-based fibers are modified to be firmly bound to various animal and plant proteins through grafting, thereby obtaining a natural, environmentally friendly, skin-friendly, comfortable, and completely degradable protein composite fiber. CN102304782A discloses a pupa protein viscose staple fiber and a method for manufacturing the same, but it uses a lot of chemical reagents and a complex process, resulting in high costs.

[0005] Therefore, there is an urgent need for a protein fiber preparation method that prevents protein loss and ensures stable performance of fiber textiles. Summary of the invention

[0006] The present invention aims to solve the problems of the prior art, and proposes a cordyceps protein fiber and a preparation method thereof. In this technical solution, the prepared cordyceps protein fiber feels soft and delicate, giving a warm feeling; the fiber textile has good resilience, and the dimensional stability is significantly better than that of regenerated cellulose fiber, and has no sense of pressure on the skin, is skin-friendly and non-sticky, and can bring more functional product choices to consumers; in addition, the preparation process involved is simple, low-cost, and can effectively prevent the loss of protein in the raw material, providing a first guarantee for the functionality of the final product cordyceps protein fiber.

[0007] In order to achieve the above technical objectives, the following technical solutions are proposed:

[0008] The first purpose of the technical scheme is: a cordyceps protein fiber, which is prepared by blending, spinning, coagulating, curing and post-treatment of cordyceps protein liquid and viscose liquid; wherein, during blending, the protein mass proportion in the cordyceps protein liquid is 1-40%, and the mass proportion of the fibrous material in the viscose liquid is 60-99%;

[0009] The finished product indicators of the Cordyceps militaris protein fiber are: dry breaking strength ≥2.06 cN / dtex, wet breaking strength ≥1.00 cN / dtex, dry breaking elongation 17±2.5%, and protein content ≥2.3%.

[0010] Furthermore, the cordyceps militaris protein liquid is prepared using silkworm pupa protein powder and cordyceps militaris extract as raw materials, wherein the silkworm pupa protein powder has a fat content of ≤5% and a protein content of ≥60%.

[0011] Furthermore, the viscose liquid has a methyl cellulose content of 8.5 to 9.2%.

[0012] The second purpose of the technical solution is: a method for preparing Cordyceps militaris protein fiber, comprising the following steps:

[0013] 1) Preparation of silkworm pupa protein solution

[0014] X1: Take silkworm pupa protein powder, wash it with 30-80℃ water to fully soak the silkworm pupa protein powder; add the surfactant (one or a mixture of two or more of dodecyl diethanolamide, polyoxyethylene fatty alcohol ether, polyoxyethylene alkylphenol ether and dodecyl alcohol amide phosphate), stir continuously, let it stand and settle, and remove the supernatant (which includes fat, ash and a small amount of dissolved protein);

[0015] Among them, this process is the pre-treatment process of silkworm pupa protein powder, which removes fat and ash and improves the purity of silkworm pupa protein powder. Water washing is mainly for degreasing and reducing fat and ash in protein powder. If there is too much fat in the silkworm pupa protein liquid, it will affect the subsequent processing, resulting in poor fiber forming, many broken ends, splitting, etc.; at the same time, it will also affect the use of equipment. In addition, water washing can make the silkworm pupa protein powder fully and evenly infiltrated, which is convenient for subsequent dissolution and reduces the phenomenon of powder agglomeration. Using 30-80℃ water washing can achieve a better degreasing effect. If it is lower than this temperature, the degreasing effect cannot be achieved; if it is higher than this temperature, part of the protein will be dissolved, resulting in protein loss. The water involved is deionized water without impurities and minerals.

[0016] The surfactant makes the fat emulsified and gathered on the surface as much as possible, which is convenient for removal from the surface. The amount of the surfactant added is 0.05-1.5% of the mass of the raw silkworm pupa protein powder, which ensures that the fat in the silkworm pupa protein powder is removed as much as possible and saves costs at the same time;

[0017] X2: Add water to the precipitate after removing the supernatant to prepare a protein solution with a mass fraction of 10-30%, and then heat it to 40-80°C; adjust the pH value to 8-14, and stir for 2-24 hours; wherein, caustic soda or other alkaline solution is used to adjust the pH;

[0018] This process is the dissolution process of silkworm pupa protein powder after pretreatment. Among them, the mass fraction of the protein solution is controlled to be 10-30% in order to facilitate subsequent mixing with viscose solution. If the mass fraction of the protein solution is too low, the mass of the viscose solution added is large, which will affect the spinning performance of the viscose; if the mass fraction of the protein solution is too high, its solubility is poor, and at the same time, the mass of the viscose solution added is small, and it is not easy to mix evenly. Control "heating to 40-80℃" to make the protein powder dissolve quickly and effectively, and at the same time, ensure the effective activity of the protein. If it is higher than this temperature, part of the protein will be denatured, resulting in waste of resources and affecting the subsequent cooling effect; if it is lower than this temperature, it will dissolve too slowly, take too long, and have low preparation efficiency. Control the "pH value to 8-14" to, first, speed up the dissolution of protein powder and ensure that the protein powder is fully dissolved; second, facilitate mixing with viscose solution. The viscose solution is alkaline. If the protein solution is acidic, the protein solution and the viscose solution will react into lumps, and the subsequent spinning will be seriously affected. The limit of "stirring for 2 to 24 hours" ensures that the protein powder is fully dissolved and the residue is reduced as much as possible, ensuring that subsequent spinning is easier to filter and reducing the phenomenon of filament separation and poor spinning formation during the production process;

[0019] X3: Use a centrifuge or filter to remove impurities from the protein solution to obtain silkworm pupa protein liquid. Further remove a small amount of protein and ash, and at the same time, ensure that the fat content in the silkworm pupa protein liquid is less than 1%;

[0020] 2) Preparation of Cordyceps militaris liquid

[0021] Y1: Take the Cordyceps militaris extract, dissolve it in ethanol with a temperature of 20-90°C and a concentration of 1-40%, filter and remove impurities to obtain a filtrate;

[0022] Among them, the mass fraction of Cordyceps militaris extract after dissolving in ethanol is 10-50%, which ensures that the Cordyceps militaris extract is fully dissolved. If the concentration is lower than this, the subsequent mixing amount of silkworm pupa protein liquid will be large, which will affect the subsequent mixing with viscose liquid; if the concentration is higher than this, the Cordyceps militaris extract has poor solubility, and mixing with silkworm pupa protein liquid and viscose liquid is easy to cause unevenness. The raw material Cordyceps militaris extract (mainly containing adenosine, cordycepin and cordyceps polysaccharide) involved can be purchased directly. Ethanol with a concentration of 1-40% is selected as the solvent. In order to fully dissolve the substances in the Cordyceps militaris extract and ensure the preparation cost at the same time, if solvent water is used, the dissolution effect is not good. The "temperature is 20-90℃". If it is higher than this temperature, it is not conducive to production operations, causing waste of resources and affecting subsequent cooling; if it is lower than this temperature, the dissolution will be too slow, the time will be too long, and the dissolution effect will be poor.

[0023] The purpose of filtering is to remove insoluble matter and impurities, so as to facilitate the subsequent mixing with the silkworm pupa protein solution, and after the Cordyceps militaris extract solution is mixed with the viscose solution, the filtering performance is better to ensure the smooth spinning;

[0024] Y2: adding a cross-linking agent (silane coupling agent) to the filtrate, stirring until the mixture is uniform, and obtaining a Cordyceps militaris liquid; wherein the amount of the silane coupling agent added is 0.5 to 5‰ of the total weight of the Cordyceps militaris extract;

[0025] Silane coupling agent improves the combination of protein and cellulose in the subsequent silkworm pupa protein liquid and reduces protein loss. The amount of silane coupling agent added is limited to 0.5-5‰ of the total weight of Cordyceps militaris extract to effectively ensure the cross-linking effect;

[0026] 3) Mix

[0027] The obtained Cordyceps militaris liquid and silkworm pupa protein liquid are mixed in a ratio of 1:1 to 10, and then 0.5 to 10% of a cross-linking agent acrylamide is added, mixed evenly, filtered to remove impurities, and the Cordyceps militaris protein liquid is obtained;

[0028] Among them, the Cordyceps militaris liquid and the silkworm pupa protein liquid are mixed in a ratio of 1:1 to 10. If the ratio here is too small, the concentration of the Cordyceps militaris protein liquid will be too low, and the amount added later will be too much, affecting the viscosity of the viscose liquid, thereby affecting the spinning effect; if the ratio is too large, the concentration will be too high, the solution will be viscous, which is not conducive to its dispersion in the viscose liquid, the filtration performance will be poor, and the subsequent spinning performance will be poor. In addition, the amount of cross-linking agent acrylamide added is controlled to be 0.5-10% to increase the combination between the Cordyceps militaris liquid and the silkworm pupa protein liquid, and reduce the subsequent loss in the viscose liquid and the spinning process;

[0029] 4) Blending

[0030] Degassing the obtained cordyceps protein liquid and viscose liquid separately, mixing them statically, and degassing them again to obtain a blended liquid;

[0031] In static mixing, the protein content in the cordyceps protein liquid is 1-40% by weight, and the methyl cellulose content in the viscose liquid is 60-99% by weight; wherein the viscose liquid is a viscose liquid with a methyl cellulose content of 8.5-9.2%;

[0032] The ratio between the cordyceps protein solution and the viscose solution is limited to ensure the functionality of the final product cordyceps protein fiber, and to ensure that the two are evenly mixed in the blending process while ensuring the subsequent spinning performance;

[0033] 5) Spinning

[0034] Two-bath wet spinning was used;

[0035] The blended liquid is sent to the spinning machine through the rubber supply pipeline, and is quantitatively fed by a metering pump. After the particle impurities are filtered out by a candle filter, the blended liquid is sent to the spinneret assembly through a curved tube. The blended liquid passes through the spinneret hole under pressure to form a thin stream of viscose;

[0036] 6) Solidification and curing

[0037] Solidification: The viscose thin stream is solidified in a solidification bath to form primary filaments;

[0038] The coagulation bath includes 250-360 g / L sodium sulfate, 80-130 g / L sulfuric acid, 10-50 g / L zinc sulfate and 8-25 g / L additives, the ratio of the coagulation bath to the viscose stream is 1.25-1.32, and the coagulation bath temperature is 40-60°C;

[0039] The limitation of the coagulation bath effectively prevents the loss of protein. In addition, the ratio of the coagulation bath to the viscose stream is controlled to be 1.25-1.32, and the coagulation bath temperature is controlled to be 40-60°C to ensure the formation of the viscose stream. Viscose spinning is an extremely intense process. Here, the limitation of the coagulation bath temperature is to ensure that the forming process is not too intense, to ensure the fiber forming, and to facilitate the CS produced in the reaction process to be formed. 2 Can be recycled as much as possible. As the temperature rises, the decomposition reaction of cellulose sulfonate will be accelerated. Too fast a reaction will lead to inadequate molding. At the same time, it will also cause the added protein and Cordyceps militaris extract to not be effectively retained on the fiber, resulting in a large loss of effective substances, and thus the quality of the finished fiber cannot be guaranteed;

[0040] Curing: After the primary filaments pass through the guide disc, they are bundled and stretched in the curing bath. In the curing bath, the primary filaments are stretched and the decomposition and regeneration process is completed. The structure and performance of the fibers are finalized and stabilized, and a fiber bundle is obtained.

[0041] 7) Post-processing

[0042] The obtained fiber bundle is cut, and after primary acid washing, desulfurization, primary water washing, secondary acid washing, secondary water washing, oiling, dehydration and drying, a finished cordyceps protein fiber is obtained.

[0043] In the present technical scheme, the Cordyceps militaris extract involved is directly purchased and obtained, which mainly contains adenosine, cordycepin, polysaccharides, rich selenium (Se) and other substances, among which adenosine has antiviral and antibacterial effects, prevents and treats cerebral thrombosis and cerebral hemorrhage, inhibits platelet accumulation to prevent thrombosis, eliminates facial spots, and resists aging and wrinkles. The cordycepin content in Cordyceps militaris is 0.05-.51%. Cordyceps militaris contains cordycepin in both its fruiting bodies and insect bodies. In Cordyceps militaris from different sources, the distribution of cordycepin in its fruiting bodies and insect bodies is significantly different. Cordycepin is 3'-deoxyadenosine, which is a nucleic acid derivative of nitrogen-containing glycosides, belongs to purine alkaloids, and is a nucleoside antibiotic. So far, the pharmacological effects of cordycepin reported at home and abroad mainly include: inhibiting microbial growth, anti-tumor, immunomodulation, anti-inflammatory, etc. Cordyceps militaris polysaccharides have biological activities, including anti-inflammatory effects, antioxidant activity, etc. Cordyceps militaris is also rich in selenium (Se), which is recognized as an essential trace element for the human body. It is the active center of glutathione peroxidase and is connected to the peptide chain of the enzyme protein in the form of selenocysteine, protecting the stability and normal permeability of the cell membrane, stimulating the production of immunoglobulins and antibodies, and enhancing the body's immune and antioxidant capabilities. At the same time, a large number of scientific practices have proved that selenium can significantly inhibit the growth of cancer cells.

[0044] In the present technical solution, the silkworm pupa protein powder is purchased directly, and is obtained by grinding, removing impurities, dissolving, extracting, purifying, and drying silkworm pupa shells, wherein the fat content of the protein powder is ≤5%, and the protein content is ≥60%.

[0045] The beneficial technical effects brought about by adopting this technical solution are:

[0046] 1. In the present invention, the cordyceps protein fiber is light yellow, soft and delicate to the touch, giving a warm feeling; the fiber textile has good resilience, and the dimensional stability is significantly better than that of regenerated cellulose fiber, and it has no sense of oppression on the skin, is skin-friendly and non-sticky. Cordyceps protein fiber is rich in polar groups such as amino and carboxyl groups, has good acid-base neutralization effect, and has excellent antibacterial properties, and is skin-friendly and close to the skin; in addition, the cordyceps protein fiber has good anti-mite and antiviral properties;

[0047] Second, in the preparation process of the Cordyceps militaris liquid of the present invention, the use of a silane coupling agent can increase the binding between protein and cellulose in subsequent processes and reduce protein loss;

[0048] 3. In the mixing process of the present invention, acrylamide is used as a cross-linking agent between Cordyceps militaris and silkworm pupa protein to increase the combination of the two, reduce waste and loss, and ensure the retention amount of the subsequent product - Cordyceps militaris protein fiber. BRIEF DESCRIPTION OF THE DRAWINGS

[0049] Figure 1 This is a cross-sectional view of the finished product of Cordyceps militaris protein fiber in Example 8. DETAILED DESCRIPTION

[0050] The following is a clear and complete description of the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0051] Example 1

[0052] This embodiment provides: a cordyceps protein fiber, which is prepared by blending, spinning, coagulating, curing and post-processing cordyceps protein liquid and viscose liquid as raw materials; wherein, during blending, the protein mass proportion in the cordyceps protein liquid is 1%, and the mass proportion of the acetal fiber in the viscose liquid is 99%. The cordyceps protein liquid is prepared by using silkworm pupa protein powder and cordyceps extract as raw materials, and the fat content in the silkworm pupa protein powder is ≤5%, and the protein content is ≥60%. And the viscose liquid is a viscose liquid with an acetal fiber content of 8.5%.

[0053] The finished product indicators of the Cordyceps militaris protein fiber are: dry breaking strength ≥2.06 cN / dtex, wet breaking strength ≥1.00 cN / dtex, dry breaking elongation 17±2.5%, and protein content ≥2.3%.

[0054] Example 2

[0055] The present embodiment provides: a cordyceps protein fiber, which is prepared by blending, spinning, coagulating, curing and post-processing cordyceps protein liquid and viscose liquid as raw materials; wherein, during blending, the protein mass proportion in the cordyceps protein liquid is 40%, and the mass proportion of the acetyl fiber in the viscose liquid is 60%. The cordyceps protein liquid is prepared by using silkworm pupa protein powder and cordyceps extract as raw materials, wherein the fat content in the silkworm pupa protein powder is ≤3%, and the protein content is ≥60%; the viscose liquid is a viscose liquid with an acetyl fiber content of 9.2%.

[0056] The finished product indicators of the Cordyceps militaris protein fiber are: dry breaking strength ≥2.06 cN / dtex, wet breaking strength ≥1.00 cN / dtex, dry breaking elongation 17±2.5%, and protein content ≥2.3%.

[0057] Example 3

[0058] This embodiment provides: a cordyceps protein fiber, which is prepared by blending, spinning, coagulating, curing and post-processing cordyceps protein liquid and viscose liquid as raw materials; wherein, during blending, the protein mass proportion in the cordyceps protein liquid is 15%, and the mass proportion of the acetyl fiber in the viscose liquid is 85%. The cordyceps protein liquid is prepared by using silkworm pupa protein powder and cordyceps extract as raw materials, wherein the fat content in the silkworm pupa protein powder is ≤2%, and the protein content is ≥60%; the viscose liquid is a viscose liquid with an acetyl fiber content of 8.9%.

[0059] The finished product indicators of the Cordyceps militaris protein fiber are: dry breaking strength ≥2.06 cN / dtex, wet breaking strength ≥1.00 cN / dtex, dry breaking elongation 17±2.5%, and protein content ≥2.3%.

[0060] Example 4

[0061] This embodiment provides: a cordyceps protein fiber, which is prepared by blending, spinning, coagulating, curing and post-processing cordyceps protein liquid and viscose liquid as raw materials; wherein, during blending, the protein mass proportion in the cordyceps protein liquid is 35%, and the mass proportion of the acetyl fiber in the viscose liquid is 65%. The cordyceps protein liquid is prepared by using silkworm pupa protein powder and cordyceps extract as raw materials, wherein the fat content in the silkworm pupa protein powder is ≤5%, and the protein content is ≥60%; the viscose liquid is a viscose liquid with an acetyl fiber content of 9.0%.

[0062] The finished product indicators of the Cordyceps militaris protein fiber are: dry breaking strength ≥2.06 cN / dtex, wet breaking strength ≥1.00 cN / dtex, dry breaking elongation 17±2.5%, and protein content ≥2.3%.

[0063] Example 5

[0064] This embodiment provides: a method for preparing Cordyceps militaris protein fiber, comprising the following steps:

[0065] 1) Preparation of silkworm pupa protein solution

[0066] X1: Take silkworm pupa protein powder, wash it with 30℃ water to fully soak the silkworm pupa protein powder; add dodecyl diethanolamide and continue stirring, let it stand and settle, and remove the supernatant;

[0067] X2: Add water to the precipitate after removing the supernatant to prepare a 30% protein solution by mass, then heat to 80°C; adjust the pH value to 14 and stir for 24 hours; wherein, caustic soda or other alkaline solution is used to adjust the pH;

[0068] X3: Use a centrifuge or filter to remove impurities from the protein solution to obtain silkworm pupa protein solution;

[0069] 2) Preparation of Cordyceps militaris liquid

[0070] Y1: Take the Cordyceps militaris extract, dissolve it in 40% ethanol at a temperature of 90°C, filter and remove impurities to obtain a filtrate;

[0071] Among them, the mass fraction of Cordyceps militaris extract dissolved in ethanol is 50%;

[0072] Y2: Add silane coupling agent and auxiliary agent to the filtrate, stir until mixed evenly, and obtain Cordyceps militaris liquid;

[0073] 3) Mix

[0074] The obtained Cordyceps militaris liquid and silkworm pupa protein liquid are mixed in a ratio of 1:10, and then 10% acrylamide is added, mixed evenly, filtered to remove impurities, and the Cordyceps militaris protein liquid is obtained;

[0075] 4) Blending

[0076] Degassing the obtained cordyceps protein liquid and viscose liquid separately, mixing them statically, and degassing them again to obtain a blended liquid;

[0077] In static mixing, the protein mass in the cordyceps protein liquid accounts for 39%, and the acetone mass in the viscose liquid accounts for 51%; among which, the viscose liquid is a viscose liquid with an acetone content of 9.1%;

[0078] 5) Spinning

[0079] Two-bath wet spinning was used;

[0080] The blended liquid is sent to the spinning machine through the rubber supply pipeline, and is quantitatively fed by a metering pump. After the particle impurities are filtered out by a candle filter, the blended liquid is sent to the spinneret assembly through a curved tube. The blended liquid passes through the spinneret hole under pressure to form a thin stream of viscose;

[0081] 6) Solidification and curing

[0082] Solidification: The viscose thin stream is solidified in a solidification bath to form primary filaments;

[0083] The coagulation bath includes 360 g / L sodium sulfate, 130 g / L sulfuric acid, 50 g / L zinc sulfate and 25 g / L additives, the specific gravity of the coagulation bath to the viscose stream is 1.32, and the coagulation bath temperature is 60°C;

[0084] Curing: After the primary filaments pass through the guide disc, they are bundled and stretched in the curing bath. In the curing bath, the primary filaments are stretched and the decomposition and regeneration process is completed. The structure and performance of the fibers are finalized and stabilized, and a fiber bundle is obtained.

[0085] 7) Post-processing

[0086] The obtained fiber bundle is cut, and after primary acid washing, desulfurization, primary water washing, secondary acid washing, secondary water washing, oiling, dehydration and drying, a finished cordyceps protein fiber is obtained.

[0087] Example 6

[0088] This embodiment provides: a method for preparing Cordyceps militaris protein fiber, comprising the following steps:

[0089] 1) Preparation of silkworm pupa protein solution

[0090] X1: Take silkworm pupa protein powder, wash it with 80℃ water to fully soak the silkworm pupa protein powder; add a mixture of polyoxyethylene fatty alcohol ether, polyoxyethylene alkylphenol ether and dodecyl alcohol amide phosphate, continue stirring, let it stand and settle, and remove the supernatant;

[0091] X2: Add water to the precipitate after removing the supernatant to prepare a 10% protein solution, then heat to 40°C; adjust the pH to 8 and stir for 2 hours; wherein, caustic soda or other alkaline solution is used to adjust the pH;

[0092] X3: Use a centrifuge or filter to remove impurities from the protein solution to obtain silkworm pupa protein solution;

[0093] 2) Preparation of Cordyceps militaris liquid

[0094] Y1: Take the Cordyceps militaris extract, dissolve it in ethanol with a temperature of 20°C and a concentration of 1-40%, filter and remove impurities to obtain a filtrate;

[0095] Among them, the mass fraction of Cordyceps militaris extract dissolved in ethanol is 10%;

[0096] Y2: Add silane coupling agent and auxiliary agent to the filtrate, stir until mixed evenly, and obtain Cordyceps militaris liquid;

[0097] 3) Mix

[0098] The obtained Cordyceps militaris liquid and silkworm pupa protein liquid are mixed in a ratio of 1:5, and then 0.5% acrylamide is added, mixed evenly, filtered to remove impurities, and the Cordyceps militaris protein liquid is obtained;

[0099] 4) Blending

[0100] Degassing the obtained cordyceps protein liquid and viscose liquid separately, mixing them statically, and degassing them again to obtain a blended liquid;

[0101] In static mixing, the protein mass in the cordyceps protein liquid accounts for 10%, and the acetone mass in the viscose liquid accounts for 90%; among which, the viscose liquid is a viscose liquid with an acetone content of 8.8%;

[0102] 5) Spinning

[0103] Two-bath wet spinning was used;

[0104] The blended liquid is sent to the spinning machine through the rubber supply pipeline, and is quantitatively fed by a metering pump. After the particle impurities are filtered out by a candle filter, the blended liquid is sent to the spinneret assembly through a curved tube. The blended liquid passes through the spinneret hole under pressure to form a thin stream of viscose;

[0105] 6) Solidification and curing

[0106] Solidification: The viscose thin stream is solidified in a solidification bath to form primary filaments;

[0107] The coagulation bath includes 250 g / L sodium sulfate, 80 g / L sulfuric acid, 10 g / L zinc sulfate and 8 g / L additives, the ratio of the coagulation bath to the viscose stream is 1.25, and the coagulation bath temperature is 40°C;

[0108] Curing: After the primary filaments pass through the guide disc, they are bundled and stretched in the curing bath. In the curing bath, the primary filaments are stretched and the decomposition and regeneration process is completed. The structure and performance of the fibers are finalized and stabilized, and a fiber bundle is obtained.

[0109] 7) Post-processing

[0110] The obtained fiber bundle is cut, and after primary acid washing, desulfurization, primary water washing, secondary acid washing, secondary water washing, oiling, dehydration and drying, a finished cordyceps protein fiber is obtained.

[0111] Example 7

[0112] This embodiment provides: a method for preparing Cordyceps militaris protein fiber, comprising the following steps:

[0113] 1) Preparation of silkworm pupa protein solution

[0114] X1: Take silkworm pupa protein powder, wash it with 50℃ water to fully soak the silkworm pupa protein powder; add dodecyl alcohol amide phosphate, continue stirring, let it stand and settle, and remove the supernatant;

[0115] X2: Add water to the precipitate after removing the supernatant to prepare a 20% protein solution, then heat to 60°C; adjust the pH to 10 and stir for 16 hours; wherein, caustic soda or other alkaline solution is used to adjust the pH;

[0116] X3: Use a centrifuge or filter to remove impurities from the protein solution to obtain silkworm pupa protein solution;

[0117] 2) Preparation of Cordyceps militaris liquid

[0118] Y1: Take the Cordyceps militaris extract, dissolve it in ethanol at a temperature of 60°C and a concentration of 25%, filter and remove impurities to obtain a filtrate;

[0119] Among them, the mass fraction of Cordyceps militaris extract after being dissolved in ethanol is 35%;

[0120] Y2: Add silane coupling agent and auxiliary agent to the filtrate, stir until mixed evenly, and obtain Cordyceps militaris liquid;

[0121] 3) Mix

[0122] The obtained Cordyceps militaris liquid and silkworm pupa protein liquid are mixed in a ratio of 1:8, and then 5% acrylamide is added, mixed evenly, filtered to remove impurities, and the Cordyceps militaris protein liquid is obtained;

[0123] 4) Blending

[0124] Degassing the obtained cordyceps protein liquid and viscose liquid separately, mixing them statically, and degassing them again to obtain a blended liquid;

[0125] In static mixing, the protein mass in the cordyceps protein liquid accounts for 28%, and the acetone mass in the viscose liquid accounts for 72%; among which, the viscose liquid is a viscose liquid with an acetone content of 9.1%;

[0126] 5) Spinning

[0127] Two-bath wet spinning was used;

[0128] The blended liquid is sent to the spinning machine through the rubber supply pipeline, and is quantitatively fed by a metering pump. After the particle impurities are filtered out by a candle filter, the blended liquid is sent to the spinneret assembly through a curved tube. The blended liquid passes through the spinneret hole under pressure to form a thin stream of viscose;

[0129] 6) Solidification and curing

[0130] Solidification: The viscose thin stream is solidified in a solidification bath to form primary filaments;

[0131] The coagulation bath includes 320 g / L sodium sulfate, 110 g / L sulfuric acid, 48 g / L zinc sulfate and 16 g / L additives, the ratio of the coagulation bath to the viscose stream is 1.30, and the coagulation bath temperature is 50°C;

[0132] Curing: After the primary filaments pass through the guide disc, they are bundled and stretched in the curing bath. In the curing bath, the primary filaments are stretched and the decomposition and regeneration process is completed. The structure and performance of the fibers are finalized and stabilized, and a fiber bundle is obtained.

[0133] 7) Post-processing

[0134] The obtained fiber bundle is cut, and after primary acid washing, desulfurization, primary water washing, secondary acid washing, secondary water washing, oiling, dehydration and drying, a finished cordyceps protein fiber is obtained.

[0135] Example 8

[0136] This embodiment takes the production of 600g of Cordyceps militaris protein fiber finished product as an example to further illustrate the technical solution. The process includes the following steps:

[0137] 1) Preparation of silkworm pupa protein solution

[0138] X1: Take silkworm pupa protein powder, wash it with 45℃ water to fully soak the silkworm pupa protein powder; add dodecyl diethanolamide and polyoxyethylene fatty alcohol ether (1% of the powder), and continue stirring, then let it stand and settle, and remove the supernatant;

[0139] X2: Add water to the washed protein powder at a ratio of 30% of the final mass fraction, heat to 70°C, adjust the pH value to 11, and stir for 4 hours; caustic soda is used to adjust the pH;

[0140] X3: Use a centrifuge to remove impurities from the solution to obtain silkworm pupa protein solution;

[0141] 2) Preparation of Cordyceps militaris liquid

[0142] Y1: Take the Cordyceps militaris extract, dissolve it in 20% ethanol at a temperature of 60°C, and filter it to obtain a filtrate;

[0143] Among them, the mass fraction of Cordyceps militaris extract after being dissolved in ethanol is 30%;

[0144] Y2: Add silane coupling agent to the filtrate and stir until the mixture is uniform to obtain Cordyceps militaris liquid;

[0145] Among them, the mass fraction of silane coupling agent added is 2.5‰.

[0146] 3) Mix

[0147] The obtained Cordyceps militaris liquid and silkworm pupa protein liquid are mixed in a ratio of 1:5, 4% acrylamide is added, the mixture is mixed evenly, and the mixture is filtered to obtain the Cordyceps militaris protein liquid;

[0148] 4) Blending

[0149] Degassing the obtained cordyceps protein liquid and viscose liquid separately, mixing them statically, and degassing them again to obtain a blended liquid;

[0150] In static mixing, the protein content in the cordyceps protein liquid is 8% by weight, and the acetone content in the viscose liquid is 92% by weight; among them, the viscose liquid is a viscose liquid with an acetone content of 8.9%;

[0151] 5) Spinning

[0152] Two-bath wet spinning was used;

[0153] The blended liquid is sent to the spinning machine through the glue supply pipeline, and is quantitatively fed by a metering pump. After the particle impurities are filtered out by a candle filter, the blended liquid is sent to the spinneret assembly through a curved pipe. The blended liquid passes through the spinneret hole under pressure to form a thin stream of viscose;

[0154] 6) Solidification and curing

[0155] Solidification: The viscose thin stream is solidified in a solidification bath to form primary filaments;

[0156] The coagulation bath includes 250-360 g / L sodium sulfate, 80-130 g / L sulfuric acid, and 10-50 g / L zinc sulfate, the ratio of the coagulation bath to the viscose stream is 1.25-1.32, and the coagulation bath temperature is 40-60°C;

[0157] Curing: After the primary filaments pass through the guide disc, they are bundled and stretched in the curing bath. In the curing bath, the primary filaments are stretched and the decomposition and regeneration process is completed. The structure and performance of the fibers are finalized and stabilized, and a fiber bundle is obtained.

[0158] 7) Post-processing

[0159] The obtained fiber bundle is cut, and after primary acid washing, desulfurization, primary water washing, secondary acid washing, secondary water washing, oiling, dehydration and drying, a finished cordyceps protein fiber is obtained.

[0160] In addition, the obtained Cordyceps militaris protein fiber finished product was cross-sectioned, and the obtained results were as follows: Figure 1 In the cross-sectional view of the finished product of Cordyceps militaris protein fiber, it can be seen that there is protein in the viscose core layer.

[0161] Comparative Example 1

[0162] Based on Example 8, the difference between this comparative example 1 and Example 8 is that the active agent dodecyl diethanolamide, polyoxyethylene fatty alcohol ether, polyoxyethylene alkylphenol ether and dodecyl alcohol amide phosphate are not used, and the rest is the same as Example 8. The results are shown in Table 1.

[0163] Comparative Example 2

[0164] Based on Example 8, the difference between this comparative example 2 and Example 8 is that in step Y2, no crosslinking agent (silane coupling agent) is added to the filtrate, and the rest is the same as Example 8. The results are shown in Table 1.

[0165] Comparative Example 3

[0166] Based on Example 8, the difference between this comparative example 3 and Example 8 is that no crosslinking agent acrylamide is added in the mixing process of step 3), and the rest is the same as Example 8. The obtained results are shown in Table 1.

[0167]

[0168] The above description is only a preferred embodiment of the present invention and does not limit the present invention in any form. Any simple modification or equivalent change made to the above embodiment based on the technical essence of the present invention shall fall within the protection scope of the present invention.

Claims

1. A Cordyceps militaris protein fiber, characterized in that: The product is prepared by using Cordyceps militaris protein liquid and viscose liquid as raw materials, through blending, spinning, coagulation, solidification and post-treatment; during blending, the protein mass proportion in the Cordyceps militaris protein liquid is 1-40%; The cordyceps militaris protein liquid is prepared using silkworm pupa protein powder and cordyceps militaris extract as raw materials, wherein the silkworm pupa protein powder has a fat content of ≤5% and a protein content of ≥60%; the viscose liquid is a viscose liquid with a methylcellulose content of 8.5-9.2%; The finished product indicators of the Cordyceps militaris protein fiber are: dry breaking strength ≥ 2.06 cN / dtex, wet breaking strength ≥ 1.00 cN / dtex, dry breaking elongation 17±2.5%, protein content ≥ 2.3%; The preparation method of the cordyceps militaris protein fiber comprises the following steps: 1) Preparation of silkworm pupa protein solution X1: Take silkworm pupa protein powder, wash with 30-80℃ water; add active agent, stir continuously, let stand to settle, and remove supernatant; The active agent is one or a mixture of two or more of dodecyl diethanolamide, polyoxyethylene fatty alcohol ether, polyoxyethylene alkylphenol ether and dodecyl alcohol amide phosphate; X2: Add water to the precipitate after removing the supernatant to prepare a protein solution with a mass fraction of 10-30%, then heat to 40-80°C; adjust the pH value to 8-14, and stir for 2-24 hours; X3: removing impurities from the protein solution to obtain silkworm pupa protein solution; 2) Preparation of Cordyceps militaris liquid Y1: Take the Cordyceps militaris extract, dissolve it in ethanol with a temperature of 20-90°C and a concentration of 1-40%, filter it, and obtain a filtrate; Y2: Add silane coupling agent to the filtrate and stir until the mixture is uniform to obtain Cordyceps militaris liquid; 3) Mix The obtained Cordyceps militaris liquid and silkworm pupa protein liquid are mixed in a ratio of 1:1 to 10, and then 0.5 to 10% of acrylamide is added, mixed evenly, and filtered to obtain the Cordyceps militaris protein liquid; 4) Blending Degassing the obtained cordyceps protein liquid and viscose liquid separately, mixing them statically, and degassing them again to obtain a blended liquid; In static mixing, the protein mass percentage in the Cordyceps militaris protein liquid is 1 to 40%; 5) Spinning Two-bath wet spinning was used; The blended liquid is sent to the spinning machine through the glue supply pipeline, and is quantitatively fed by a metering pump. After the particle impurities are filtered out by a candle filter, the blended liquid is sent to the spinneret assembly through a curved pipe. The blended liquid passes through the spinneret hole under pressure to form a thin stream of viscose; 6) Solidification and curing The viscose thin stream is solidified in a coagulation bath, the ratio of the coagulation bath to the viscose thin stream is 1.25-1.32, and the coagulation bath temperature is 40-60°C, to obtain primary filaments; After the primary filaments pass through the guide disc, they are bundled and stretched in a curing bath; in the curing bath, the primary filaments are stretched and the decomposition and regeneration process is completed, wherein the structure and performance of the fibers are finalized and stabilized, and a fiber bundle is obtained; 7) Post-processing The obtained fiber bundle is cut, and after primary acid washing, desulfurization, primary water washing, secondary acid washing, secondary water washing, oiling, dehydration and drying, a finished cordyceps protein fiber is obtained.

2. The Cordyceps militaris protein fiber according to claim 1, characterized in that: The amount of the active agent added is 0.05-1.5% of the mass of the silkworm pupa protein powder.

3. The Cordyceps militaris protein fiber according to claim 1, characterized in that: In step X3, impurities are removed by using a centrifuge or a filter.

4. The Cordyceps militaris protein fiber according to claim 1, characterized in that: In step Y1, the mass fraction of the Cordyceps militaris extract after being dissolved in ethanol is 10 to 50%.

5. The Cordyceps militaris protein fiber according to claim 1, characterized in that: In step Y2, the amount of silane coupling agent added is 0.5 to 5‰ of the total weight of the Cordyceps militaris extract.

6. The Cordyceps militaris protein fiber according to claim 1, characterized in that: In step 6), the coagulation bath includes 250-360 g / L sodium sulfate, 80-130 g / L sulfuric acid, 10-50 g / L zinc sulfate and 8-25 g / L auxiliary agent.

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