CN115198386B - Microporous pure protein fiber and preparation method thereof - Google Patents
Microporous pure protein fiber and preparation method thereof Download PDFInfo
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- CN115198386B CN115198386B CN202210920855.0A CN202210920855A CN115198386B CN 115198386 B CN115198386 B CN 115198386B CN 202210920855 A CN202210920855 A CN 202210920855A CN 115198386 B CN115198386 B CN 115198386B
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- 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
- D01F4/00—Monocomponent artificial filaments or the like of proteins; Manufacture thereof
- D01F4/06—Monocomponent artificial filaments or the like of proteins; Manufacture thereof from globulins, e.g. groundnut protein
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- 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
- D01F4/00—Monocomponent artificial filaments or the like of proteins; Manufacture thereof
-
- 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
- D01F4/00—Monocomponent artificial filaments or the like of proteins; Manufacture thereof
- D01F4/02—Monocomponent artificial filaments or the like of proteins; Manufacture thereof from fibroin
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- General Chemical & Material Sciences (AREA)
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Abstract
The invention belongs to the technical field of textile material preparation, and particularly relates to a microporous pure protein fiber and a preparation method thereof, wherein the preparation method comprises the following steps: boiling the protein slurry, cooling to 50-60 ℃, adding the boiling hot solution, then adding the protein coagulant, and obtaining the microporous pure protein fiber through standing sedimentation, suction filtration, dry spinning and low-temperature condensation shaping. The invention adopts pure natural, safe and harmless preparation raw materials, adopts ultra-low temperature congealing technology to prepare microporous pure protein fibers, and the prepared fibers have multiple functions of softness, light weight, warmth retention, moisture retention and the like.
Description
Technical Field
The invention belongs to the technical field of textile material preparation, and particularly relates to a microporous pure protein fiber and a preparation method thereof.
Background
The existing mass-produced protein fibers are mostly prepared by mixing basic textile materials with protein, the carrier of the produced regenerated protein fibers, such as soybean fibers, is vinylon, the carrier of milk protein fibers is acrylic fibers, the carrier of silkworm pupa protein fibers is regenerated cellulose fibers and the like, and the protein content in the fibers is low, the protein content is about 2-10%, and the maximum protein content is only 65%. Moreover, because the fiber belongs to the blend fiber and is not a high-purity protein fiber, the cross-section structure of the formed fiber is compact, and the apparent performance is consistent with the carrier performance. At present, the existing protein fiber has certain defects, and because the regenerated protein fiber has a long production process, and the carriers are all chemical fibers, the chemical reagents and the auxiliary agents are used more, the toxicity is high, and the protein content is low.
Chinese patent CN114086270A entitled "preparation method of composite vegetable protein fiber" reports that various vegetable protein slurries are compounded to prepare composite protein slurry so as to solve the problems of water solubility and compatibility, improve the fixation rate of protein in fiber and reduce protein shedding; the method adopts wet spinning and is combined with coagulating liquid to coagulate protein fiber. Chinese patent CN113957560a entitled "a method for preparing a hair protein flame retardant cellulose fiber" reports that a hair protein fiber having a silky feel is prepared using a hair protein slurry, and an ultraviolet screening agent is added to the fiber for sun screening, and the fiber is combined with protein through a curing agent to prevent protein loss; the raw materials of the composite material still adopt chemical fibers, and more chemical reagents and auxiliaries are used.
Disclosure of Invention
The invention aims to solve the problems in the prior art, and provides a microporous pure protein fiber and a preparation method thereof, wherein the microporous pure protein fiber is prepared by adopting pure natural, safe and harmless preparation raw materials and adopting an ultralow-temperature congealing technology, and the prepared fiber has multiple functions of softness, light weight, heat preservation, moisture preservation and the like.
The technical scheme of the invention is as follows:
a method for preparing microporous pure protein fiber, comprising the following steps:
boiling the protein slurry, cooling to 50-60 ℃, adding the boiling hot solution, then adding the protein coagulant, and obtaining the microporous pure protein fiber through standing sedimentation, suction filtration, dry spinning and low-temperature condensation shaping.
Further, the condensing temperature in the low-temperature condensing and shaping step is-196 to-20 ℃, for example, -196 ℃, -180 ℃, -170 ℃, -160 ℃, -100 ℃, -80 ℃, -60 ℃, -40 ℃, -20 ℃ and the like, but the condensing temperature is not limited to the recited values, and the values within the above numerical ranges are applicable; the condensation time is 0.5 to 1440min, and may be, for example, 0.5min, 5min, 15min, 30min, 45min, 60min, 100min, 140min, 300min, 7h, 10h, 15h, 18h, 20h, 24h, etc., but is not limited to the above-mentioned values, and values within the above-mentioned numerical ranges are applicable.
Preferably, the condensing temperature is-35 ℃ and the condensing time is 25min.
Further, the cooling rate is 2-8 ℃/min.
Preferably, the rate of cooling is 6deg.C/min.
Further, the volume ratio of the boiling hot solution to the protein slurry is (5-15): (300-500), the boiling hot solution affects the strength too much, and if too little, the porosity. Preferably, the volume ratio of the boiling hot solution to the protein slurry is 10:400; it may also be 5:300, 5:500, 5:400, 15:300, 15:500, 15:400, 10:300, 10:500, etc., but is not limited to the recited point values, as long as values within the above-mentioned numerical ranges are equally applicable.
Further, the boiling hot solution is an aqueous solution of a multifunctional small molecule compound;
further, the functional group of the multi-functional group small molecule is one or a combination of more of amino, hydroxyl and carboxyl; the boiling hot solution is a solution obtained by dissolving one or more kinds of small multifunctional molecules in a boiling aqueous solution, and therefore, it is known that the temperature of the boiling hot solution is the boiling temperature.
The mass concentration of the aqueous solution of the polyfunctional small molecule compound is 20 to 60mg/mL, and for example, 20mg/mL, 25mg/mL, 30mg/mL, 35mg/mL, 40mg/mL, 50mg/mL, 60mg/mL, etc., but the concentration is not limited to the values listed, and any value within the above-mentioned numerical ranges is applicable.
Further, the multifunctional small molecule is selected from one or more of 1, 3-dimethylol urea, L-citrulline, N-acetyl-D-alanine, L-theanine, 1-amino ring Ding Jiasuan, L-glutamine, boc-D-serine, malonic acid, citric acid, butane tetracarboxylic acid and citric acid betaine.
Preferably, the multifunctional small molecule is 1, 3-dimethylol urea solution, L-threonine, or citric acid betaine; the mass ratio of the 1, 3-dimethylol urea solution to the L-threonine to the citric acid betaine is 0.2-0.6:1-2:0.7-1.5.
More preferably, the mass ratio of the 1, 3-dimethylol urea solution, the L-threonine and the citric acid betaine is 0.5:1.5:0.1.
Further, the protein coagulant comprises one or more of magnesium chloride, calcium sulfate, magnesium sulfate, calcium chloride, sodium carbonate, acetic acid, sodium hydroxide, urea, acetone, ethanol, hydrochloric acid, sulfuric acid, ammonium sulfate, sodium phosphate and sodium sulfate.
The invention also protects the microporous pure protein fiber prepared by the preparation method, and the microporous pure protein fiber comprises the following raw materials in percentage by mass: 0.1 to 0.3 percent of protein coagulant, 99.7 to 99.9 percent of protein slurry; preferably, the protein coagulant is 0.2%, and the protein slurry is supplemented to 100%.
Further, the preparation raw materials of the protein slurry comprise the following components in percentage by mass: 5% -85% of protein, and the balance of water is supplemented to 100%; the mass percentage of the protein in the raw materials for preparing the protein slurry may be 5%, 25%, 45%, 60%, 75%, 85%, etc., but is not limited to the values listed, and any value within the above-mentioned numerical range is applicable.
The preparation steps of the protein slurry are as follows: and uniformly mixing the protein and water at the temperature of 5-40 ℃ to obtain the protein slurry. The temperature may be 5℃and 15℃and 20℃and 30℃and 40℃respectively, but the values are not limited to the values listed, and any values within the above-mentioned range may be used.
Further, the protein comprises one or more of milk protein, peanut protein, corn cheese, fibroin and collagen.
Further, the protein contains one or more of cysteine, leucine, isoleucine, glycine, methionine, tyrosine, histidine, threonine, alanine, tryptophan, lysine, aspartic acid, valine, phenylalanine, proline, serine, glutamic acid and arginine;
preferably, the protein contains threonine, aspartic acid, serine and arginine, wherein the molar ratio of threonine, aspartic acid, serine and arginine is (2-3): (0.5-1.5): (1-2): (2.5-3.5). Preferably, the molar ratio of threonine, aspartic acid, serine, arginine is 2.5:1:1.5:3.
according to the preparation method of the microporous pure protein fiber, if the boiling aqueous solution is directly added into the protein slurry at 50-60 ℃, the surface and the inner nanocrystal cores of the coagulated protein slurry are closely stacked together, and bubbles are easy to break after being treated by a low-temperature condensation technology, so that the opening rate of the protein fiber is low and the strength is reduced. In order to solve the technical problems, the inventor carries out improved research on the preparation method, and discovers that when a multifunctional small molecule is introduced into boiling aqueous solution and is added into protein slurry at 50-60 ℃, the pre-orientation degree of the external and surface nanocrystal cores of the protein slurry can be controlled, the dimensional stability and the pore uniformity of a pore structure are improved, on one hand, the problem that pure protein fibers are easy to crack in the prior art is solved, and the dry breaking strength of the protein fibers reaches 0.8-2.5 cN/dtex; on the other hand, the high-bulking degree of the pure protein fiber is endowed, and the softness and skin-friendly property of the pure protein fiber are improved.
The invention has the beneficial effects that:
the preparation method of the microporous pure protein fiber provided by the invention adopts pure natural, safe and harmless preparation raw materials, does not use a chemical fiber carrier, and uses an ultralow-temperature congealing technology to prepare the microporous pure protein fiber by condensation shaping, wherein the fiber has multiple functions of softness, light weight, warmth retention, moisture retention and the like, the total protein content is more than 99%, the fiber moisture regain is more than 60%, and the fiber hollow rate is more than 30%.
Detailed Description
For further understanding of the present invention, the following description will clearly and fully describe the technical solutions of the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. 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.
Materials, reagents and the like used in the examples described below are commercially available unless otherwise specified.
The experimental methods used in the following examples are conventional methods unless otherwise specified.
The invention provides a preparation method of microporous pure protein fiber, which comprises the following steps:
firstly, adding 5-85% by mass of protein into water with the total mass of the protein and the water being 100%, and uniformly mixing the protein and the water at 5-40 ℃ to prepare protein slurry;
then, the protein slurry with the mass percentage of 99.7 to 99.9 percent is boiled according to the total mass of the protein slurry and the protein coagulant of 100 percent, and then the temperature is reduced to 50 to 60 ℃ at the speed of 2 to 5 ℃/min, and the volume ratio of the boiling hot solution to the protein slurry is (5 to 15): (300-500), adding boiling hot solution with the concentration of 20-60 mg/mL, then adding protein coagulant, and sequentially performing standing sedimentation, suction filtration and dry spinning operation; it should be noted that the steps of sedimentation, suction filtration and dry spinning adopted in the present invention are all common methods and operation steps in the field, and are not described herein;
finally, condensing for 0.5 min-1440 min at the temperature of minus 196 ℃ to minus 20 ℃ and performing low-temperature condensation shaping to obtain the microporous pure protein fiber.
The proteins used in the above method comprise one or more of milk protein, peanut protein, corn cheese, fibroin and collagen; the protein coagulant comprises one or more of magnesium chloride, calcium sulfate, magnesium sulfate, calcium chloride, sodium carbonate, acetic acid, sodium hydroxide, urea, acetone, ethanol, hydrochloric acid, sulfuric acid, ammonium sulfate, sodium phosphate and sodium sulfate; the boiling hot solution is an aqueous solution comprising one or more of 1, 3-dimethylol urea, L-citrulline, N-acetyl-D-alanine, L-theanine, 1-amino ring Ding Jiasuan, L-glutamine, boc-D-serine, malonic acid, citric acid, butane tetracarboxylic acid, and citric acid betaine.
The specific surface area of the microporous pure protein fiber prepared by the preparation method is 1000-1200 m 2 Per gram, the relative density is 0.02-0.04 g/m 3 The moisture regain is 60-75%, the fineness is 0.7-5D, the dry breaking strength is 1.0-2.5 CN/DTEX, and the biodegradation rate is 100%.
Example 1
The embodiment provides a preparation method of microporous pure protein fiber, which comprises the following steps:
adding 50% by mass of peanut protein into water with the total mass of the peanut protein and the water being 100%, and uniformly mixing the peanut protein and the water at 25 ℃ to obtain peanut protein slurry;
the peanut protein pulp with the mass percentage of 99.8 percent is boiled to be cooled to 55 ℃ at the speed of 3 ℃/min based on 100 percent of the total mass of the peanut protein pulp and the magnesium chloride, and the volume ratio of the 1, 3-dimethylol urea solution to the peanut protein pulp is 10:400, adding boiling 1, 3-dimethylol urea aqueous solution with the concentration of 40mg/mL, and then adding magnesium chloride;
sequentially performing standing sedimentation, suction filtration and dry spinning operation, condensing for 0.5min at the temperature of-196 ℃, and shaping to obtain the microporous pure protein fiber.
Example 2
Adding 85% fibroin into water with the total mass of fibroin and water being 100%, and uniformly mixing fibroin and water at 40 ℃ to obtain fibroin slurry;
boiling fibroin slurry with the mass percentage of 99.9 percent based on 100 percent of the total mass of the fibroin slurry and the ethanol, cooling to 60 ℃ at the speed of 5 ℃/min, and mixing the L-theanine solution with the fibroin slurry according to the volume ratio of 15:500, adding boiling L-theanine aqueous solution with the concentration of 60mg/mL, and then adding ethanol;
sequentially performing standing sedimentation, suction filtration and dry spinning operation, condensing for 720min at the temperature of minus 100 ℃, and shaping to obtain the microporous pure protein fiber.
Example 3
Adding 5% by mass of milk protein into water with the total mass of the milk protein and the water being 100%, and uniformly mixing the milk protein and the water at 5 ℃ to obtain milk protein slurry;
the milk protein slurry with the mass percentage of 99.7 percent is boiled to be cooled to 50 ℃ at the speed of 2 ℃/min based on 100 percent of the total mass of the milk protein slurry and the sodium sulfate, and the volume ratio of the citric acid solution to the milk protein slurry is 5:300, adding boiling citric acid aqueous solution with the concentration of 20mg/mL, and then adding sodium sulfate;
sequentially performing standing sedimentation, suction filtration and dry spinning operation, condensing for 1440min at-20 ℃, and shaping to obtain microporous pure protein fiber.
To demonstrate the unique advantages of the microporous pure protein fibers prepared by the method of the present invention, protein fibers prepared by the following comparative examples were provided and subjected to comparative experiments.
Comparative example 1
The preparation method of this comparative example was the same as in example 2, except that the temperature of the low-temperature condensing setting was 20℃and the condensing time was 1440min.
Comparative example 2
The preparation method of this comparative example was the same as in example 2, except that the boiling hot solution was directly added without the step of cooling to 50 to 60 ℃ after boiling the protein slurry. The preparation method comprises the following specific steps:
adding 85% fibroin into water with the total mass of fibroin and water being 100%, and uniformly mixing fibroin and water at 40 ℃ to obtain fibroin slurry;
the fibroin slurry with the mass percentage of 99.9 percent is boiled according to the total mass of the fibroin slurry and the ethanol of 100 percent, and the volume ratio of the L-theanine solution to the fibroin slurry is 15:500, adding boiling aqueous L-theanine solution with a concentration of 60mg/mL, followed by ethanol;
sequentially performing standing sedimentation, suction filtration and dry spinning operation, condensing for 720min at the temperature of minus 100 ℃, and shaping to obtain the microporous pure protein fiber.
Comparative example 3
The preparation method of this comparative example was the same as in example 2, except that the boiling hot solution was replaced with a boiling aqueous solution.
Comparative example 4
The preparation method of this comparative example was the same as in example 2, except that the fibroin slurry was boiled and then cooled to 60℃at a rate of 20℃per minute.
Test examples
The microporous pure protein fibers prepared in examples 1 to 3 and comparative examples 1 to 4 were subjected to performance test.
Adopting a Bet specific surface area tester to test the specific surface area; relative density tests were performed on a water basis, see GB/T4472-2011; the moisture regain test is carried out by referring to GB/T9994-2018; performing a dry crack strength test by referring to GB/T14337; meanwhile, a total organic carbon analyzer is adopted to test the biodegradation rate according to GB/T19277.1-2011. The test results are shown in table 1 below:
table 1 table of data from performance tests
As can be seen from the comparison of the experimental data, the protein fiber cannot be molded by adopting the preparation method of the comparative example 1, and the pure protein fiber with excellent physical properties cannot be obtained, which indicates that the condensation time and stability in the preparation process are important for molding the protein fiber; if the cooling step (comparative example 2) in boiling the protein slurry and boiling hot solution is omitted, the specific surface area, moisture regain and dry break strength of the protein fiber are reduced; when the boiling hot solution containing the polyfunctional substance was replaced with the boiling water solution (comparative example 3), the specific surface area of the protein fiber was changed from 1200m 2 The/g drop is 700m 2 Per g, relative density is from 0.032g/m 3 Up to 0.6g/m 3 The dry breaking strength is also reduced to 0.5cN/dtex, which indicates that boiling the hot solution can promote the pore-forming rate of bubbles in the fiber; the rate of cooling in comparative example 4 was not in the range of 2-8 deg.C/min, and the dry break strength of the protein was reduced to 0.4cN/dtex.
The foregoing description is only a preferred embodiment of the present invention and is not intended to limit the present invention, but although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the technical solutions described in the foregoing embodiments, or that equivalents may be substituted for part of the technical features thereof. Any modification, equivalent replacement, variation, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. A method for preparing microporous pure protein fiber, which is characterized by comprising the following steps:
after the protein slurry is boiled, the temperature is reduced to 50-60 ℃ at a temperature reduction rate of 2-8 ℃/min, and the volume ratio of the boiling hot solution to the protein slurry is (5-15): adding boiling hot solution in the proportion of (300-500), then adding protein coagulant, and carrying out standing sedimentation, suction filtration, dry spinning and low-temperature condensation shaping to obtain microporous pure protein fibers;
the boiling hot solution is an aqueous solution of a multifunctional small molecular compound selected from one or more of 1, 3-dimethylol urea, L-citrulline, N-acetyl-D-alanine, L-theanine, 1-amino ring Ding Jiasuan, L-glutamine, boc-D-serine, malonic acid, citric acid, butane tetracarboxylic acid and citric acid betaine;
the condensing temperature in the low-temperature condensing and shaping step is minus 196 ℃ to minus 20 ℃ and the condensing time is 0.5min to 1440min.
2. The method of claim 1, wherein the volume ratio of boiling hot solution to protein slurry is 10:400.
3. The preparation method of claim 1, wherein the mass concentration of the aqueous solution of the multifunctional small molecular compound is 20-60 mg/mL.
4. The method of claim 1, wherein the protein coagulant comprises one or more of magnesium chloride, calcium sulfate, magnesium sulfate, calcium chloride, sodium carbonate, acetic acid, sodium hydroxide, urea, acetone, ethanol, hydrochloric acid, sulfuric acid, ammonium sulfate, sodium phosphate, sodium sulfate.
5. A microporous pure protein fiber prepared by the preparation method according to any one of claims 1 to 4, wherein the raw materials of the microporous pure protein fiber comprise the following components in percentage by mass: 0.1-0.3% of protein coagulant and 99.7-99.9% of protein slurry.
6. The microporous pure protein fiber according to claim 5, wherein the raw materials for preparing the protein slurry comprise the following components in percentage by mass: 5% -85% of protein and the balance of water to 100%; the preparation steps of the protein slurry are as follows: and uniformly mixing the protein and water at the temperature of 5-40 ℃ to obtain the protein slurry.
7. The microporous pure protein fiber of claim 6, wherein the protein comprises one or more of milk protein, peanut protein, corn cheese, silk protein, collagen.
8. The microporous pure protein fiber according to claim 6, wherein the protein contains one or more of cysteine, leucine, isoleucine, glycine, methionine, tyrosine, histidine, threonine, alanine, tryptophan, lysine, aspartic acid, valine, phenylalanine, proline, serine, glutamic acid, arginine.
9. The microporous pure protein fiber according to claim 8, wherein the protein contains threonine, aspartic acid, serine and arginine, wherein the molar ratio of threonine, aspartic acid, serine and arginine is (2-3): 0.5-1.5): 1-2): 2.5-3.5.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5750064A (en) * | 1996-01-19 | 1998-05-12 | E. I. Du Pont De Nemours And Company | Dry spinning process for producing zein fibers |
| CN101724920A (en) * | 2009-11-13 | 2010-06-09 | 东华大学 | Method for preparing regenerated silk fiber by means of dry spinning |
| CN102181957A (en) * | 2011-03-30 | 2011-09-14 | 东华大学 | Preparation method for regenerated fibroin fiber |
| CN110512300A (en) * | 2018-05-22 | 2019-11-29 | 浙江大学 | Preparation method, product and application of antibacterial porous fiber with oriented pore structure |
| CN114134587A (en) * | 2021-12-24 | 2022-03-04 | 上海天同纺织科技有限公司 | Preparation method of high-performance regenerated pure keratin fiber |
-
2022
- 2022-08-02 CN CN202210920855.0A patent/CN115198386B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5750064A (en) * | 1996-01-19 | 1998-05-12 | E. I. Du Pont De Nemours And Company | Dry spinning process for producing zein fibers |
| CN101724920A (en) * | 2009-11-13 | 2010-06-09 | 东华大学 | Method for preparing regenerated silk fiber by means of dry spinning |
| CN102181957A (en) * | 2011-03-30 | 2011-09-14 | 东华大学 | Preparation method for regenerated fibroin fiber |
| CN110512300A (en) * | 2018-05-22 | 2019-11-29 | 浙江大学 | Preparation method, product and application of antibacterial porous fiber with oriented pore structure |
| CN114134587A (en) * | 2021-12-24 | 2022-03-04 | 上海天同纺织科技有限公司 | Preparation method of high-performance regenerated pure keratin fiber |
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