CN116446064A - Cordyceps militaris protein fiber and preparation method thereof - Google Patents
Cordyceps militaris protein fiber and preparation method thereof Download PDFInfo
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- CN116446064A CN116446064A CN202211705588.1A CN202211705588A CN116446064A CN 116446064 A CN116446064 A CN 116446064A CN 202211705588 A CN202211705588 A CN 202211705588A CN 116446064 A CN116446064 A CN 116446064A
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- cordyceps militaris
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- 102000004169 proteins and genes Human genes 0.000 title claims abstract description 188
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- 239000000835 fiber Substances 0.000 title claims abstract description 112
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
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- 230000001112 coagulating effect Effects 0.000 claims description 25
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- OFEZSBMBBKLLBJ-BAJZRUMYSA-N cordycepin Chemical compound C1=NC=2C(N)=NC=NC=2N1[C@@H]1O[C@H](CO)C[C@H]1O OFEZSBMBBKLLBJ-BAJZRUMYSA-N 0.000 description 9
- OFEZSBMBBKLLBJ-UHFFFAOYSA-N cordycepine Natural products C1=NC=2C(N)=NC=NC=2N1C1OC(CO)CC1O OFEZSBMBBKLLBJ-UHFFFAOYSA-N 0.000 description 9
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- VEVVRTWXUIWDAW-UHFFFAOYSA-N dodecan-1-amine;phosphoric acid Chemical compound OP(O)(O)=O.CCCCCCCCCCCCN VEVVRTWXUIWDAW-UHFFFAOYSA-N 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
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- HKJIIHGOQMKEAV-UHFFFAOYSA-N methanol;prop-2-enamide Chemical compound OC.NC(=O)C=C HKJIIHGOQMKEAV-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
- D01F2/06—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from viscose
- D01F2/08—Composition of the spinning solution or the bath
- D01F2/10—Addition to the spinning solution or spinning bath of substances which exert their effect equally well in either
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
- Y02P70/62—Manufacturing or production processes characterised by the final manufactured product related technologies for production or treatment of textile or flexible materials or products thereof, including footwear
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Artificial Filaments (AREA)
Abstract
The invention provides cordyceps militaris protein fiber and a preparation method thereof, and belongs to the field of functional cellulose fiber preparation. The cordyceps militaris protein liquid and the viscose are used as raw materials and are prepared through blending, spinning, solidification and post-treatment; wherein, during blending, the mass ratio of protein in the cordyceps militaris protein liquid is 1-40%, and the mass ratio of alpha-fiber in the viscose liquid is 60-99%; the finished product indexes of the cordyceps militaris protein fiber are as follows: the dry breaking strength is more than or equal to 2.06cN/dtex, the wet breaking strength is more than or equal to 1.00cN/dtex, the dry breaking elongation is 17+/-2.5%, and the protein content is more than or equal to 2.3%. The related cordyceps militaris protein fiber has soft and fine handfeel and gives people warm feel; the fiber textile has good rebound resilience, the dimensional stability is obviously better than that of regenerated cellulose fiber, the fiber textile has no oppression to skin and is skin-friendly and non-sticky, and more functional product choices can be brought to consumers.
Description
Technical Field
The invention relates to cordyceps militaris protein fiber and a preparation method thereof, and belongs to the field of functional cellulose fiber preparation.
Background
The regenerated cellulose fiber is a degradable material which takes natural cellulose (such as cotton, hemp, bamboo, tree, shrub and the like) as a raw material, and active hydroxyl groups in natural cellulose molecules and a plurality of functional molecules are subjected to graft copolymerization in different production links to realize modification. Wherein, the regenerated cellulose fiber with better performance can be manufactured by only changing the physical structure of the natural cellulose without changing the chemical structure, such as: the fabric has good air permeability, good hygroscopicity, good elasticity, soft, smooth and cool hand feeling, is not easy to generate static electricity, and has soft cotton, luster of silk and smoothness of hemp; more easy to color, good color fastness and the like.
Silkworm chrysalis is rich in proteins and microelements, is an important nutritional product, and is mostly used for manufacturing feed or as a main raw material of nutritional products. The silkworm chrysalis protein powder is prepared by taking silkworm chrysalis shells as raw materials and performing the procedures of crushing, impurity removal, dissolution, extraction, purification, drying and the like, wherein the fat content of the protein powder is less than or equal to 5 percent, and the protein content is more than or equal to 60 percent. Cordyceps militaris is rich in adenosine, cordycepin, cordyceps polysaccharide and the like, and is mixed with viscose spinning solution to prepare novel fiber which is rich in amino acid, antibacterial, anti-mite, anti-inflammatory and antiviral effects.
The prior art CN106381543a discloses that the following main components are included: viscose fiber, silkworm chrysalis meal, shell powder, aromatic polyamide and surfactant, wherein the aromatic polyamide is added as a main modifier for enhancing the strength of the fiber; the shell powder and the silkworm chrysalis powder are added, so that the fabric can permanently emit fragrance, and after being washed for 100 times, the fabric can still emit intense fragrance after being worn next to the skin, but the aim is to obtain the high-strength viscose fiber. CN108867056a discloses that protein is firmly bound on cellulose through a crosslinking reaction, so that the bio-based fiber is modified to be firmly bound with various animal and plant proteins through grafting, and a natural, environment-friendly, skin-friendly, comfortable and completely degradable protein composite fiber is obtained. CN102304782a discloses a kind of pupa protein viscose staple fibre and its manufacturing method, but its used chemical reagents are many, and the process is complex, resulting in high cost.
Therefore, a protein fiber preparation method for preventing protein loss and ensuring stable performance of fiber textiles is urgently needed.
Disclosure of Invention
The invention aims to solve the problems in the prior art, and provides cordyceps militaris protein fibers and a preparation method thereof. In the technical scheme, the prepared cordyceps militaris protein fiber has soft and fine handfeel and gives people warm feeling; the fiber textile has good rebound resilience, the dimensional stability is obviously better than that of regenerated cellulose fiber, the fiber textile has no oppression to skin and is skin-friendly and non-sticky, and more functional product choices can be brought to consumers; in addition, the related preparation process is simple, the cost is low, the loss of protein in the raw materials can be effectively prevented, and the prior guarantee is provided for the functionality of the cordyceps militaris protein fiber as a final product.
In order to achieve the technical purpose, the following technical scheme is provided:
the first purpose of the technical scheme is that: the cordyceps militaris protein fiber is prepared by taking cordyceps militaris protein liquid and viscose liquid as raw materials and carrying out blending, spinning, solidification and post-treatment; wherein, during blending, the mass ratio of protein in the cordyceps militaris protein liquid is 1-40%, and the mass ratio of alpha-fiber in the viscose liquid is 60-99%;
the finished product indexes of the cordyceps militaris protein fiber are as follows: the dry breaking strength is more than or equal to 2.06cN/dtex, the wet breaking strength is more than or equal to 1.00cN/dtex, the dry breaking elongation is 17+/-2.5%, and the protein content is more than or equal to 2.3%.
Further, the cordyceps militaris protein liquid is prepared from silkworm chrysalis protein powder and cordyceps militaris extract, wherein the fat content in the silkworm chrysalis protein powder is less than or equal to 5%, and the protein content is more than or equal to 60%.
Further, the viscose is viscose with the content of alpha-fiber of 8.5-9.2 percent.
The second purpose of the technical proposal is that: a preparation method of Cordyceps militaris protein fiber comprises the following steps:
1) Preparation of silkworm chrysalis protein liquid
X1: taking silkworm chrysalis protein powder, and washing with water at 30-80 ℃ to fully infiltrate the silkworm chrysalis protein powder; adding an active agent (one or more of dodecyl diethanolamide, polyoxyethylene fatty alcohol ether, polyoxyethylene alkylphenol ether and dodecyl amide phosphate), continuously stirring, standing for precipitation, and removing supernatant (including fat, ash and small part of dissolved protein);
wherein, the procedure is a pretreatment process of silkworm chrysalis protein powder, which removes fat and ash and improves the purity of the silkworm chrysalis protein powder. The washing is mainly used for degreasing, reducing fat and ash in protein powder, and if too much fat is contained in silkworm chrysalis protein liquid, the subsequent processing can be influenced, so that the fiber is poor in molding, more in broken ends, yarn separation and the like; at the same time, the use of the device is also affected. In addition, the silkworm chrysalis protein powder can be fully and uniformly soaked by water washing, so that the subsequent dissolution is facilitated, and the phenomenon that powder is aggregated into lumps is reduced. The degreasing agent is washed by water at 30-80 ℃, so that a better degreasing effect can be achieved, and if the degreasing agent is smaller than the temperature, the degreasing effect cannot be reduced; above this temperature, part of the protein is dissolved, resulting in protein loss. The water is deionized water, and has no impurity and mineral substances.
The active agent enables fat to be emulsified and aggregated on the surface as much as possible, is convenient to remove from the surface, the addition amount of the active agent is 0.05-1.5% of the mass of the silkworm chrysalis protein powder, the fat in the silkworm chrysalis protein powder is ensured to be removed as much as possible, and meanwhile, the cost is saved;
x2: adding water into the sediment after supernatant fluid removal to prepare a protein solution with the mass fraction of 10-30%, and then heating to 40-80 ℃; regulating the pH value to 8-14, and stirring for 2-24 h; wherein, caustic soda or other alkali liquor is adopted for regulating the pH value;
the procedure is a silkworm chrysalis protein powder dissolving process after pretreatment. Wherein, the mass fraction of the protein solution is controlled to be 10-30%, so that the protein solution is convenient to be mixed with viscose in the follow-up process, and if the mass fraction of the protein solution is too low, the mass of the viscose is larger, and the spinning performance of the viscose is affected; if the mass fraction of the protein solution is too high, the solubility of the protein solution is poor, and meanwhile, the mass of the added viscose is small, so that the protein solution is not easy to mix uniformly. The heating is controlled to be 40-80 ℃, so that the protein powder is quickly and effectively dissolved, and meanwhile, the effective activity of the protein is ensured, and if the temperature is higher than the effective activity, part of the protein is denatured, so that the resource waste is caused, and the subsequent cooling effect is influenced; if the temperature is less than this, the dissolution will be too slow, the time will be too long, and the production efficiency will be low. Controlling the pH value to be 8-14, firstly accelerating the dissolution of the protein powder and ensuring the full dissolution of the protein powder; 2. the spinning solution is convenient to mix with viscose, the viscose is alkaline, if the protein solution is acidic, the protein solution and the viscose react to form lumps, and the subsequent spinning is seriously affected. The limitation of stirring 2-24 ensures that the protein powder is fully dissolved, reduces the residue in the protein powder as much as possible, ensures that the subsequent spinning is easier to filter, and reduces the phenomena of yarn separation, poor spinning forming and the like in the production process;
x3: removing impurities from the protein solution by using a centrifuge or a filter to obtain silkworm chrysalis protein solution. Further removing a small part of protein and ash, and simultaneously ensuring that the fat content in the silkworm chrysalis protein liquid is less than 1%;
2) Preparation of Cordyceps militaris liquid
Y1: dissolving Cordyceps militaris extract in ethanol with the concentration of 1-40% and the temperature of 20-90 ℃, and filtering to remove impurities to obtain filtrate;
wherein, the mass fraction of the Cordyceps militaris extract after being dissolved in the ethanol is 10-50%, which ensures that the Cordyceps militaris extract is fully dissolved and is smaller than the concentration, thus leading to more subsequent mixing amount of silkworm chrysalis protein liquid and affecting the subsequent mixing with viscose liquid; above the concentration, cordyceps militaris extract has poor solubility, and is easy to cause non-uniformity when mixed with silkworm chrysalis protein liquid and viscose liquid. The related raw material Cordyceps militaris extract (mainly containing adenosine, cordycepin and Cordyceps polysaccharide) can be directly purchased. Ethanol with the concentration of 1-40% is selected as a solvent, so that substances in the cordyceps militaris extract are fully dissolved, the preparation cost is ensured, and if solvent water is adopted, the dissolution effect is poor. The temperature is limited to be 20-90 ℃, and is more than the temperature, so that the production operation is not facilitated, the resource waste is caused, and the subsequent cooling is influenced; if the temperature is less than this, the dissolution will be too slow, and the dissolution effect will be poor.
The filtering is to remove insoluble matters and impurities, so that the subsequent mixing with silkworm chrysalis protein liquid is facilitated, and the filtering performance is good after the cordyceps militaris extract solution is mixed with viscose liquid, so that the smooth spinning is ensured;
y2: adding a cross-linking agent (silane coupling agent) into the filtrate, and stirring until the mixture is uniformly mixed to obtain cordyceps militaris liquid; wherein the addition amount of the silane coupling agent is 0.5-5 per mill of the total weight of the cordyceps militaris extract;
the silane coupling agent improves the combination of protein and cellulose in the subsequent silkworm chrysalis protein liquid, and reduces the protein loss. The addition amount of the silane coupling agent is limited to 0.5-5 per mill of the total weight of the cordyceps militaris extract, so that the crosslinking effect is effectively ensured;
3) Mixing
1, the method comprises the following steps: 1-10, mixing the obtained cordyceps militaris liquid with silkworm chrysalis protein liquid, adding 0.5-10% of cross-linking agent (acryloylmethanol amine), uniformly mixing, and filtering to remove impurities to obtain cordyceps militaris protein liquid;
wherein, setting Cordyceps militaris liquid and silkworm chrysalis protein liquid to 1: 1-10, if the proportion is too small, the concentration of the cordyceps militaris protein liquid is low, and the subsequent adding amount is too large, so that the viscosity of the viscose liquid is influenced, and the spinning effect is influenced; the mixture ratio is too large, the concentration is too high, the solution is sticky, the dispersion of the solution in viscose is not facilitated, the filtering performance is poor, and the subsequent spinning performance is poor. In addition, the addition amount of the cross-linking agent, namely the acrylamide is controlled to be 0.5-10%, so that the combination between the cordyceps militaris liquid and the silkworm chrysalis protein liquid is increased, and the subsequent loss in the viscose liquid and the spinning process is reduced;
4) Blending
Respectively defoaming the obtained cordyceps militaris protein liquid and the viscose liquid, then statically mixing, and then defoaming to obtain a blending liquid;
in static mixing, the mass ratio of protein in the cordyceps militaris protein liquid is 1-40%, and the mass ratio of alpha-fiber in the viscose liquid is 60-99%; wherein the viscose is viscose with the content of alpha-fiber of 8.5-9.2 percent;
wherein, the proportion between the cordyceps militaris protein liquid and the viscose is limited to ensure the functionality of the cordyceps militaris protein fiber of the final product and ensure the uniform mixing of the cordyceps militaris protein liquid and the viscose in the blending process and the subsequent spinning performance;
5) Spinning process
Two-bath wet spinning is adopted;
feeding the blending liquid into a spinning machine through a glue supply pipeline, quantitatively feeding the blending liquid by a metering pump, filtering out particle impurities by a candle filter, feeding the blending liquid into a spinneret assembly by a curved pipe, and forming viscose trickles through spinneret holes under pressure;
6) Solidification and curing
And (3) solidification: solidifying and molding the viscose trickle in a coagulating bath to obtain a primary strand silk;
wherein the coagulating bath comprises 250-360g/L sodium sulfate, 80-130g/L sulfuric acid, 10-50g/L zinc sulfate and 8-25g/L auxiliary agent, the specific gravity of the coagulating bath and viscose trickle is 1.25-1.32, and the coagulating bath temperature is 40-60 ℃;
the coagulation bath is limited, and protein loss is effectively prevented. And controlling the specific gravity of the coagulating bath and the viscose trickle to be 1.25-1.32, and controlling the coagulating bath temperature to be 40-60 ℃ so as to ensure the forming of the viscose trickle. The viscose spinning forming is a very intense process, where the coagulation bath temperature is limited so that the forming process is not too intense, ensuring the fiber forming and facilitating the CS to be produced in the reaction process 2 Can be recovered as much as possible. The temperature rise accelerates the decomposition reaction of cellulose sulfonate, so that insufficient molding is caused by too fast reaction, and meanwhile, the added protein and cordyceps militaris extract cannot be effectively reserved on the fiber, so that a large amount of effective substances are lost, and the quality of a fiber finished product cannot be ensured;
curing: after passing through a yarn guiding disc, the primary yarn is bundled and stretched in a curing bath; in the curing bath, the primary yarn is stretched and simultaneously the decomposition and regeneration process is completed, wherein the structure of the fiber is shaped and the performance is stable, and the fiber bundle is obtained;
7) Post-treatment
Cutting off the obtained fiber bundles, and carrying out primary acid washing, desulfurization, primary water washing, secondary acid washing, secondary water washing, oiling, dehydration and drying to obtain the cordyceps militaris protein fiber finished product.
In the technical scheme, the related Cordyceps militaris extract is directly purchased and obtained and mainly contains substances such as adenosine, cordycepin, polysaccharide, rich selenium (Se) and the like, wherein the adenosine has the effects of resisting virus and bacteria, preventing and treating cerebral thrombosis and cerebral hemorrhage, inhibiting platelet accumulation, preventing thrombosis, eliminating facial plaques, resisting aging and preventing wrinkles. The cordycepin content in Cordyceps militaris is 0.05-51%, both the fruiting body and the body of Cordyceps militaris contain cordycepin, and the distribution difference of cordycepin in the fruiting body and the body of Cordyceps militaris is remarkable. Cordycepin, namely 3' -deoxyadenosine, is a nucleic acid derivative of nitrogen-containing glycoside, belongs to purine alkaloids, and is a nucleoside antibiotic. The pharmacological actions of cordycepin reported at home and abroad mainly comprise: inhibit microbial growth, resist tumor, regulate immunity, resist inflammation, etc. Cordyceps militaris polysaccharide has biological activities including anti-inflammatory effect, antioxidant activity, etc. Cordyceps militaris also contains abundant selenium (Se), which is known by people to be a trace element necessary for human body, is an active center of glutathione peroxidase, is connected to peptide chains of enzyme proteins in a selenium cysteine form, protects normal permeability of cell membrane stability, stimulates production of immunoglobulin and antibody, and enhances immunity and antioxidant capacity of the organism. Meanwhile, a great deal of scientific practice proves that selenium can obviously inhibit the growth of cancer cells.
In the technical scheme, the silkworm chrysalis protein powder is directly purchased and obtained by adopting silkworm chrysalis shells through the procedures of crushing, impurity removal, dissolution, extraction, purification, drying and the like, wherein the fat content of the protein powder is less than or equal to 5 percent, and the protein content is more than or equal to 60 percent.
By adopting the technical scheme, the beneficial technical effects brought are as follows:
1. in the invention, the related cordyceps militaris protein fiber is light yellow, has soft and fine hand feeling and gives people warm feeling; the fiber textile has good rebound resilience, the dimensional stability is obviously better than that of regenerated cellulose fiber, and the fiber textile has no oppression to skin and is skin-friendly and non-sticky. The cordyceps militaris protein fiber is rich in polar groups such as amino groups and carboxyl groups, has a good acid-base neutralization effect, and has excellent antibacterial performance, and is skin-friendly; in addition, the cordyceps militaris protein fiber has good anti-mite and antiviral properties;
2. in the preparation process of the cordyceps militaris liquid, the silane coupling agent is adopted, so that the combination between the protein and the cellulose can be increased in the subsequent process, and the loss of the protein is reduced;
3. in the mixing process, the acrylamide-methanol amine is adopted as the cross-linking agent between the cordyceps militaris and the silkworm chrysalis protein, so that the combination of the cordyceps militaris and the silkworm chrysalis protein is increased, the waste and the loss are reduced, and the retention quantity of a subsequent product, namely cordyceps militaris protein fiber, is ensured.
Drawings
FIG. 1 is a cross-sectional view of the final product of the protein fiber of Cordyceps militaris in example 8.
Detailed Description
In the following, it is obvious that the embodiments described are only some embodiments of the present invention, but not all embodiments, by clearly and completely describing the technical solutions in the embodiments of the present invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The present embodiment provides: the cordyceps militaris protein fiber is prepared by taking cordyceps militaris protein liquid and viscose liquid as raw materials and carrying out blending, spinning, solidification and post-treatment; wherein, during blending, the mass ratio of protein in the cordyceps militaris protein liquid is 1 percent, and the mass ratio of alpha-fiber in the viscose liquid is 99 percent. The cordyceps militaris protein liquid is prepared by taking silkworm chrysalis protein powder and cordyceps militaris extract as raw materials, wherein the fat content in the silkworm chrysalis protein powder is less than or equal to 5%, and the protein content is more than or equal to 60%. And the viscose is viscose with the content of alpha-fiber of 8.5 percent.
The finished product indexes of the cordyceps militaris protein fiber are as follows: the dry breaking strength is more than or equal to 2.06cN/dtex, the wet breaking strength is more than or equal to 1.00cN/dtex, the dry breaking elongation is 17+/-2.5%, and the protein content is more than or equal to 2.3%.
Example 2
The present embodiment provides: the cordyceps militaris protein fiber is prepared by taking cordyceps militaris protein liquid and viscose liquid as raw materials and carrying out blending, spinning, solidification and post-treatment; wherein, during blending, the mass ratio of protein in the cordyceps militaris protein liquid is 40 percent, and the mass ratio of alpha-fiber in the viscose liquid is 60 percent. The cordyceps militaris protein liquid is prepared by taking silkworm chrysalis protein powder and cordyceps militaris extract as raw materials, wherein the fat content in the silkworm chrysalis protein powder is less than or equal to 3%, and the protein content is more than or equal to 60%; the viscose is viscose with a alpha-fiber content of 9.2%.
The finished product indexes of the cordyceps militaris protein fiber are as follows: the dry breaking strength is more than or equal to 2.06cN/dtex, the wet breaking strength is more than or equal to 1.00cN/dtex, the dry breaking elongation is 17+/-2.5%, and the protein content is more than or equal to 2.3%.
Example 3
The present embodiment provides: the cordyceps militaris protein fiber is prepared by taking cordyceps militaris protein liquid and viscose liquid as raw materials and carrying out blending, spinning, solidification and post-treatment; wherein, during blending, the mass ratio of protein in the cordyceps militaris protein liquid is 15 percent, and the mass ratio of alpha-fiber in the viscose liquid is 85 percent. The cordyceps militaris protein liquid is prepared by taking silkworm chrysalis protein powder and cordyceps militaris extract as raw materials, wherein the fat content in the silkworm chrysalis protein powder is less than or equal to 2%, and the protein content is more than or equal to 60%; the viscose is viscose with a alpha-fiber content of 8.9%.
The finished product indexes of the cordyceps militaris protein fiber are as follows: the dry breaking strength is more than or equal to 2.06cN/dtex, the wet breaking strength is more than or equal to 1.00cN/dtex, the dry breaking elongation is 17+/-2.5%, and the protein content is more than or equal to 2.3%.
Example 4
The present embodiment provides: the cordyceps militaris protein fiber is prepared by taking cordyceps militaris protein liquid and viscose liquid as raw materials and carrying out blending, spinning, solidification and post-treatment; wherein, during blending, the mass ratio of protein in the cordyceps militaris protein liquid is 35%, and the mass ratio of alpha-fiber in the viscose liquid is 65%. The cordyceps militaris protein liquid is prepared by taking silkworm chrysalis protein powder and cordyceps militaris extract as raw materials, wherein the fat content in the silkworm chrysalis protein powder is less than or equal to 5%, and the protein content is more than or equal to 60%; the viscose is viscose with a alpha-fiber content of 9.0%.
The finished product indexes of the cordyceps militaris protein fiber are as follows: the dry breaking strength is more than or equal to 2.06cN/dtex, the wet breaking strength is more than or equal to 1.00cN/dtex, the dry breaking elongation is 17+/-2.5%, and the protein content is more than or equal to 2.3%.
Example 5
The present embodiment provides: a preparation method of Cordyceps militaris protein fiber comprises the following steps:
1) Preparation of silkworm chrysalis protein liquid
X1: taking silkworm chrysalis protein powder, and washing with water at 30 ℃ to fully infiltrate the silkworm chrysalis protein powder; adding dodecyl diethanolamide, stirring, standing for precipitation, and removing supernatant;
x2: adding water into the precipitate after supernatant removal to prepare a protein solution with the mass fraction of 30%, and then heating to 80 ℃; regulating the pH value to be 14, and stirring for 24 hours; wherein, caustic soda or other alkali liquor is adopted for regulating the pH value;
x3: removing impurities from the protein solution by using a centrifuge or a filter to obtain silkworm chrysalis protein solution;
2) Preparation of Cordyceps militaris liquid
Y1: dissolving Cordyceps militaris extract in 40% ethanol at 90deg.C, filtering to remove impurities to obtain filtrate;
wherein, the mass fraction of the Cordyceps militaris extract after being dissolved in ethanol is 50%;
y2: adding a silane coupling agent and an auxiliary agent into the filtrate, and stirring until the mixture is uniformly mixed to obtain cordyceps militaris liquid;
3) Mixing
1, the method comprises the following steps: 10, mixing the obtained cordyceps militaris liquid with silkworm chrysalis protein liquid, adding 10% of acrylamide, uniformly mixing, and filtering to remove impurities to obtain cordyceps militaris protein liquid;
4) Blending
Respectively defoaming the obtained cordyceps militaris protein liquid and the viscose liquid, then statically mixing, and then defoaming to obtain a blending liquid;
in static mixing, the mass ratio of protein in the cordyceps militaris protein liquid is 39%, and the mass ratio of alpha-fiber in the viscose liquid is 51%; wherein the viscose is viscose with a fiber A content of 9.1%;
5) Spinning process
Two-bath wet spinning is adopted;
feeding the blending liquid into a spinning machine through a glue supply pipeline, quantitatively feeding the blending liquid by a metering pump, filtering out particle impurities by a candle filter, feeding the blending liquid into a spinneret assembly by a curved pipe, and forming viscose trickles through spinneret holes under pressure;
6) Solidification and curing
And (3) solidification: solidifying and molding the viscose trickle in a coagulating bath to obtain a primary strand silk;
wherein the coagulating bath comprises 360g/L sodium sulfate, 130g/L sulfuric acid, 50g/L zinc sulfate and 25g/L auxiliary agent, the specific gravity of the coagulating bath and viscose trickle is 1.32, and the coagulating bath temperature is 60 ℃;
curing: after passing through a yarn guiding disc, the primary yarn is bundled and stretched in a curing bath; in the curing bath, the primary yarn is stretched and simultaneously the decomposition and regeneration process is completed, wherein the structure of the fiber is shaped and the performance is stable, and the fiber bundle is obtained;
7) Post-treatment
Cutting off the obtained fiber bundles, and carrying out primary acid washing, desulfurization, primary water washing, secondary acid washing, secondary water washing, oiling, dehydration and drying to obtain the cordyceps militaris protein fiber finished product.
Example 6
The present embodiment provides: a preparation method of Cordyceps militaris protein fiber comprises the following steps:
1) Preparation of silkworm chrysalis protein liquid
X1: taking silkworm chrysalis protein powder, and washing with water at 80 ℃ to fully infiltrate the silkworm chrysalis protein powder; adding polyoxyethylene fatty alcohol ether, polyoxyethylene alkylphenol ether and dodecyl alcohol amide phosphate, mixing, continuously stirring, standing for precipitation, and removing supernatant;
x2: adding water into the precipitate after supernatant removal to prepare a protein solution with the mass fraction of 10%, and then heating to 40 ℃; adjusting the pH value to 8, and stirring for 2 hours; wherein, caustic soda or other alkali liquor is adopted for regulating the pH value;
x3: removing impurities from the protein solution by using a centrifuge or a filter to obtain silkworm chrysalis protein solution;
2) Preparation of Cordyceps militaris liquid
Y1: dissolving Cordyceps militaris extract in 1-40% ethanol at 20deg.C, filtering to remove impurities to obtain filtrate;
wherein, the mass fraction of the Cordyceps militaris extract after being dissolved in ethanol is 10%;
y2: adding a silane coupling agent and an auxiliary agent into the filtrate, and stirring until the mixture is uniformly mixed to obtain cordyceps militaris liquid;
3) Mixing
1, the method comprises the following steps: 5, mixing the obtained cordyceps militaris liquid with the silkworm chrysalis protein liquid, adding 0.5% of acrylamide, uniformly mixing, and filtering to remove impurities to obtain the cordyceps militaris protein liquid;
4) Blending
Respectively defoaming the obtained cordyceps militaris protein liquid and the viscose liquid, then statically mixing, and then defoaming to obtain a blending liquid;
in static mixing, the mass ratio of protein in the cordyceps militaris protein liquid is 10%, and the mass ratio of alpha fiber in the viscose liquid is 90%; wherein the viscose is viscose with a fiber A content of 8.8%;
5) Spinning process
Two-bath wet spinning is adopted;
feeding the blending liquid into a spinning machine through a glue supply pipeline, quantitatively feeding the blending liquid by a metering pump, filtering out particle impurities by a candle filter, feeding the blending liquid into a spinneret assembly by a curved pipe, and forming viscose trickles through spinneret holes under pressure;
6) Solidification and curing
And (3) solidification: solidifying and molding the viscose trickle in a coagulating bath to obtain a primary strand silk;
wherein the coagulating bath comprises 250g/L sodium sulfate, 80g/L sulfuric acid, 10g/L zinc sulfate and 8g/L auxiliary agent, the specific gravity of the coagulating bath and viscose trickle is 1.25, and the coagulating bath temperature is 40 ℃;
curing: after passing through a yarn guiding disc, the primary yarn is bundled and stretched in a curing bath; in the curing bath, the primary yarn is stretched and simultaneously the decomposition and regeneration process is completed, wherein the structure of the fiber is shaped and the performance is stable, and the fiber bundle is obtained;
7) Post-treatment
Cutting off the obtained fiber bundles, and carrying out primary acid washing, desulfurization, primary water washing, secondary acid washing, secondary water washing, oiling, dehydration and drying to obtain the cordyceps militaris protein fiber finished product.
Example 7
The present embodiment provides: a preparation method of Cordyceps militaris protein fiber comprises the following steps:
1) Preparation of silkworm chrysalis protein liquid
X1: taking silkworm chrysalis protein powder, and washing with water at 50 ℃ to fully infiltrate the silkworm chrysalis protein powder; adding dodecyl alcohol amide phosphate, continuously stirring, standing for precipitation, and removing supernatant;
x2: adding water into the precipitate after supernatant removal to prepare a protein solution with the mass fraction of 20%, and then heating to 60 ℃; regulating the pH value to 10, and stirring for 16h; wherein, caustic soda or other alkali liquor is adopted for regulating the pH value;
x3: removing impurities from the protein solution by using a centrifuge or a filter to obtain silkworm chrysalis protein solution;
2) Preparation of Cordyceps militaris liquid
Y1: dissolving Cordyceps militaris extract in 25% ethanol at 60deg.C, filtering to remove impurities to obtain filtrate;
wherein, the mass fraction of the Cordyceps militaris extract after being dissolved in ethanol is 35%;
y2: adding a silane coupling agent and an auxiliary agent into the filtrate, and stirring until the mixture is uniformly mixed to obtain cordyceps militaris liquid;
3) Mixing
1, the method comprises the following steps: 8, mixing the obtained cordyceps militaris liquid with silkworm chrysalis protein liquid, adding 5% of acrylamide, uniformly mixing, and filtering to remove impurities to obtain cordyceps militaris protein liquid;
4) Blending
Respectively defoaming the obtained cordyceps militaris protein liquid and the viscose liquid, then statically mixing, and then defoaming to obtain a blending liquid;
in static mixing, the mass ratio of protein in the cordyceps militaris protein liquid is 28%, and the mass ratio of alpha-fiber in the viscose liquid is 72%; wherein the viscose is viscose with a fiber A content of 9.1%;
5) Spinning process
Two-bath wet spinning is adopted;
feeding the blending liquid into a spinning machine through a glue supply pipeline, quantitatively feeding the blending liquid by a metering pump, filtering out particle impurities by a candle filter, feeding the blending liquid into a spinneret assembly by a curved pipe, and forming viscose trickles through spinneret holes under pressure;
6) Solidification and curing
And (3) solidification: solidifying and molding the viscose trickle in a coagulating bath to obtain a primary strand silk;
wherein the coagulating bath comprises 320g/L sodium sulfate, 110g/L sulfuric acid, 48g/L zinc sulfate and 16g/L auxiliary agent, the specific gravity of the coagulating bath and viscose trickle is 1.30, and the coagulating bath temperature is 50 ℃;
curing: after passing through a yarn guiding disc, the primary yarn is bundled and stretched in a curing bath; in the curing bath, the primary yarn is stretched and simultaneously the decomposition and regeneration process is completed, wherein the structure of the fiber is shaped and the performance is stable, and the fiber bundle is obtained;
7) Post-treatment
Cutting off the obtained fiber bundles, and carrying out primary acid washing, desulfurization, primary water washing, secondary acid washing, secondary water washing, oiling, dehydration and drying to obtain the cordyceps militaris protein fiber finished product.
Example 8
In this example, 600g of a finished product of Cordyceps militaris protein fiber is produced as an example, and the technical scheme is further described. The method comprises the following steps:
1) Preparation of silkworm chrysalis protein liquid
X1: taking silkworm chrysalis protein powder, washing with water at 45 ℃ to fully infiltrate the silkworm chrysalis protein powder; adding dodecyl diethanolamide and polyoxyethylene fatty alcohol ether (1% of the powder), continuously stirring, standing for precipitation, and removing supernatant;
x2: supplementing water to the washed protein powder according to the proportion of 30% of the final mass fraction, and heating to 70 ℃; adjusting the pH value to 11, and stirring for 4 hours; wherein, caustic soda is adopted for regulating the pH value;
x3: removing impurities from the solution by using a centrifugal machine to obtain silkworm chrysalis protein liquid;
2) Preparation of Cordyceps militaris liquid
Y1: dissolving Cordyceps militaris extract in 20% ethanol at 60deg.C, and filtering to obtain filtrate;
wherein, the mass fraction of the Cordyceps militaris extract after being dissolved in ethanol is 30%;
y2: adding silane coupling agent into the filtrate, and stirring until the mixture is uniformly mixed to obtain Cordyceps militaris liquid;
wherein the mass fraction of the silane coupling agent is 2.5 per mill,
3) Mixing
Mixing the obtained Cordyceps militaris liquid with silkworm chrysalis protein liquid at a ratio of 1:5, adding 4% of acryloylmethanol amine, uniformly mixing, and filtering to obtain Cordyceps militaris protein liquid;
4) Blending
Respectively defoaming the obtained cordyceps militaris protein liquid and the viscose liquid, then statically mixing, and then defoaming to obtain a blending liquid;
in static mixing, the mass ratio of protein in the cordyceps militaris protein liquid is 8%, and the mass ratio of alpha-fiber in the viscose liquid is 92%; wherein the viscose is viscose with a fiber A content of 8.9%;
5) Spinning process
Two-bath wet spinning is adopted;
feeding the blending liquid into a spinning machine through a glue supply pipeline, quantitatively feeding the blending liquid by a metering pump, filtering out particle impurities by a candle filter, feeding the blending liquid into a spinneret assembly by a curved pipe, and forming viscose trickles through spinneret holes under pressure;
6) Solidification and curing
And (3) solidification: solidifying and molding the viscose trickle in a coagulating bath to obtain a primary strand silk;
wherein the coagulating bath comprises 250-360g/L sodium sulfate, 80-130g/L sulfuric acid and 10-50g/L zinc sulfate, the specific gravity of the coagulating bath and viscose trickles is 1.25-1.32, and the coagulating bath temperature is 40-60 ℃;
curing: after passing through a yarn guiding disc, the primary yarn is bundled and stretched in a curing bath; in the curing bath, the primary yarn is stretched and simultaneously the decomposition and regeneration process is completed, wherein the structure of the fiber is shaped and the performance is stable, and the fiber bundle is obtained;
7) Post-treatment
Cutting off the obtained fiber bundles, and carrying out primary acid washing, desulfurization, primary water washing, secondary acid washing, secondary water washing, oiling, dehydration and drying to obtain the cordyceps militaris protein fiber finished product.
The obtained cordyceps militaris protein fiber product was subjected to cross-section, and the result is shown in fig. 1. Wherein, in the sectional view of the cordyceps militaris protein fiber finished product, the protein can be seen to be in the viscose core layer.
Comparative example 1
On the basis of example 8, this comparative example 1 differs from example 8 in that the active agents dodecyl diethanolamide, polyoxyethylene fatty alcohol ether, polyoxyethylene alkylphenol ether and dodecyl alcohol amide phosphate are not used, and the remainder is the same as example 8. The results obtained are shown in Table 1.
Comparative example 2
On the basis of example 8, this comparative example 2 differs from example 8 in that a crosslinking agent (silane coupling agent) was not added to the filtrate in step Y2, and the remainder was the same as example 8. The results obtained are shown in Table 1.
Comparative example 3
On the basis of example 8, this comparative example 3 differs from example 8 in that the crosslinking agent acrylamide was not added in the step 3) mixing step, and the remainder was the same as in example 8. The results obtained are shown in Table 1.
The foregoing description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and any simple modification, equivalent variation, etc. of the above embodiment according to the technical matter of the present invention fall within the scope of the present invention.
Claims (10)
1. The cordyceps militaris protein fiber is characterized in that cordyceps militaris protein liquid and viscose are used as raw materials, and the cordyceps militaris protein fiber is prepared through blending, spinning, solidification and post-treatment; wherein, during blending, the mass ratio of protein in the cordyceps militaris protein liquid is 1-40%, and the mass ratio of alpha-fiber in the viscose liquid is 60-99%;
the finished product indexes of the cordyceps militaris protein fiber are as follows: the dry breaking strength is more than or equal to 2.06cN/dtex, the wet breaking strength is more than or equal to 1.00cN/dtex, the dry breaking elongation is 17+/-2.5%, and the protein content is more than or equal to 2.3%.
2. The cordyceps militaris protein fiber according to claim 1, wherein the cordyceps militaris protein liquid is prepared from silkworm chrysalis protein powder and cordyceps militaris extract, wherein the fat content in the silkworm chrysalis protein powder is less than or equal to 5%, and the protein content is more than or equal to 60%.
3. The cordyceps militaris protein fiber according to claim 1 or 2, wherein the viscose is a viscose with a alpha-fiber content of 8.5-9.2%.
4. The preparation method of the cordyceps militaris protein fiber is characterized by comprising the following steps of:
1) Preparation of silkworm chrysalis protein liquid
X1: taking silkworm chrysalis protein powder, and washing with water at 30-80 ℃; adding an active agent, continuously stirring, standing for precipitation, and removing supernatant;
x2: adding water into the sediment after supernatant liquid removal to prepare a protein solution with the mass fraction of 10-30%, and then heating to 40-80 ℃; regulating the pH value to 8-14, and stirring for 2-24 h;
x3: removing impurities from the protein solution to obtain silkworm chrysalis protein solution;
2) Preparation of Cordyceps militaris liquid
Y1: dissolving Cordyceps militaris extract in ethanol with the temperature of 20-90 ℃ and the concentration of 1-40%, and filtering to obtain filtrate;
y2: adding silane coupling agent into the filtrate, and stirring until the mixture is uniformly mixed to obtain Cordyceps militaris liquid;
3) Mixing
1, the method comprises the following steps: 1-10, mixing the obtained cordyceps militaris liquid with silkworm chrysalis protein liquid, adding 0.5-10% of acrylamide and methanol amine, uniformly mixing, and filtering to obtain cordyceps militaris protein liquid;
4) Blending
Respectively defoaming the obtained cordyceps militaris protein liquid and the viscose liquid, then statically mixing, and then defoaming to obtain a blending liquid;
in static mixing, the mass ratio of protein in the cordyceps militaris protein liquid is 1-40%, and the mass ratio of alpha-fiber in the viscose liquid is 60-99%; wherein the viscose is viscose with the content of alpha-fiber of 8.5-9.2 percent;
5) Spinning process
Two-bath wet spinning is adopted;
feeding the blending liquid into a spinning machine through a glue supply pipeline, quantitatively feeding the blending liquid by a metering pump, filtering out particle impurities by a candle filter, feeding the blending liquid into a spinneret assembly by a curved pipe, and forming viscose trickles through spinneret holes under pressure;
6) Solidification and curing
Solidifying and forming the viscose trickle in a coagulating bath, wherein the specific gravity of the coagulating bath and the viscose trickle is 1.25-1.32, and the coagulating bath temperature is 40-60 ℃ to obtain a primary strand silk;
after passing through a yarn guiding disc, the primary yarn is bundled and stretched in a curing bath; in the curing bath, the primary yarn is stretched and simultaneously the decomposition and regeneration process is completed, wherein the structure of the fiber is shaped and the performance is stable, and the fiber bundle is obtained;
7) Post-treatment
Cutting off the obtained fiber bundles, and carrying out primary acid washing, desulfurization, primary water washing, secondary acid washing, secondary water washing, oiling, dehydration and drying to obtain the cordyceps militaris protein fiber finished product.
5. The method for preparing a protein fiber of Cordyceps militaris according to claim 4, wherein the activator is one or more of dodecyl diethanolamide, polyoxyethylene fatty alcohol ether, polyoxyethylene alkylphenol ether and dodecyl alcohol amide phosphate.
6. The method for preparing cordyceps militaris protein fibers according to claim 4 or 5, wherein the activator is
The addition amount is 0.05 to 1.5 percent of the mass of the silkworm chrysalis protein powder.
7. The method of producing a protein fiber of Cordyceps militaris according to claim 4, wherein in step X3, a centrifuge or a filter is used to remove impurities.
8. The method for producing a protein fiber of Cordyceps militaris according to claim 4, wherein in step Y1, the mass fraction of the Cordyceps militaris extract after dissolution in ethanol is 10 to 50%.
9. The method for preparing protein fiber of Cordyceps militaris according to claim 4, wherein in step Y2, the silane coupling agent is added in an amount of 0.5-5% by weight based on the total weight of Cordyceps militaris extract.
10. The method for preparing protein fiber of Cordyceps militaris according to claim 4, wherein in step 6), the coagulation bath comprises 250-360g/L sodium sulfate, 80-130g/L sulfuric acid, 10-50g/L zinc sulfate and 8-25g/L auxiliary agent.
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