CN112760745A - Textile fiber with radiation protection function and preparation method thereof - Google Patents
Textile fiber with radiation protection function and preparation method thereof Download PDFInfo
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- CN112760745A CN112760745A CN202110064787.8A CN202110064787A CN112760745A CN 112760745 A CN112760745 A CN 112760745A CN 202110064787 A CN202110064787 A CN 202110064787A CN 112760745 A CN112760745 A CN 112760745A
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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
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/02—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from cellulose, cellulose derivatives, or proteins
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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
- 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
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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
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/10—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained by reactions only involving carbon-to-carbon unsaturated bonds as constituent
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Abstract
The invention discloses a textile fiber with radiation protection function and a preparation method thereof, which utilizes steam containing silver ions to carry out high-pressure flash explosion on feather fiber, so that protein hydrophilic groups are exposed, and the silver ions are combined on a peptide chain, so that regenerated protein fiber obtains the function of preventing ionizing radiation; the disulfide threitol is utilized to extend the inherent disulfide bond of the keratin, so that the keratin recovers better mechanical property; the steam explosion improves the yield of the regenerated protein fiber. A proper amount of cysteine complexing agent is added in the preparation process of the nano titanium dioxide photocatalyst sol, and the amino group of the cysteine complexing agent is complexed with Ti, so that the nano titanium dioxide can be effectively prevented from polymerizing and precipitating, and the amino group of the cysteine complexing agent is better combined with regenerated protein fibers to obtain the regenerated protein fibers with radiation protection; cysteine-SH can be combined with free sulfydryl of the regenerated protein fiber to form a new disulfide bond, so that the binding property of the regenerated protein fiber and the nano titanium dioxide photocatalyst sol is enhanced, and the mechanical property of the regenerated protein fiber is further improved.
Description
Technical Field
The invention relates to the technical field of fibers, in particular to a textile fiber with a radiation-proof function and a preparation method thereof.
Background
With the rapid development of the global intensive breeding industry, the lack of protein feed resources seriously restricts the sustainable development of the breeding industry. The protein content of the poultry feather is as high as about 90 percent, and the poultry feather is considered as a protein resource with great potential value internationally. China has abundant bulk low-value protein resources such as feathers, and only about 70 ten thousand tons of feather leftovers are produced every year, but feather keratin has a complex structure and hard texture and is insoluble in water, so the bioavailability of the feather keratin is improved by physical or chemical means. Without proper processing, the feather has little value in utilization and causes environmental pollution.
The feather keratin is regenerated to prepare the regenerated keratin fiber, and waste resources can be effectively utilized. The environment pollution is serious, the ionizing radiation is filled around the human body, and the ultraviolet ray injury is also great.
Therefore, it is necessary to design a textile fiber with radiation protection function and a preparation method thereof, which utilizes the modified regenerated keratin and resists the ionizing radiation and the ultraviolet radiation.
Disclosure of Invention
The invention aims to provide a textile fiber with a radiation protection function and a preparation method thereof, so as to solve the problems in the background technology.
In order to solve the technical problems, the invention provides the following technical scheme: a textile fiber with radiation protection function comprises the following steps:
the method comprises the following steps: carrying out flash explosion treatment on animal feathers at 1.2-2.5 KPa;
step two: adding the exploded and flashed feather into a protein dissolving solution, hermetically stirring for 12h at 70 ℃, and centrifuging to remove undissolved feather residues to obtain a keratin solution;
step three: adding a proper amount of hydrochloric acid and sodium sulfate into the keratin solution obtained in the step two to precipitate and separate out keratin at the isoelectric point (pH4.6) of the keratin solution, thereby obtaining regenerated keratin;
step four: preparing nano titanium dioxide photocatalyst sol, and soaking the regenerated keratin obtained in the step three in the prepared nano titanium dioxide photocatalyst sol to obtain modified regenerated keratin;
step five: the modified regenerated keratin and polyvinyl alcohol are blended, and a textile fiber finished product is spun by a wet spinning process.
According to the technical scheme, the specific method for treating the animal feathers by flash explosion comprises the following steps: putting the feather into a steam flash explosion machine reactor, adding silver ions into steam, processing for 1-5min under 1.2-2.5KPa, then instantly releasing pressure within 0.1s, and collecting a steam explosion sample for later use.
According to the above technical scheme, the preparation of the regenerated keratin: soaking the feather treated in the first step in 4 mmol/L1, 4-dithiothreitol solution, hermetically stirring at 70 ℃ for 12h, and centrifuging to remove undissolved feather residues to obtain keratin solution.
According to the technical scheme, the preparation of the nano titanium dioxide photocatalyst sol comprises the following steps: slowly dripping titanium tetrachloride into distilled water to form a uniform and transparent titanium compound solution A, dissolving ammonium metavanadate in the titanium compound solution A, adjusting the pH value with ammonia water to form a colloidal solution B, filtering and washing the solution B, and adding a cysteine complexing agent into a filter cake.
According to the technical scheme, the preparation of the titanium compound solution A comprises the following steps: 0.1mol/L titanium tetrachloride was added dropwise at a rate of 1d/s to 20 times deionized water to give a colorless clear solution.
According to the technical scheme, the preparation of the nano titanium dioxide photocatalyst sol comprises the following steps: adding a titanium compound solution A into a solution of 1: 1, adjusting the pH value to 7-8 by ammonia water, and stirring while adding to obtain white colloidal precipitate; carrying out vacuum filtration on the solution B, carrying out oil bath on the prepared sol at 100 ℃ for 6h, and washing out chloride ions in the sol to obtain light yellow transparent vanadium-nitrogen co-doped nano titanium dioxide transparent photocatalyst sol; slowly dripping cysteine complexing agent into the vanadium-nitrogen co-doped nano titanium dioxide transparent photocatalyst sol under the condition of rapid stirring, stirring for a period of time after dripping is finished, uniformly mixing the two, and sealing and standing at room temperature for later use.
According to the above technical scheme, the preparation of the modified regenerated keratin comprises the following steps: and (3) soaking the regenerated keratin obtained in the step (three) in the prepared nano titanium dioxide photocatalyst sol for 1-3 days, and continuously stirring at the temperature of 30-38 ℃ in the soaking process to obtain the modified regenerated keratin.
According to the technical scheme, the blending method of the modified regenerated keratin and the polyvinyl alcohol comprises the following steps: dissolving the modified regenerated keratin in hexafluoroisopropanol, and stirring for 1h on a stirring machine at normal temperature to obtain a modified regenerated keratin solution with the mass fraction of 15%; preparing a polyvinyl alcohol/hexafluoroisopropanol solution with the mass fraction of 2% at 80 ℃, and mixing the two solutions according to the keratin content of 70% respectively at 40 ℃; and stirring the mixed solution on a magnetic stirring machine for 1 hour at normal temperature to fully mix the keratin and the polyvinyl alcohol to prepare a mixed solution, standing the mixed solution for 2 hours for defoaming, and thus obtaining the spinning solution.
According to the technical scheme, the wet spinning process method comprises the following steps: the spinning speed of the spinning solution is controlled by a metering pump, the spinning solution passes through a spinning nozzle and enters hexanol solution, and moisture and reaction residual substances are removed and solidified into filaments; the coagulation bath is kept for about 10s, and the coagulation bath is wound on a drawing roller A through a godet roller and enters a drawing main roller B, the speed of a roller C is not too high, and otherwise, the filament is easy to break.
According to the technical scheme, the textile fiber with the radiation protection function prepared by the preparation method of the textile fiber with the radiation protection function mainly comprises the following raw material components in parts by weight: 40-50 parts of regenerated keratin, 1-5 parts of nano titanium dioxide photocatalyst gel and 10-12.5 parts of polyvinyl alcohol.
Compared with the prior art, the invention has the following beneficial effects: in the invention, the raw materials are mixed,
(1) performing high-pressure flash explosion on the feather fibers by using the steam added with silver ions, so that the feather fiber structure is obviously damaged and the regular and compact structure gradually disappears; the space between the crystal faces of the feather fibers is increased, and the crystallinity is obviously reduced; the conformation of the feather fiber macromolecule peptide segment is changed from intermolecular beta folding to intramolecular beta folding, the association of hydrogen bonds among peptide chains is weakened, the relative content of beta folding is obviously reduced, and the relative content of random coil is increased; the microstructure of the protein crystal is destroyed, the melting temperature is reduced, so that part of hydrophilic groups in the protein molecule are exposed to form hydrogen bonds with water molecules, and silver ions are also bonded to the peptide chain, so that the regenerated protein fiber has the function of preventing ionizing radiation; then, dithiothreitol with a dithiol structure is used for extending the inherent disulfide bond of the keratin, so that the regenerated protein fiber can recover better mechanical property; the yield of the regenerated protein fiber is improved by steam explosion;
(2) the preparation process of the nano titanium dioxide photocatalyst sol slowly drops titanium chloride into distilled water to form a uniform and transparent titanium compound solution A, then a proper amount of ammonium metavanadate is dissolved in the transparent solution, the pH value is adjusted by ammonia water to form a colloidal solution B, the colloidal solution B is filtered and washed, a proper amount of cysteine complexing agent is added into a filter cake, the cysteine complexing agent has an antioxidation effect, the amino group of the cysteine complexing agent is complexed with Ti to effectively prevent the nano titanium dioxide from polymerizing and prevent the nano titanium dioxide from precipitating, the aggregation and precipitation of the titanium dioxide seriously influence the combination effect of the titanium dioxide and protein fibers, and the sol prepared by the complexing agent is not easy to precipitate;
(3) soaking the regenerated protein fiber subjected to dithiol chain extension into the nano titanium dioxide photocatalyst sol, and continuously stirring in the soaking process to obtain the regenerated protein fiber with radiation protection; cysteine-SH can be combined with free sulfydryl of the regenerated protein fiber to form a new disulfide bond, so that the binding property of the regenerated protein fiber and the nano titanium dioxide photocatalyst sol is enhanced, and the mechanical property of the regenerated protein fiber is further improved.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides the technical scheme that: a textile fiber with a radiation protection function comprises the following raw material components in parts by weight: 40-50 parts of regenerated keratin, 1-5 parts of nano titanium dioxide photocatalyst gel and 10-12.5 parts of polyvinyl alcohol.
A preparation method of textile fiber with radiation protection function comprises the following steps:
the method comprises the following steps: carrying out flash explosion treatment on animal feathers at 1.2-2.5 KPa;
step two: adding the exploded and flashed feather into a protein dissolving solution, hermetically stirring for 12h at 70 ℃, and centrifuging to remove undissolved feather residues to obtain a keratin solution;
step three: adding a proper amount of hydrochloric acid and sodium sulfate into the keratin solution obtained in the step two to precipitate and separate out keratin at the isoelectric point (pH4.6) of the keratin solution, thereby obtaining regenerated keratin;
step four: preparing nano titanium dioxide photocatalyst sol, and soaking the regenerated keratin obtained in the step three in the prepared nano titanium dioxide photocatalyst sol to obtain modified regenerated keratin;
step five: the modified regenerated keratin and polyvinyl alcohol are blended, and a textile fiber finished product is spun by a wet spinning process.
According to the technical scheme, the specific method for treating the animal feathers by flash explosion comprises the following steps: putting the feather into a steam flash explosion machine reactor, adding silver ions into steam, processing for 1-5min under 1.2-2.5KPa, then instantly releasing pressure within 0.1s, and collecting a steam explosion sample for later use.
According to the above technical scheme, the preparation of the regenerated keratin: soaking the feather treated in the first step in 4 mmol/L1, 4-dithiothreitol solution, hermetically stirring at 70 ℃ for 12h, and centrifuging to remove undissolved feather residues to obtain keratin solution.
According to the technical scheme, the preparation of the nano titanium dioxide photocatalyst sol comprises the following steps: slowly dripping titanium tetrachloride into distilled water to form a uniform and transparent titanium compound solution A, dissolving ammonium metavanadate in the titanium compound solution A, adjusting the pH value with ammonia water to form a colloidal solution B, filtering and washing the solution B, and adding a cysteine complexing agent into a filter cake.
According to the technical scheme, the preparation of the titanium compound solution A comprises the following steps: 0.1mol/L titanium tetrachloride was added dropwise at a rate of 1d/s to 20 times deionized water to give a colorless clear solution.
According to the technical scheme, the preparation of the nano titanium dioxide photocatalyst sol comprises the following steps: adding a titanium compound solution A into a solution of 1: 1, adjusting the pH value to 7-8 by ammonia water, and stirring while adding to obtain white colloidal precipitate; carrying out vacuum filtration on the solution B, carrying out oil bath on the prepared sol at 100 ℃ for 6h, and washing out chloride ions in the sol to obtain light yellow transparent vanadium-nitrogen co-doped nano titanium dioxide transparent photocatalyst sol; slowly dripping cysteine complexing agent into the vanadium-nitrogen co-doped nano titanium dioxide transparent photocatalyst sol under the condition of rapid stirring, stirring for a period of time after dripping is finished, uniformly mixing the two, and sealing and standing at room temperature for later use.
According to the above technical scheme, the preparation of the modified regenerated keratin comprises the following steps: and (3) soaking the regenerated keratin obtained in the step (three) in the prepared nano titanium dioxide photocatalyst sol for 1-3 days, and continuously stirring at the temperature of 30-38 ℃ in the soaking process to obtain the modified regenerated keratin.
According to the technical scheme, the blending method of the modified regenerated keratin and the polyvinyl alcohol comprises the following steps: dissolving the modified regenerated keratin in hexafluoroisopropanol, and stirring for 1h on a stirring machine at normal temperature to obtain a modified regenerated keratin solution with the mass fraction of 15%; preparing a polyvinyl alcohol/hexafluoroisopropanol solution with the mass fraction of 2% at 80 ℃, and mixing the two solutions according to the keratin content of 70% respectively at 40 ℃; and stirring the mixed solution on a magnetic stirring machine for 1 hour at normal temperature to fully mix the keratin and the polyvinyl alcohol to prepare a mixed solution, standing the mixed solution for 2 hours for defoaming, and thus obtaining the spinning solution.
According to the technical scheme, the wet spinning process method comprises the following steps: the spinning speed of the spinning solution is controlled by a metering pump, the spinning solution passes through a spinning nozzle and enters hexanol solution, and moisture and reaction residual substances are removed and solidified into filaments; the coagulation bath is kept for about 10s, and the coagulation bath is wound on a drawing roller A through a godet roller and enters a drawing main roller B, the speed of a roller C is not too high, and otherwise, the filament is easy to break.
Example 1
A textile fiber with a radiation protection function comprises the following raw material components in parts by weight: 40 parts of regenerated keratin, 3 parts of nano titanium dioxide photocatalyst gel and 10 parts of polyvinyl alcohol.
A preparation method of textile fiber with radiation protection function comprises the following steps:
the method comprises the following steps: carrying out flash explosion treatment on animal feathers at 1.8 KPa;
step two: adding the exploded and flashed feather into a protein dissolving solution, hermetically stirring for 12h at 70 ℃, and centrifuging to remove undissolved feather residues to obtain a keratin solution;
step three: adding a proper amount of hydrochloric acid and sodium sulfate into the keratin solution obtained in the step two to precipitate and separate out keratin at the isoelectric point (pH4.6) of the keratin solution, thereby obtaining regenerated keratin;
step four: preparing nano titanium dioxide photocatalyst sol, and soaking the regenerated keratin obtained in the step three in the prepared nano titanium dioxide photocatalyst sol to obtain modified regenerated keratin;
step five: the modified regenerated keratin and polyvinyl alcohol are blended, and a textile fiber finished product is spun by a wet spinning process.
According to the technical scheme, the specific method for treating the animal feathers by flash explosion comprises the following steps: putting the feather into a steam flash explosion machine reactor, adding silver ions into steam, treating for 1-5min at 1.8KPa, then instantly releasing pressure within 0.1s, and collecting a steam explosion sample for later use.
According to the above technical scheme, the preparation of the regenerated keratin: soaking the feather treated in the first step in 4 mmol/L1, 4-dithiothreitol solution, hermetically stirring at 70 ℃ for 12h, and centrifuging to remove undissolved feather residues to obtain keratin solution.
According to the technical scheme, the preparation of the nano titanium dioxide photocatalyst sol comprises the following steps: slowly dripping titanium tetrachloride into distilled water to form a uniform and transparent titanium compound solution A, dissolving ammonium metavanadate in the titanium compound solution A, adjusting the pH value with ammonia water to form a colloidal solution B, filtering and washing the solution B, and adding a cysteine complexing agent into a filter cake.
According to the technical scheme, the preparation of the titanium compound solution A comprises the following steps: 0.1mol/L titanium tetrachloride was added dropwise at a rate of 1d/s to 20 times deionized water to give a colorless clear solution.
According to the technical scheme, the preparation of the nano titanium dioxide photocatalyst sol comprises the following steps: adding a titanium compound solution A into a solution of 1: 1, adjusting the pH value to 7.5 by ammonia water, and stirring while adding to obtain white colloidal precipitate; carrying out vacuum filtration on the solution B, carrying out oil bath on the prepared sol at 100 ℃ for 6h, and washing out chloride ions in the sol to obtain light yellow transparent vanadium-nitrogen co-doped nano titanium dioxide transparent photocatalyst sol; slowly dripping cysteine complexing agent into the vanadium-nitrogen co-doped nano titanium dioxide transparent photocatalyst sol under the condition of rapid stirring, stirring for a period of time after dripping is finished, uniformly mixing the two, and sealing and standing at room temperature for later use.
According to the above technical scheme, the preparation of the modified regenerated keratin comprises the following steps: and (3) soaking the regenerated keratin obtained in the step (three) in the prepared nano titanium dioxide photocatalyst sol for 2d, and continuously stirring at the temperature of 35 ℃ in the soaking process to obtain the modified regenerated keratin.
According to the technical scheme, the blending method of the modified regenerated keratin and the polyvinyl alcohol comprises the following steps: dissolving the modified regenerated keratin in hexafluoroisopropanol, and stirring for 1h on a stirring machine at normal temperature to obtain a modified regenerated keratin solution with the mass fraction of 15%; preparing a polyvinyl alcohol/hexafluoroisopropanol solution with the mass fraction of 2% at 80 ℃, and mixing the two solutions according to the keratin content of 70% respectively at 40 ℃; and stirring the mixed solution on a magnetic stirring machine for 1 hour at normal temperature to fully mix the keratin and the polyvinyl alcohol to prepare a mixed solution, standing the mixed solution for 2 hours for defoaming, and thus obtaining the spinning solution.
According to the technical scheme, the wet spinning process method comprises the following steps: the spinning speed of the spinning solution is controlled by a metering pump, the spinning solution passes through a spinning nozzle and enters hexanol solution, and moisture and reaction residual substances are removed and solidified into filaments; the coagulation bath is kept for about 10s, and the coagulation bath is wound on a drawing roller A through a godet roller and enters a drawing main roller B, the speed of a roller C is not too high, and otherwise, the filament is easy to break.
Example 2
A textile fiber with a radiation protection function comprises the following raw material components in parts by weight: 50 parts of regenerated keratin, 5 parts of nano titanium dioxide photocatalyst gel and 12.5 parts of polyvinyl alcohol.
A preparation method of textile fiber with radiation protection function comprises the following steps:
the method comprises the following steps: carrying out flash explosion treatment on animal feathers at 1.6 KPa;
step two: adding the exploded and flashed feather into a protein dissolving solution, hermetically stirring for 12h at 70 ℃, and centrifuging to remove undissolved feather residues to obtain a keratin solution;
step three: adding a proper amount of hydrochloric acid and sodium sulfate into the keratin solution obtained in the step two to precipitate and separate out keratin at the isoelectric point (pH4.6) of the keratin solution, thereby obtaining regenerated keratin;
step four: preparing nano titanium dioxide photocatalyst sol, and soaking the regenerated keratin obtained in the step three in the prepared nano titanium dioxide photocatalyst sol to obtain modified regenerated keratin;
step five: the modified regenerated keratin and polyvinyl alcohol are blended, and a textile fiber finished product is spun by a wet spinning process.
According to the technical scheme, the specific method for treating the animal feathers by flash explosion comprises the following steps: putting the feathers into a steam flash explosion reactor, adding silver ions into steam, processing for 3min under 1.6KPa, then instantly releasing pressure within 0.1s, and collecting a steam explosion sample for later use.
According to the above technical scheme, the preparation of the regenerated keratin: soaking the feather treated in the first step in 4 mmol/L1, 4-dithiothreitol solution, hermetically stirring at 70 ℃ for 12h, and centrifuging to remove undissolved feather residues to obtain keratin solution.
According to the technical scheme, the preparation of the nano titanium dioxide photocatalyst sol comprises the following steps: slowly dripping titanium tetrachloride into distilled water to form a uniform and transparent titanium compound solution A, dissolving ammonium metavanadate in the titanium compound solution A, adjusting the pH value with ammonia water to form a colloidal solution B, filtering and washing the solution B, and adding a cysteine complexing agent into a filter cake.
According to the technical scheme, the preparation of the titanium compound solution A comprises the following steps: 0.1mol/L titanium tetrachloride was added dropwise at a rate of 1d/s to 20 times deionized water to give a colorless clear solution.
According to the technical scheme, the preparation of the nano titanium dioxide photocatalyst sol comprises the following steps: adding a titanium compound solution A into a solution of 1: 1, adjusting the pH value to 7.8 by ammonia water, and stirring while adding to obtain white colloidal precipitate; carrying out vacuum filtration on the solution B, carrying out oil bath on the prepared sol at 100 ℃ for 6h, and washing out chloride ions in the sol to obtain light yellow transparent vanadium-nitrogen co-doped nano titanium dioxide transparent photocatalyst sol; slowly dripping cysteine complexing agent into the vanadium-nitrogen co-doped nano titanium dioxide transparent photocatalyst sol under the condition of rapid stirring, stirring for a period of time after dripping is finished, uniformly mixing the two, and sealing and standing at room temperature for later use.
According to the above technical scheme, the preparation of the modified regenerated keratin comprises the following steps: and (3) soaking the regenerated keratin obtained in the step (three) in the prepared nano titanium dioxide photocatalyst sol for 2d, and continuously stirring at the temperature of 36 ℃ in the soaking process to obtain the modified regenerated keratin.
According to the technical scheme, the blending method of the modified regenerated keratin and the polyvinyl alcohol comprises the following steps: dissolving the modified regenerated keratin in hexafluoroisopropanol, and stirring for 1h on a stirring machine at normal temperature to obtain a modified regenerated keratin solution with the mass fraction of 15%; preparing a polyvinyl alcohol/hexafluoroisopropanol solution with the mass fraction of 2% at 80 ℃, and mixing the two solutions according to the keratin content of 70% respectively at 40 ℃; and stirring the mixed solution on a magnetic stirring machine for 1 hour at normal temperature to fully mix the keratin and the polyvinyl alcohol to prepare a mixed solution, standing the mixed solution for 2 hours for defoaming, and thus obtaining the spinning solution.
According to the technical scheme, the wet spinning process method comprises the following steps: the spinning speed of the spinning solution is controlled by a metering pump, the spinning solution passes through a spinning nozzle and enters hexanol solution, and moisture and reaction residual substances are removed and solidified into filaments; the coagulation bath is kept for about 10s, and the coagulation bath is wound on a drawing roller A through a godet roller and enters a drawing main roller B, the speed of a roller C is not too high, and otherwise, the filament is easy to break.
In order to verify the beneficial effects of the invention, the following tests are specially carried out:
test 1 Wet tensile Property test
Preparing a regenerated modified keratin film soaked with nano titanium dioxide photocatalyst sol and a regenerated keratin film not soaked with sol on glass, balancing the film for 48 hours in a humid environment (21 ℃, 90 percent RH), testing according to an ASTM D882-02 method, and testing the tensile property of a film sample on a universal material tester. The grip interval and the grip separation speed were set to 50mm and 50mm/min, respectively, and the sample size was 10mm × 100 mm. Before testing, the samples were equilibrated for more than 48h under standard conditions (21 ℃, 65 RH%). Samples of each condition 3 identical films were prepared and 5 specimens were cut from each film for tensile testing.
TABLE 1 Keratin film tensile Property test values
As can be seen from Table 1, the regenerated keratin film prepared by the method has good mechanical properties, the tensile strength of the regenerated keratin film is further improved after the nanometer titanium dioxide photocatalyst sol is modified, and the elongation at break of the regenerated keratin film is also improved.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Finally, it should be noted that: 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 changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A preparation method of textile fiber with radiation protection function comprises the following steps:
the method comprises the following steps: carrying out flash explosion treatment on animal feathers at 1.2-2.5 KPa;
step two: adding the exploded and flashed feather into a protein dissolving solution, hermetically stirring for 12h at 70 ℃, and centrifuging to remove undissolved feather residues to obtain a keratin solution;
step three: adding a proper amount of hydrochloric acid and sodium sulfate into the keratin solution obtained in the step two to precipitate and separate out keratin at the isoelectric point (pH4.6) of the keratin solution, thereby obtaining regenerated keratin;
step four: preparing nano titanium dioxide photocatalyst sol, and soaking the regenerated keratin obtained in the step three in the prepared nano titanium dioxide photocatalyst sol to obtain modified regenerated keratin;
step five: the modified regenerated keratin and polyvinyl alcohol are blended, and a textile fiber finished product is spun by a wet spinning process.
2. The method for preparing textile fiber with radiation protection function according to claim 1, is characterized in that: step one the specific method for treating animal feathers by flash explosion comprises the following steps: putting the feather into a steam flash explosion machine reactor, adding silver ions into steam, processing for 1-5min under 1.2-2.5KPa, then instantly releasing pressure within 0.1s, and collecting a steam explosion sample for later use.
3. The method for preparing textile fiber with radiation protection function according to claim 1, is characterized in that: step two, preparation of the regenerated keratin: soaking the feather treated in the first step in 4 mmol/L1, 4-dithiothreitol solution, hermetically stirring at 70 ℃ for 12h, and centrifuging to remove undissolved feather residues to obtain keratin solution.
4. The method for preparing textile fiber with radiation protection function according to claim 1, is characterized in that: secondly, preparing the nano titanium dioxide photocatalyst sol: slowly dripping titanium tetrachloride into distilled water to form a uniform and transparent titanium compound solution A, dissolving ammonium metavanadate in the titanium compound solution A, adjusting the pH value with ammonia water to form a colloidal solution B, filtering and washing the solution B, and adding a cysteine complexing agent into a filter cake.
5. The method for preparing textile fiber with radiation protection function according to claim 4, is characterized in that: preparation of the titanium compound solution A: 0.1mol/L titanium tetrachloride was added dropwise at a rate of 1d/s to 20 times deionized water to give a colorless clear solution.
6. The method for preparing textile fiber with radiation protection function according to claim 5, is characterized in that: the preparation of the nano titanium dioxide photocatalyst sol comprises the following steps: adding a titanium compound solution A into a solution of 1: 1, adjusting the pH value to 7-8 by ammonia water, and stirring while adding to obtain white colloidal precipitate; carrying out vacuum filtration on the solution B, carrying out oil bath on the prepared sol at 100 ℃ for 6h, and washing out chloride ions in the sol to obtain light yellow transparent vanadium-nitrogen co-doped nano titanium dioxide transparent photocatalyst sol; slowly dripping cysteine complexing agent into the vanadium-nitrogen co-doped nano titanium dioxide transparent photocatalyst sol under the condition of rapid stirring, stirring for a period of time after dripping is finished, uniformly mixing the two, and sealing and standing at room temperature for later use.
7. The method for preparing textile fiber with radiation protection function according to claim 6, is characterized in that: the preparation of the modified regenerated keratin comprises the following steps: and (3) soaking the regenerated keratin obtained in the step (three) in the prepared nano titanium dioxide photocatalyst sol for 1-3 days, and continuously stirring at the temperature of 30-38 ℃ in the soaking process to obtain the modified regenerated keratin.
8. The method for preparing textile fiber with radiation protection function according to claim 7, is characterized in that: the blending method of the modified regenerated keratin and the polyvinyl alcohol comprises the following steps: dissolving the modified regenerated keratin in hexafluoroisopropanol, and stirring for 1h on a stirring machine at normal temperature to obtain a modified regenerated keratin solution with the mass fraction of 15%; preparing a polyvinyl alcohol/hexafluoroisopropanol solution with the mass fraction of 2% at 80 ℃, and mixing the two solutions according to the keratin content of 70% respectively at 40 ℃; and stirring the mixed solution on a magnetic stirring machine for 1 hour at normal temperature to fully mix the keratin and the polyvinyl alcohol to prepare a mixed solution, standing the mixed solution for 2 hours for defoaming, and thus obtaining the spinning solution.
9. The method for preparing textile fiber with radiation protection function according to claim 8, is characterized in that: the wet spinning process method comprises the following steps: the spinning speed of the spinning solution is controlled by a metering pump, the spinning solution passes through a spinning nozzle and enters hexanol solution, and moisture and reaction residual substances are removed and solidified into filaments; the coagulation bath is kept for about 10s, and the coagulation bath is wound on a drawing roller A through a godet roller and enters a drawing main roller B, the speed of a roller C is not too high, and otherwise, the filament is easy to break.
10. The method for preparing textile fiber with radiation protection function according to claim 1, is characterized in that: the textile fiber with the radiation protection function prepared by the preparation method mainly comprises the following raw material components in parts by weight: 40-50 parts of regenerated keratin, 1-5 parts of nano titanium dioxide photocatalyst gel and 10-12.5 parts of polyvinyl alcohol.
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