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CN110965149A - Water lily protein fiber and preparation process thereof - Google Patents

Water lily protein fiber and preparation process thereof Download PDF

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Publication number
CN110965149A
CN110965149A CN201910974964.9A CN201910974964A CN110965149A CN 110965149 A CN110965149 A CN 110965149A CN 201910974964 A CN201910974964 A CN 201910974964A CN 110965149 A CN110965149 A CN 110965149A
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water lily
protein fiber
acetic acid
lily protein
protein
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黄惠标
宋慎群
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Jiangsu Kangyichen Life Technology Co ltd
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Jiangsu Kangyichen Life Technology Co ltd
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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/02Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from cellulose, cellulose derivatives, or proteins
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07KPEPTIDES
    • C07K1/00General methods for the preparation of peptides, i.e. processes for the organic chemical preparation of peptides or proteins of any length
    • C07K1/14Extraction; Separation; Purification
    • C07K1/30Extraction; Separation; Purification by precipitation
    • C07K1/303Extraction; Separation; Purification by precipitation by salting out
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07KPEPTIDES
    • C07K1/00General methods for the preparation of peptides, i.e. processes for the organic chemical preparation of peptides or proteins of any length
    • C07K1/14Extraction; Separation; Purification
    • C07K1/34Extraction; Separation; Purification by filtration, ultrafiltration or reverse osmosis
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07KPEPTIDES
    • C07K1/00General methods for the preparation of peptides, i.e. processes for the organic chemical preparation of peptides or proteins of any length
    • C07K1/14Extraction; Separation; Purification
    • C07K1/36Extraction; Separation; Purification by a combination of two or more processes of different types
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F2/00Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
    • D01F2/06Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from viscose
    • D01F2/08Composition of the spinning solution or the bath

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • General Health & Medical Sciences (AREA)
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  • Health & Medical Sciences (AREA)
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  • Engineering & Computer Science (AREA)
  • Analytical Chemistry (AREA)
  • Medicinal Chemistry (AREA)
  • Molecular Biology (AREA)
  • Proteomics, Peptides & Aminoacids (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Textile Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Artificial Filaments (AREA)

Abstract

The invention provides a water lily protein fiber and a preparation process thereof, wherein the process comprises the following steps: pretreating the water lily plant to obtain water lily tissue powder; adding water lily tissue powder into acetic acid solution, taking supernatant, and salting out to obtain water lily protein precipitate; dissolving the precipitate in acetic acid solution, and dialyzing the supernatant to obtain water lily protein material; dispersing water lily protein material in spinnable regenerated cellulose spinning solution to form mixed spinning solution; and (4) spinning and post-treating the mixed spinning solution to obtain the water lily protein fiber. The water lily protein fiber prepared by the method disclosed by the invention is hydrophilic, moisture-keeping, soft, fine, durable, antibacterial, environment-friendly, renewable and degradable, and has protein content.

Description

Water lily protein fiber and preparation process thereof
Technical Field
The invention relates to the field of textiles, in particular to a water lily protein fiber and a preparation process thereof.
Background
Protein resources are quite abundant in nature, including vegetable proteins and animal proteins, and silk and wool are used as textile raw materials with excellent performance, and are essentially animal protein fibers. The protein fiber is made of vital protein, and has outstanding biological performance, good skin feeling and good health care function.
Nymphaea tetragona belongs to the family Nymphaeaceae, genus Nymphaea, perennial aquatic plant. The water lily fiber is a novel natural cellulose which is newly developed, has better moisture absorption, antibiosis, ventilation and perspiration performance, has obvious bacteriostasis to gram negative bacteria such as escherichia coli and fungi due to unique water lily alkaloid components, and is a rare natural plant material. The water lily fibers are widely distributed, and footprints of the water lily can be found all over the world except for the Antarctic. With the increasing maturity of water lily fiber extraction technology, scientific derivatives taking water lily fibers as the leading factor are continuously developed and applied, but the extraction of proteins from water lily for textile application is a subject to be researched in the industry.
Therefore, there is a need to provide a new solution.
Disclosure of Invention
In order to solve the technical problems in the prior art, the invention discloses a water lily protein fiber and a preparation process thereof, and the specific technical scheme is as follows:
the invention provides a water lily protein fiber preparation process, which comprises the following steps:
s1, preprocessing the water lily plant to obtain water lily tissue powder;
s2, adding the water lily tissue powder into an acetic acid solution, taking the supernatant, and salting out to obtain a water lily protein precipitate;
s3, dissolving the precipitate in an acetic acid solution, and dialyzing the supernatant to obtain a water lily protein raw material;
s4, dispersing the water lily protein raw material in a spinnable regenerated cellulose spinning solution to form a mixed spinning solution;
s5, spinning and post-treating the mixed spinning solution to obtain the water lily protein fiber.
Further, step S1 specifically includes:
s11, cleaning, drying and crushing the water lily plants to obtain tissue powder, wherein the water lily plants comprise water lily seeds, water lily leaves and water lily stems;
s12, adding the tissue powder obtained in the step S11 into a sodium hydroxide solution, soaking, stirring for 1-6 hours, cleaning, filtering and drying to obtain the water lily tissue powder, wherein the concentration of the sodium hydroxide solution is 0.05-3 mol/L.
Further, step S2 specifically includes:
s21, adding the water lily tissue powder obtained in the step S1 into an acetic acid solution, fully extracting for 5-10h, centrifuging for 5-30min, and taking supernatant, wherein the material-liquid ratio of the water lily tissue powder to the acetic acid solution is 1:5-30, the concentration of the acetic acid solution is 0.1-0.5mol/L, and the centrifugal rotation speed is 2000-;
s22, salting out the supernatant obtained in the step S21 for 3-15h by adopting sodium chloride to obtain a precipitate;
s23, centrifuging the sediment obtained in the step S22 to obtain the water lily protein sediment.
Further, step S3 specifically includes:
s31, dissolving the water lily protein precipitate obtained in the step S2 in an acetic acid solution, centrifuging for 5-30min, and taking supernatant, wherein the material-liquid ratio of the precipitate to the acetic acid solution is 1: 5-30;
s32, dialyzing the supernatant obtained in the step S31 by using an acetic acid solution, and drying to obtain the water lily protein raw material, wherein the concentration of the acetic acid solution is 0.05-0.3 mol/L.
Further, in step S4, the content of the water lily protein raw material is 1-15 wt%.
Further, in step S4, the spinnable regenerated cellulose spinning solution is a viscose spinning solution, and the mass concentration of the viscose spinning solution is 20-50%.
Further, step S5 specifically includes:
s51, filtering, defoaming and curing the mixed spinning solution obtained in the step S4, and then sending the mixed spinning solution to a spinning machine, wherein the spinning solution is extruded out of spinneret holes of a spinneret of the spinning machine through a metering pump to form a spinning trickle, the aperture of each spinneret hole is 0.03-0.8 mm, and the stretching multiple of the spinneret is 0.8-1.4 times;
S52. the spinning trickle formed in the step S51 enters a first coagulation bath to form tows, the tows passing through the first coagulation bath are sent to a second coagulation bath through a first drawing roller, the tows passing through the second coagulation bath are sent to a third coagulation bath through a second drawing roller, and the tows passing through the third coagulation bath are drawn by a third drawing roller and then output to obtain the water lily protein fiber; the temperature of the first coagulation bath is 42-46 ℃, the temperature of the second coagulation bath is 82-88 ℃, the temperature of the third coagulation bath is 80-85 ℃, the draft ratio of the second drawing roller is 40-60%, the draft ratio of the third drawing roller is 5-10%, the total draft ratio is controlled to be 3.0-3.4, and the pH value of the third coagulation bath is 1.5H2SO4
S53, cutting the water lily protein fibers in the step S52 by a cutting device to ensure that the cutting length is 38-55 mm, and forming the water lily protein fiber short fibers;
s54, sequentially adopting NaOH aqueous solution and hot water to wash the water lily protein fiber short fiber obtained in the step S53, and drying to obtain a finished product, wherein the temperature of the NaOH aqueous solution is 30-70 ℃, the concentration of the NaOH aqueous solution is 2-8g/L, the temperature of the hot water is 30-50 ℃, and the drying temperature is 40-80 ℃.
In addition, the invention also provides a water lily protein fiber which is prepared by the method, wherein the linear density of the water lily protein fiber is 1.5-1.67dtex, the dry breaking strength is 2-3 (cN/tex), the wet breaking strength is 1-1.5 (CN/tex), the dry breaking elongation is 17-19%, and the super-long elongation is 0.08-0.12%.
In addition, the invention also provides a yarn spun by the water lily protein fiber prepared by the method.
In addition, the invention also provides the application of the water lily protein fiber prepared by the method or the yarn spun by the water lily protein fiber prepared by the method, and the water lily protein fiber is suitable for non-woven products or fillings; the yarn spun by the water lily protein fiber is suitable for producing close-fitting textile fabric, home textile fabric, infant clothes or socks.
The invention has the following beneficial effects:
1. the invention extracts the protein of the water lily plants such as the water lily seeds, the water lily stems and leaves and the like, takes the regenerated cellulose fiber as a matrix, and adds the extracted water lily protein into the regenerated cellulose spinning solution to prepare the water lily protein fiber.
2. The water lily protein fiber provided by the invention has high antibacterial performance, can resist bacteria for a long time, has the antibacterial effect of 99 percent, can achieve the antibacterial effect of 99 percent after being washed by water for 20 times, and is suitable for home textile fabrics, underwear fabrics, infant clothes and socks. The invention has the advantages of beautifying and protecting skin, and the like, and the water lily protein fiber is environment-friendly, renewable and degradable.
3. The preparation process of the water lily protein fiber provided by the invention is simple, the water lily plant is firstly crushed, the water lily tissue powder is added into an acetic acid solution, and the supernatant is taken for salting out to obtain the water lily protein precipitate; then dissolving the precipitate in acetic acid solution, taking supernatant for dialysis to obtain the water lily protein raw material, wherein the obtained protein has small molecular weight and is easy to be absorbed by human body, and the fabric prepared by adopting the water lily protein fiber has better moisture retention, antibacterial property and comfort.
4. The water lily protein fiber provided by the invention has good spinnability, the linear density of the water lily protein fiber is 1.5-1.67dtex, the dry breaking strength is 2-3 (cN/tex), the wet breaking strength is 1-1.5 (CN/tex), the dry breaking elongation is 17-19%, the ultra-long elongation is 0.08-0.12%, and the water lily protein fiber has good strength and moisture retention performance and is suitable for manufacturing close-fitting textile fabrics, home textile fabrics and non-woven fabric products.
Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a process flow chart of the preparation process of the water lily protein fiber of the invention.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the drawings are illustrative and intended to be illustrative of the invention and are not to be construed as limiting the invention.
In the description of the present invention, it is to be understood that the terms "upper", "lower", "top", "bottom", "inner", "outer", and the like, indicate orientations or positional relationships based on those shown in the drawings, are merely for convenience in describing the present invention and simplifying the description, and do not indicate or imply that the referenced devices or elements must have a particular orientation, be constructed and operated in a particular orientation, and thus, are not to be construed as limiting the present invention. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
In the present invention, unless otherwise expressly stated or limited, the terms "mounted," "connected," "secured," and the like are to be construed broadly and can, for example, be fixedly connected, detachably connected, or integrally formed; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or may be connected through the interior of two elements or in interactive relation with one another. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
Please refer to fig. 1, which is a process flow diagram of the preparation process of the water lily protein fiber of the present invention.
Example 1
As shown in figure 1, the preparation process of the water lily protein fiber comprises the following steps:
s1, preprocessing the water lily plant to obtain water lily tissue powder. Step S1 specifically includes:
s11, cleaning, drying and crushing the water lily plants to obtain tissue powder, wherein the water lily plants comprise water lily seeds, water lily leaves and water lily stems;
s12, adding the tissue powder obtained in the step S11 into a sodium hydroxide solution, soaking, stirring for 3 hours, cleaning, filtering and drying to obtain the water lily tissue powder, wherein the concentration of the sodium hydroxide solution is 0.1 mol/L.
S2, adding the water lily tissue powder into an acetic acid solution, taking the supernatant, and salting out to obtain a water lily protein precipitate. Step S2 specifically includes:
s21, adding the water lily tissue powder obtained in the step S1 into an acetic acid solution, fully extracting for 8 hours, centrifuging for 15min, and taking supernatant, wherein the material-liquid ratio of the water lily tissue powder to the acetic acid solution is 1: 16, the concentration of the acetic acid solution is 0.3mol/L, and the centrifugal rotating speed is 4000 r/min;
s22, salting out the supernatant obtained in the step S21 for 8 hours by adopting sodium chloride to obtain a precipitate;
s23, centrifuging the sediment obtained in the step S22 to obtain the water lily protein sediment.
S3, dissolving the precipitate in acetic acid solution, and dialyzing the supernatant to obtain the water lily protein raw material. Step S3 specifically includes:
s31, dissolving the water lily protein precipitate obtained in the step S2 in an acetic acid solution, centrifuging for 15min, and taking supernatant, wherein the material-liquid ratio of the precipitate to the acetic acid solution is 1: 8;
s32, dialyzing the supernatant obtained in the step S31 by using an acetic acid solution, and drying to obtain the water lily protein raw material, wherein the concentration of the acetic acid solution is 0.1 mol/L.
S4, dispersing the water lily protein raw material in a spinnable regenerated cellulose spinning solution to form a mixed spinning solution; wherein the content of the water lily protein raw material is 6 wt%. The spinnable regenerated cellulose spinning solution is viscose fiber spinning solution, and the mass concentration of the viscose fiber spinning solution is 30%.
S5, spinning and post-treating the mixed spinning solution to obtain the water lily protein fiber. Step S5 specifically includes:
s51, filtering, defoaming and curing the mixed spinning solution obtained in the step S4, and then sending the mixed spinning solution to a spinning machine, wherein the spinning solution is extruded out of spinneret holes of a spinneret of the spinning machine through a metering pump to form a spinning trickle, the aperture of each spinneret hole is 0.06mm, and the stretching multiple of the spinneret is 1.2 times;
s52, feeding the spinning trickle formed in the step S51 into a first coagulation bath to form tows, conveying the tows passing through the first coagulation bath into a second coagulation bath through a first drawing roller, conveying the tows passing through the second coagulation bath into a third coagulation bath through a second drawing roller, and drawing the tows passing through the third coagulation bath through a third drawing roller and outputting the tows to obtain the water lily protein fibers; the temperature of the first coagulation bath is 42-46 ℃, the temperature of the second coagulation bath is 82-88 ℃, the temperature of the third coagulation bath is 80-85 ℃, the draft ratio of the second drawing roller is 50%, the draft ratio of the third drawing roller is 8%, the total draft ratio is controlled to be 3.0-3.4, and the third coagulation bath comprises H with the pH value of 1.52SO4
S53, cutting the water lily protein fiber in the step S52 by a cutting device to ensure that the cutting length is 38mm, and forming the water lily protein fiber short fiber;
s54, sequentially adopting NaOH aqueous solution and hot water to wash the water lily protein fiber short fibers obtained in the step S53, and drying to obtain finished products, wherein the temperature of the NaOH aqueous solution is 45 ℃, the concentration of the NaOH aqueous solution is 4g/L, the temperature of the hot water is 38 ℃, and the drying temperature is 80 ℃.
Example 2
As shown in figure 1, the preparation process of the water lily protein fiber comprises the following steps:
s1, preprocessing the water lily plant to obtain water lily tissue powder. Step S1 specifically includes:
s11, cleaning, drying and crushing the water lily plants to obtain tissue powder, wherein the water lily plants comprise water lily seeds, water lily leaves and water lily stems;
s12, adding the tissue powder obtained in the step S11 into a sodium hydroxide solution, soaking, stirring for 1 hour, cleaning, filtering and drying to obtain the water lily tissue powder, wherein the concentration of the sodium hydroxide solution is 0.05 mol/L.
S2, adding the water lily tissue powder into an acetic acid solution, taking the supernatant, and salting out to obtain a water lily protein precipitate. Step S2 specifically includes:
s21, adding the water lily tissue powder obtained in the step S1 into an acetic acid solution, fully extracting for 5 hours, centrifuging for 5 minutes, and taking supernatant, wherein the material-liquid ratio of the water lily tissue powder to the acetic acid solution is 1:5, the concentration of the acetic acid solution is 0.1mol/L, and the centrifugal rotating speed is 2000 r/min;
s22, salting out the supernatant obtained in the step S21 for 38 hours by adopting sodium chloride to obtain a precipitate;
s23, centrifuging the sediment obtained in the step S22 to obtain the water lily protein sediment.
S3, dissolving the precipitate in acetic acid solution, and dialyzing the supernatant to obtain the water lily protein raw material. Step S3 specifically includes:
s31, dissolving the water lily protein precipitate obtained in the step S2 in an acetic acid solution, centrifuging for 5min, and taking supernatant, wherein the material-liquid ratio of the precipitate to the acetic acid solution is 1: 5;
s32, dialyzing the supernatant obtained in the step S31 by using an acetic acid solution, and drying to obtain the water lily protein raw material, wherein the concentration of the acetic acid solution is 0.05 mol/L.
S4, dispersing the water lily protein raw material in a spinnable regenerated cellulose spinning solution to form a mixed spinning solution; wherein the content of the water lily protein raw material is 1 wt%. The spinnable regenerated cellulose spinning solution is viscose fiber spinning solution, and the mass concentration of the viscose fiber spinning solution is 20%.
S5, spinning and post-treating the mixed spinning solution to obtain the water lily protein fiber. Step S5 specifically includes:
s51, filtering, defoaming and curing the mixed spinning solution obtained in the step S4, and then sending the mixed spinning solution to a spinning machine, wherein the spinning solution is extruded out of spinneret holes of a spinneret of the spinning machine through a metering pump to form a spinning trickle, the aperture of each spinneret hole is 0.03mm, and the stretching multiple of the spinneret is 0.8 times;
s52, feeding the spinning trickle formed in the step S51 into a first coagulation bath to form tows, conveying the tows passing through the first coagulation bath into a second coagulation bath through a first drawing roller, conveying the tows passing through the second coagulation bath into a third coagulation bath through a second drawing roller, and drawing the tows passing through the third coagulation bath through a third drawing roller and outputting the tows to obtain the water lily protein fibers; the temperature of the first coagulation bath is 42-46 ℃, the temperature of the second coagulation bath is 82-88 ℃, the temperature of the third coagulation bath is 80-85 ℃, the draft ratio of the second drawing roller is 40%, the draft ratio of the third drawing roller is 5%, the total draft ratio is controlled to be 3.0-3.4, and the third coagulation bath comprises H with the pH value of 1.52SO4
S53, cutting the water lily protein fiber in the step S52 by a cutting device to enable the cutting length to be 55mm, and forming the water lily protein fiber short fiber;
s54, sequentially adopting NaOH aqueous solution and hot water to wash the water lily protein fiber short fibers obtained in the step S53, and drying to obtain a finished product, wherein the temperature of the NaOH aqueous solution is 30 ℃, the concentration of the NaOH aqueous solution is 2g/L, the temperature of the hot water is 30-DEG C, and the drying temperature is 40 ℃.
Example 3
As shown in figure 1, the preparation process of the water lily protein fiber comprises the following steps:
s1, preprocessing the water lily plant to obtain water lily tissue powder. Step S1 specifically includes:
s11, cleaning, drying and crushing the water lily plants to obtain tissue powder, wherein the water lily plants comprise water lily seeds, water lily leaves and water lily stems;
s12, adding the tissue powder obtained in the step S11 into a sodium hydroxide solution, soaking, stirring for 6 hours, cleaning, filtering and drying to obtain the water lily tissue powder, wherein the concentration of the sodium hydroxide solution is 0.33 mol/L.
S2, adding the water lily tissue powder into an acetic acid solution, taking the supernatant, and salting out to obtain a water lily protein precipitate. Step S2 specifically includes:
s21, adding the water lily tissue powder obtained in the step S1 into an acetic acid solution, fully extracting for 10h, centrifuging for 30min, and taking supernatant, wherein the material-liquid ratio of the water lily tissue powder to the acetic acid solution is 1:30, the concentration of the acetic acid solution is 1mol/L, and the centrifugal rotating speed is 8000 r/min;
s22, salting out the supernatant obtained in the step S21 for 15 hours by adopting sodium chloride to obtain a precipitate;
s23, centrifuging the sediment obtained in the step S22 to obtain the water lily protein sediment.
S3, dissolving the precipitate in acetic acid solution, and dialyzing the supernatant to obtain the water lily protein raw material. Step S3 specifically includes:
s31, dissolving the water lily protein precipitate obtained in the step S2 in an acetic acid solution, centrifuging for 30min, and taking supernatant, wherein the material-liquid ratio of the precipitate to the acetic acid solution is 1: 30;
s32, dialyzing the supernatant obtained in the step S31 by using an acetic acid solution, and drying to obtain the water lily protein raw material, wherein the concentration of the acetic acid solution is 0.3 mol/L.
S4, dispersing the water lily protein raw material in a spinnable regenerated cellulose spinning solution to form a mixed spinning solution; wherein the content of the water lily protein raw material is 15 wt%. The spinnable regenerated cellulose spinning solution is viscose fiber spinning solution, and the mass concentration of the viscose fiber spinning solution is 50%.
S5, spinning and post-treating the mixed spinning solution to obtain the water lily protein fiber. Step S5 specifically includes:
s51, filtering, defoaming and curing the mixed spinning solution obtained in the step S4, and then sending the mixed spinning solution to a spinning machine, wherein the spinning solution is extruded out of spinneret holes of a spinneret of the spinning machine through a metering pump to form a spinning trickle, the aperture of each spinneret hole is 0.8mm, and the stretching multiple of the spinneret is 1.4 times;
s52, feeding the spinning trickle formed in the step S51 into a first coagulation bath to form tows, conveying the tows passing through the first coagulation bath into a second coagulation bath through a first drawing roller, conveying the tows passing through the second coagulation bath into a third coagulation bath through a second drawing roller, and drawing the tows passing through the third coagulation bath through a third drawing roller and outputting the tows to obtain the water lily protein fibers; the temperature of the first coagulation bath is 42-46 ℃, the temperature of the second coagulation bath is 82-88 ℃, the temperature of the third coagulation bath is 80-85 ℃, the draft ratio of the second drawing roller is 60%, the draft ratio of the third drawing roller is 10%, the total draft ratio is controlled to be 3.0-3.4, and the third coagulation bath comprises H with the pH value of 1.52SO4
S53, cutting the water lily protein fiber in the step S52 by a cutting device to enable the cutting length to be 55mm, and forming the water lily protein fiber short fiber;
s54, sequentially adopting NaOH aqueous solution and hot water to wash the water lily protein fiber short fibers obtained in the step S53, and drying to obtain a finished product, wherein the temperature of the NaOH aqueous solution is 70 ℃, the concentration of the NaOH aqueous solution is 8g/L, the temperature of the hot water is 50 ℃, and the drying temperature is 80 ℃.
The water lily protein fiber prepared by the method has the linear density of 1.5-1.67dtex, the dry breaking strength of 2-3 (cN/tex), the wet breaking strength of 1-1.5 (CN/tex), the dry breaking elongation of 17-19% and the ultra-long elongation of 0.08-0.12%.
The invention also provides a yarn spun by the water lily protein fiber.
The water lily protein fiber prepared by the method is suitable for non-woven products or fillings; the yarn spun by the water lily protein fiber is suitable for producing close-fitting textile fabric, home textile fabric, infant clothes or socks.
The invention has the following beneficial effects:
1. the invention extracts the protein of the water lily plants such as the water lily seeds, the water lily stems and leaves and the like, takes the regenerated cellulose fiber as a matrix, and adds the extracted water lily protein into the regenerated cellulose spinning solution to prepare the water lily protein fiber, the protein is easy to be absorbed by the human body, and the moisture retention and the flexibility can be better realized by combining with the regenerated cellulose fiber.
2. The water lily protein fiber provided by the invention has high antibacterial performance, can resist bacteria for a long time, has the antibacterial effect of 99 percent, can achieve the antibacterial effect of 99 percent after being washed by water for 20 times, and is suitable for home textile fabrics, underwear fabrics, infant clothes and socks. The invention has the advantages of beautifying and protecting skin, and the like, and the water lily protein fiber is environment-friendly, renewable and degradable.
3. The preparation process of the water lily protein fiber provided by the invention is simple, the water lily plant is firstly crushed, the water lily tissue powder is added into an acetic acid solution, and the supernatant is taken for salting out to obtain the water lily protein precipitate; then dissolving the precipitate in acetic acid solution, taking supernatant for dialysis to obtain the water lily protein raw material, wherein the obtained protein not only has small molecular weight and is easy to be absorbed by human body, but also the fabric prepared by adopting the water lily protein fiber has better moisture retention, antibacterial property and comfort.
4. The water lily protein fiber provided by the invention has good spinnability, the linear density of the water lily protein fiber is 1.5-1.67dtex, the dry breaking strength is 2-3 (cN/tex), the wet breaking strength is 1-1.5 (CN/tex), the dry breaking elongation is 17-19%, the ultra-long elongation is 0.08-0.12%, and the water lily protein fiber has good strength and moisture retention performance and is suitable for manufacturing close-fitting textile fabrics, home textile fabrics and non-woven fabric products.
The performance of the water lily protein fiber prepared by the process method provided by one embodiment of the invention, and the detection results of the detection report given by the fiber detection in Nantong city are shown in the following table 1:
TABLE 1
Figure BDA0002233297290000101
As can be seen from Table 1, the water lily protein fiber prepared by the invention has various performance indexes reaching the textile performance standard and has good spinnability.
The water lily protein fiber prepared by the process method of one embodiment of the invention is used as a filler, and the detection results of the detection report given by the national clothing quality supervision and inspection center (Tianjin) of the Tian textile Standard detection and certification GmbH are shown in the following table 2:
TABLE 2
Figure BDA0002233297290000111
In table 2, the regenerated cellulose fibers (containing proteins) are the water lily protein fibers prepared by the method of the present invention.
As shown in Table 2, after the water lily protein fiber and the polyester fiber are mixed, the white filler has the performances of hydrophilic moisture retention, softness, fineness, lasting antibiosis, protein content, environmental protection, regeneration and degradability.
The fiber content of the water lily protein fiber prepared by the process method provided by one embodiment of the invention and the detection results of the inspection report given by the national cotton printing and dyeing product quality supervision and inspection center are shown in the following table 3:
TABLE 3
Figure BDA0002233297290000112
In table 3, regenerated cellulose fibers (containing proteins) are the water lily protein fibers prepared by the method of the present invention.
As can be seen from Table 3, the water lily protein fiber prepared by the method of the present invention is 100% regenerated cellulose fiber.
The water lily protein fiber prepared by the process method provided by one embodiment of the invention has antibacterial property, and the detection results of the test report given by the Guangdong province microorganism analysis and detection center are shown in the following table 4:
TABLE 4
Figure BDA0002233297290000113
Figure BDA0002233297290000121
As can be seen from Table 4, before water washing, the antibacterial efficacy of the water lily protein fiber prepared by the method of the invention is as high as 99% or more, and after 20 times of washing, the efficacy of the water lily protein fiber for resisting staphylococcus aureus is still as high as 99%. The initial antimicrobial efficacy of conventional fiber fabrics is about 80%, but after 20 washes, the efficacy is only 30% to 40%.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example" or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples described in this specification can be combined and combined by one skilled in the art.
While embodiments of the present invention have been shown and described above, it is to be understood that the above embodiments are exemplary and not to be construed as limiting the present invention, and that changes, modifications and variations may be made therein by those of ordinary skill in the art within the scope of the present invention.

Claims (10)

1. A water lily protein fiber preparation process is characterized by comprising the following steps:
s1, preprocessing the water lily plant to obtain water lily tissue powder;
s2, adding the water lily tissue powder into an acetic acid solution, taking the supernatant, and salting out to obtain a water lily protein precipitate;
s3, dissolving the precipitate in an acetic acid solution, and dialyzing the supernatant to obtain a water lily protein raw material;
s4, dispersing the water lily protein raw material in a spinnable regenerated cellulose spinning solution to form a mixed spinning solution;
s5, spinning and post-treating the mixed spinning solution to obtain the water lily protein fiber.
2. The process for preparing water lily protein fiber according to claim 1, wherein the step S1 specifically comprises:
s11, cleaning, drying and crushing the water lily plants to obtain tissue powder, wherein the water lily plants comprise water lily seeds, water lily leaves and water lily stems;
s12, adding the tissue powder obtained in the step S11 into a sodium hydroxide solution, soaking, stirring for 1-6 hours, cleaning, filtering and drying to obtain the water lily tissue powder, wherein the concentration of the sodium hydroxide solution is 0.05-3 mol/L.
3. The process for preparing water lily protein fiber according to claim 1, wherein the step S2 specifically comprises:
s21, adding the water lily tissue powder obtained in the step S1 into an acetic acid solution, fully extracting for 5-10h, centrifuging for 5-30min, and taking supernatant, wherein the material-liquid ratio of the water lily tissue powder to the acetic acid solution is 1:5-30, the concentration of the acetic acid solution is 0.1-0.5mol/L, and the centrifugal rotation speed is 2000-;
s22, salting out the supernatant obtained in the step S21 for 3-15h by adopting sodium chloride to obtain a precipitate;
s23, centrifuging the sediment obtained in the step S22 to obtain the water lily protein sediment.
4. The process for preparing water lily protein fiber according to claim 1, wherein the step S3 specifically comprises:
s31, dissolving the water lily protein precipitate obtained in the step S2 in an acetic acid solution, centrifuging for 5-30min, and taking supernatant, wherein the material-liquid ratio of the precipitate to the acetic acid solution is 1: 5-30;
s32, dialyzing the supernatant obtained in the step S31 by using an acetic acid solution, and drying to obtain the water lily protein raw material, wherein the concentration of the acetic acid solution is 0.05-0.3 mol/L.
5. The process for preparing water lily protein fiber according to claim 1, wherein in step S4, the water lily protein material content is 1-15 wt%.
6. The process for preparing water lily protein fiber according to claim 1, wherein in step S4, the spinnable regenerated cellulose spinning solution is viscose spinning solution, and the mass concentration of the viscose spinning solution is 20-50%.
7. The process for preparing water lily protein fiber according to claim 1, wherein the step S5 specifically comprises:
s51, filtering, defoaming and curing the mixed spinning solution obtained in the step S4, and then sending the mixed spinning solution to a spinning machine, wherein the spinning solution is extruded out of spinneret holes of a spinneret of the spinning machine through a metering pump to form a spinning trickle, the aperture of each spinneret hole is 0.03-0.8 mm, and the stretching multiple of the spinneret is 0.8-1.4 times;
s52, feeding the spinning trickle formed in the step S51 into a first coagulation bath to form tows, conveying the tows passing through the first coagulation bath into a second coagulation bath through a first drawing roller, conveying the tows passing through the second coagulation bath into a third coagulation bath through a second drawing roller, and drawing the tows passing through the third coagulation bath through a third drawing roller and outputting the tows to obtain the water lily protein fibers; the temperature of the first coagulation bath is 42-46 ℃, the temperature of the second coagulation bath is 82-88 ℃, the temperature of the third coagulation bath is 80-85 ℃, the draft ratio of the second drawing roller is 40-60%, the draft ratio of the third drawing roller is 5-10%, the total draft ratio is controlled to be 3.0-3.4, and the pH value of the third coagulation bath is 1.52SO4
S53, cutting the water lily protein fibers in the step S52 by a cutting device to enable the cutting length to be 38-55 mm, and forming the water lily protein fiber short fibers;
s54, sequentially adopting NaOH aqueous solution and hot water to wash the water lily protein fiber short fiber obtained in the step S53, and drying to obtain a finished product, wherein the temperature of the NaOH aqueous solution is 30-70 ℃, the concentration of the NaOH aqueous solution is 2-8g/L, the temperature of the hot water is 30-50 ℃, and the drying temperature is 40-80 ℃.
8. A water lily protein fiber, which is characterized in that: the water lily protein fiber is prepared by the method of any one of claims 1 to 7, and has the linear density of 1.5 to 1.67dtex, the dry breaking strength of 2 to 3(cN/tex), the wet breaking strength of 1 to 1.5(CN/tex), the dry breaking elongation of 17 to 19 percent and the ultra-long elongation of 0.08 to 0.12 percent.
9. A yarn spun using the water lily protein fiber of claim 8.
10. Use of the water lily protein fiber of claim 8 or the yarn spun from the water lily protein fiber of claim 9, wherein the water lily protein fiber is suitable for non-woven products or fillings; the yarn spun by the water lily protein fiber is suitable for producing close-fitting textile fabric, home textile fabric, infant clothes or socks.
CN201910974964.9A 2019-10-14 2019-10-14 Water lily protein fiber and preparation process thereof Pending CN110965149A (en)

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CN111349976A (en) * 2020-04-14 2020-06-30 江苏康溢臣生命科技有限公司 Preparation method of regenerated cellulose fiber extracted from lotus plants
CN112126998A (en) * 2020-10-13 2020-12-25 江苏康溢臣生命科技有限公司 Preparation method of multifunctional viscose containing plant protein
CN113584677A (en) * 2021-09-03 2021-11-02 佳莱科技有限公司 Nerve-soothing woven fabric and preparation method thereof
CN115110176A (en) * 2022-08-10 2022-09-27 江苏康溢臣生命科技有限公司 Preparation method of saussurea involucrate protein fiber
CN115717280A (en) * 2022-11-24 2023-02-28 西安工程大学 Multifunctional regenerated cellulose fiber based on waste lotus stems and preparation method thereof

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CN111349976A (en) * 2020-04-14 2020-06-30 江苏康溢臣生命科技有限公司 Preparation method of regenerated cellulose fiber extracted from lotus plants
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CN115717280B (en) * 2022-11-24 2024-03-22 西安工程大学 Multifunctional regenerated cellulose fiber based on waste lotus stalks and preparation method thereof

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