CN106012092B - A kind of multifunctional protein fiber and preparation method thereof - Google Patents
A kind of multifunctional protein fiber and preparation method thereof Download PDFInfo
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- CN106012092B CN106012092B CN201610641350.5A CN201610641350A CN106012092B CN 106012092 B CN106012092 B CN 106012092B CN 201610641350 A CN201610641350 A CN 201610641350A CN 106012092 B CN106012092 B CN 106012092B
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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
-
- 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
-
- 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
- D01F1/103—Agents inhibiting growth of microorganisms
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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
-
- 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
- D01F8/18—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from other substances
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/51—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with sulfur, selenium, tellurium, polonium or compounds thereof
- D06M11/55—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with sulfur, selenium, tellurium, polonium or compounds thereof with sulfur trioxide; with sulfuric acid or thiosulfuric acid or their salts
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/12—Aldehydes; Ketones
- D06M13/127—Mono-aldehydes, e.g. formaldehyde; Monoketones
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/04—Vegetal fibres
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- Chemical & Material Sciences (AREA)
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- Health & Medical Sciences (AREA)
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Abstract
The invention discloses a kind of multifunctional protein fiber and its preparation technology, use soybean protein, polyvinyl alcohol (PVA), carboxymethyl chitosan for fiber main raw material(s), by add with antibacterial and mouldproof, mosquito-proof insect prevention, refrigerant function natural additive, prepare the spinning solution with multiple functions, spinning solution is made by Semifinished fibre using wet spinning technology, the mechanical property of azelon is improved by rear finishing duplex technique again, finally gives the multifunctional protein fiber of good mechanical performance.A kind of multifunctional protein fiber provided by the invention and its preparation technology, overcome the problems such as azelon function common in the market is single, and complex manufacturing, function be not lasting, production cost is higher.Prepared multifunctional protein fiber has soft pro-skin, moisture absorption hydrofuge, antibacterial and mouldproof, repelling mosquitoes and preventing insects, refrigerant skin toner and other effects, and prepared multifunctional protein fiber has good market prospects.
Description
Technical field
The present invention relates to technical field of textile industry, more particularly to one kind using soybean protein, polyvinyl alcohol to be main former
Multifunctional protein fiber of material and preparation method thereof.
Background technology
With the increase of world population, people gradually rise to the demand of fiber, it is contemplated that to the year two thousand fifty, fiber it is total
Demand will reach hundred million tons of 0.9-1.With the improvement of people ' s living standards and scientific and technical development, people knit to clothes
Thing proposes higher requirement.Natural fiber is ventilative etc. with its natural environmental-protective, comfortable feel harmless to skin, moisture absorption at present
Advantage enjoys consumers.
The preparing raw material protein of azelon is derived from milk, peanut, corn and soybean etc. more.Contain what is enriched in soybean
Protein, and cost is cheap, therefore soybean protein turns into the primary raw material of azelon.Soybean fiber has feel soft
The advantages that sliding, bright gloss, moisture absorption, good wet guilding.
There are much patents in terms of soybean fiber manufacture craft at present, for example, patent《A kind of compound egg
White fiber and preparation method thereof》(application number：201110073928.9) in describe collagen, soybean protein and polyethylene
Alcohol mixes, modification by copolymerization, the method for preparing compound protein fiber, improves the mechanical property of simple proteins fiber.Patent《Soybean
Azelon and preparation method thereof》(application number：201110110949.3) in describe to enter soybean protein using chemical method
Row modification, so as to strengthen the acid-fast alkali-proof of soybean fiber.Patent《It is a kind of to prepare the electrostatic spinning containing azelon
Method》(application number：201310264109.1) describe azelon spinning technique is improved using method of electrostatic spinning, make
Protein-contg polymer solution carries out electrospinning in the atmosphere of crosslinking agent and water, avoids shadow of the cross-linking reaction to Electrospun profile
Ring.
However, the preparation now concerning azelon only rests on how to change the aspect of performance of azelon, prepare
Azelon function it is single, it is impossible to meet the needs of people are refrigerant to summer clothes, mosquito-proof, anti-mite etc.；In addition, azelon
There is easy bacteria-developing in use and cause usage time short in fiber prepared by cross-linking polyvinyl alcohol, the shortcomings such as hydrothermal is low.It is logical
The fiber prepared by the multifunctional fibre preparation method in fiber surface coating functions material is crossed easily with washing times
Increase feature decrease fast.Therefore, the soybean protein viscose rayon with anti-microbial property can not only meet people to clothing
The research of anti-microbial property, also play an important roll for the life-span of clothing in itself, and can be with soybean fiber and polyethylene
The selection for the additive that alcohol copolymerization plays antibacterial action is also most important, is used in the patent of Application No. 201310327891.7
Antimicrobial component be Nano Silver, silver ion, which can diffuse out, in wearing process is unfavorable for human body skin and health care of body.
The content of the invention
In order to overcome above-mentioned deficiency of the prior art, the invention provides a kind of multifunctional protein fiber and its preparation side
Method, to overcome azelon function single, do not possess Vermins-proof and mosquito-driving function, do not possess disinfecting and sterilizing functions and PVA and albumen
Fiber is copolymerized the problem of not hydrothermal.
In order to realize the purpose of the present invention, the technical solution adopted by the present invention is as follows：
A kind of multifunctional protein fiber, include the raw material of following parts by weight：
30 parts -35 parts of soybean protein, 50 parts -55 parts of polyvinyl alcohol, 4 parts -5 parts of functional additive, carboxymethyl chitosan 10
- 15 parts of part, 3 parts -6 parts of calcium gluconate；
Wherein, the functional additive includes the effective raw material of following mass parts：
Berberine 1.2-1.5 parts, aloe extract 1.0-1.2 parts, natural anophelifuge 0.6-0.8 parts, 0.8 part of menthol,
0.4 part -0.7 part of bamboo charcoal micropowder.
The present invention also has following additional technical feature：
Preferably, purity >=95% of soybean protein, the degree of polymerization of polyvinyl alcohol are 2000-3000, the polyvinyl alcohol
Alcoholysis degree be more than 99%.
Preferably, purity >=95% of soybean protein.
Preferably, the soybean protein is extracted from soybean meal, mainly with a diameter of 5-20um in soybean
Albumen orbicule exist.
The present invention also provides the preparation method of above-mentioned multifunctional protein fiber, specifically includes following steps：
It is prepared by A aftergrowth albumen spinning base fluid：Soybean protein is dissolved in water, the quality of the water for soybean protein and
6-7.5 times of polyvinyl alcohol gross mass, is warming up to 60-80 DEG C, is stirred continuously middle addition carboxymethyl chitosan, makes its dissolving equal
It is even, it is warming up to 80-100 DEG C, regulation pH value to 8-9, adds polyvinyl alcohol in high-speed stirred, make soybean protein, carboxymethyl chitosan
Sugar and polyvinyl alcohol fully dissolve well mixed, and the speed of the high-speed stirred is 250-300 revolutions per seconds；
It is prepared by B functional additives：Xiang Shuizhong adds berberine, bamboo charcoal micropowder, aloe extract, natural anophelifuge, peppermint
Stirred after brain, dispersant, you can obtain functional additive, the quality of the water is the effective raw material of the functional additive
4-6 times；
It is prepared by C spinning solutions：The functional additive that step B is obtained is added in the spinning base fluid in step A, and stirring is equal
It is even；Regulation pH value is 5-7, and adds initiator, after temperature is 50-60 DEG C of reaction 6-10 hour, adds calcium gluconate, stirs
Mix uniformly, filtered, standing and defoaming, spinning solution is made, wherein initiator is ammonium persulfate, benzoyl peroxide or cerous nitrate
Ammonium or its any combination；
D spinning techniques：The spinning solution that step C is obtained uses wet spinning technology, is sprayed through spinneret, spinning head
A diameter of 0.1mm~0.4mm, spinneret spouting velocity are 15-17m/min, then through drawing-off, drying, heat-setting process, are made half
Finished fiber；
E postfinishing process：The Semifinished fibre that step D is obtained carries out hydroformylation processing, minute processing time 20-40, control
Hydroformylation temperature processed is 70-80 DEG C, hydroformylation when pH value be 4~6, through washing, drying, oiling to obtain multifunctional protein fiber.
Preferably, described dispersant model SP-724, HT-5168 and carbon black dispersant are according to 2:2:1 mixes, institute
With dispersant, manufacturer is mainly：Bo Cheng Chemical Co., Ltd.s of Guangdong city, Guangdong Heng Yu Chemical Co., Ltd.s.
Preferably, the addition of the dispersant is the 0.5%-1% of water quality.
Preferably, the initiator is the 0.15%~4% of soybean protein quality fraction..
Preferably, the quality of the water is soybean protein and the 5.4%-22% of polyvinyl alcohol gross mass.
Preferably, the mass ratio of soybean protein and polyvinyl alcohol described in step A is 1：2.
Preferably, the acid adjusted described in step A and step C used in pH value is hydrochloric acid, sulfuric acid, one kind in acetic acid or more
Kind；It is the one or more in sodium hydroxide, potassium hydroxide and disodium ethylene diamine tetraacetate to adjust the alkali used in pH value.
Preferably, natural anophelifuge described in step B is Cypress ethereal oil and Lavender according to 1:1 mass ratio mix and
Into Cypress ethereal oil and Lavender are purchased in market.
Preferably, aloe extract described in step B is using fresh Somalia aloe as raw material, after cleaning, crushing, is added
The alcohol reflux extraction 2-3 hours that mass fraction for fresh 4-6 times of Somalia aloe quality is 50-70%, concentrated spray are done
It is dry to form.
Preferably, initiator amount described in step C is the 0.15%~4% of soybean protein quality.
Preferably, hydroformylation liquid is formed by formaldehyde, sulfuric acid, sodium sulphate and soft water compounding used in hydroformylation processing described in step E, first
Aldehyde is 26 ± 1g/L, and sulfuric acid content is 220 ± 4g/L, and sodium sulphate content is 72 ± 2g/L.
Preferably, the heater is temperature-controllable heater.
The technical solution adopted in the present invention is：The present invention uses soybean protein, polyvinyl alcohol (PVA) and carboxymethyl chitosan
Sugar is the main raw material(s) of fiber, and three forms crosslinking；Natural additive is mainly by aloe extract, natural anophelifuge, peppermint
Brain and bamboo charcoal micropowder composition, aloe extract have good disinfecting and sterilizing functions；Natural anophelifuge is Cypress ethereal oil and smokes clothing
Careless essential oil mixes according to one to one mass ratio, and raw material is natural, is advantageous to improve fibroid while solving the problems, such as mosquito repellent
Energy；Menthol has refrigerant function, but also has sterilizing function；Bamboo-charcoal particles, which have, eliminates that peculiar smell, moisture absorption be mould proof, antibacterial drive
Worm function；Raw material can be blended, and by additive granule size, the influence of group, the mechanical property of azelon can be by shadow
Ring, raw material is different, and the mixing of itself and additive can also influence the mechanical property of azelon, and method of the invention is testing greatly
On the basis of measuring material, this material combination is obtained.
Compared with prior art, the beneficial effects of the invention are as follows：
The multifunctional protein fiber of the present invention has a variety of work(such as ventilative moisture absorption, antibacterial and mouldproof, mosquito-proof insect prevention, refrigerant skin toner
Can, solve the problems, such as that current soybean fiber function is single, the functional additive employed in the present invention is naturally to add
Add agent, abundance, cost are cheap, harmless, and have healthcare function；
It is steady to add molecular structure by crosslinked carboxymethyl chitosan and calcium gluconate for the multifunctional protein fiber of the present invention
It is qualitative, solve the shortcomings that fiber hydrothermal prepared by azelon cross-linking polyvinyl alcohol present in prior art is low, energy
100 DEG C of hydrothermal from the prior art are brought up to 147 DEG C；
Multifunctional protein fiber function prepared by the present invention is lasting, and manufactured fabric will not be with the increase of washing times
Function decrease fast；
The fracture strength of multifunctional protein fiber provided by the present invention is apparently higher than prior art, preparation technology, technique
Relatively simple, production cost is relatively low, is worthy to be popularized.
Embodiment
With reference to instantiation, the invention will be further described, but embodiments of the present invention are unlimited so.
Embodiment 1
Weigh raw material：Soybean protein 3kg, polyvinyl alcohol (DP=2000) 5kg, carboxymethyl chitosan 1kg, calcium gluconate
0.5kg,
Functional additive 0.45kg (berberine 120g, aloe extract 100g, natural anophelifuge 80g, menthol 80g, bamboo
Charcoal micro mist 70g), water volume.
Prepare multifunctional protein fiber：
It is prepared by aftergrowth albumen spinning base fluid：Soybean protein is dissolved in 48kg water, using temperature-controllable heater, risen
Temperature to 60-80 DEG C, be stirred continuously middle addition carboxymethyl chitosan, be uniformly dissolved it, be warming up to 80 DEG C, by add hydrochloric acid and
Sodium hydroxide adjusts pH value to 8, adds polyvinyl alcohol in high-speed stirred, makes soybean protein, carboxymethyl chitosan and polyvinyl alcohol
Fully dissolving is well mixed, and the speed of the high-speed stirred is 250 revolutions per seconds；
(2) prepared by functional additive：Berberine, aloe extract, natural anophelifuge, menthol, bamboo are added into 2kg water
Charcoal micro mist, dispersant SP-724 200g, functional additive solution can be obtained by stirring, wherein natural anophelifuge is Cypress ethereal oil
Mixed with Lavender according to one to one mass ratio, aloe extract is the warp using fresh Somalia aloe as raw material
Clean, dry the moisture for removing aloe surface, after crushing, the mass fraction for being incorporated as fresh 5 times of Somalia aloe quality is 50-
70% alcohol reflux is extracted 2.5 hours, reclaims ethanol, and concentrated spray is dried and formed；
(3) prepared by spinning solution：The functional additive that step (2) is obtained is added in the spinning base fluid in step (1), is stirred
Mix uniformly；It is 5 to adjust pH value, and adds 3% ammonium persulfate of protein quality, make soybean protein, carboxymethyl chitosan and
Polyvinyl alcohol produces polymerisation, after temperature is reacted 10 hours for 60 DEG C, adds calcium gluconate, stirs, filtered, quiet
Vacuum defoamation is put, spinning solution is made；
(4) spinning technique：The spinning solution that step (3) is obtained uses wet spinning technology, sprays, is adopted through spinneret
With a diameter of 0.3mm of spinning head, spinneret spouting velocity be 16m/min again through drawing-off, drying, heat-setting process, be made half
Finished fiber；
(5) postfinishing process：Formaldehyde, sulfuric acid, sodium sulphate and soft water are re-dubbed hydroformylation liquid, make content of formaldehyde for 26 ±
1g/L, sulfuric acid content are 220 ± 4g/L, and sodium sulphate content is 72 ± 2g/L, and the Semifinished fibre that step (4) is obtained carries out aldehyde
Change is handled, and 30 minutes processing times, control hydroformylation temperature as 80 DEG C, and through washing, drying, the step such as oil obtains multifunctional protein
Fiber.
The mechanical property that the present embodiment has carried out anti-microbial property, repelling effect and fiber to the multifunctional protein fiber is surveyed
Examination.
The test of the anti-microbial property of azelon uses Japanese Industrial Standards JIS L1902:2008 are carried out.
It is as follows that the repelling effect of azelon tests taken method：
(1) mosquito being collected into is imported into the A rooms and B rooms of mosquito-proof measure of merit case, makes the number base of mosquito in two Room
Originally it is consistent；The salt water of the 100% of equivalent is taken to be respectively placed in the lower floor of A rooms and B rooms in being used as bait in culture dish；
(2) mosquito is under the attraction of salt, after a while, when mosquito falls within the gauze of A rooms and B rooms or arbitrarily scattered
When two is indoor, the fiber without mosquito-proof effect is put in the upper strata of A rooms drawer, as control, mosquito-proof regenerated celulose fibre is put
Enter the upper strata of B rooms drawer；The baffle plate of left and right is closed, observes the active situation of mosquito；
(3) after a few minutes, the baffle plate between two Room is opened, mosquito activity direction is observed, treats that the land situation of mosquito is substantially steady
Regularly, the indoor mosquito sum of record two.The different mosquito-proof regenerated celulose fibres of mosquito repellent agent content are calculated according to equation below
Mosquito repellent rate, the mosquito-proof effect of the fiber is evaluated.
Its calculation formula is：Mosquito repellent rate=the Room of (two Room mosquito sum-B rooms mosquito populations)/two mosquito sum
The Mechanics Performance Testing of fiber is carried out on fibrous material Mechanics Performance Testing experimental provision.
Measured test result is as shown in table 1.
Table 1：The test result of embodiment 1
Embodiment 2
Weigh raw material：Soybean protein 3.5kg, polyvinyl alcohol (DP=3000) 5kg, carboxymethyl chitosan 1.5kg, glucose
Sour calcium 0.4kg, functional additive 0.5kg (berberine 150g, aloe extract 120g, natural anophelifuge 80g, menthol 80g,
Bamboo charcoal micropowder 70g), water volume.
(1) prepared by aftergrowth albumen spinning base fluid：Soybean protein is dissolved in 50kg water, heated using temperature-controllable
Device, 60 DEG C are warming up to, are stirred continuously middle addition carboxymethyl chitosan, are uniformly dissolved it, 100 DEG C are warming up to, by adding salt
Acid and sodium hydroxide adjust pH value to 8, add polyvinyl alcohol in high-speed stirred, make soybean protein, carboxymethyl chitosan and poly- second
Enol fully dissolves well mixed, and the speed of the high-speed stirred is 250 revolutions per seconds；
(2) prepared by functional additive：Xiang Shuizhong adds berberine, aloe extract, natural anophelifuge, menthol, bamboo charcoal
Micro mist, dispersant HT-5168 300g, functional additive solution can be obtained by stirring, wherein natural anophelifuge be Cypress ethereal oil and
Lavender mixes according to one to one mass ratio, and aloe extract is using fresh Somalia aloe as raw material, through washing
Only the moisture for removing aloe surface, is dried, after crushing, the mass fraction for being incorporated as fresh 5 times of Somalia aloe quality is 50-
70% alcohol reflux is extracted 2.5 hours, reclaims ethanol, and concentrated spray is dried and formed；
(3) prepared by spinning solution：The functional additive that step (2) is obtained is added in the spinning base fluid in step (1), is stirred
Mix uniformly；It is 6 to adjust pH value, and adds 3% ammonium persulfate of protein quality, make soybean protein, carboxymethyl chitosan and
Polyvinyl alcohol produces polymerisation, after temperature is reacted 8 hours for 55 DEG C, adds calcium gluconate, stirs, filtered, quiet
Vacuum defoamation is put, spinning solution is made；
(4) spinning technique：The spinning solution that step (3) is obtained uses wet spinning technology, sprays, is adopted through spinneret
With a diameter of 0.3mm of spinning head, spinneret spouting velocity be 16m/min again through drawing-off, drying, heat-setting process, be made half
Finished fiber；
(5) postfinishing process：Formaldehyde, sulfuric acid, sodium sulphate and soft water are re-dubbed hydroformylation liquid, it is 26g/L to make content of formaldehyde,
Sulfuric acid content is 220g/L, sodium sulphate content 72g/L, and the Semifinished fibre that step (4) is obtained carries out hydroformylation processing, processing
30 minutes time, it is 80 DEG C to control hydroformylation temperature, and through washing, drying, the step such as oil obtains multifunctional protein fiber.
The present embodiment carries out anti-microbial property, repelling effect using method of the same race with embodiment 1 to the multifunctional protein fiber
And the Mechanics Performance Testing of fiber, gained test result such as table 2 below.
Table 2：The test result of embodiment 2
Embodiment 3
Weigh raw material：Soybean protein 3.5kg, polyvinyl alcohol 5.2kg, carboxymethyl chitosan 1.2kg, calcium gluconate
0.6kg,
Functional additive 0.4kg (berberine 120g, aloe extract 100g, natural anophelifuge 60g, menthol 80g, bamboo
Charcoal micro mist 40g), water volume.
Prepare multifunctional protein fiber：
(1) prepared by aftergrowth albumen spinning base fluid：Soybean protein is dissolved in 60kg water, heated using temperature-controllable
Device, 80 DEG C are warming up to, are stirred continuously middle addition carboxymethyl chitosan, are uniformly dissolved it, 90 DEG C are warming up to, by adding hydrochloric acid
PH value is adjusted to 9 with sodium hydroxide, is added polyvinyl alcohol in high-speed stirred, is made soybean protein, carboxymethyl chitosan and polyethylene
Alcohol fully dissolves well mixed, and the speed of the high-speed stirred is 300 revolutions per seconds；
(2) prepared by functional additive：Xiang Shuizhong adds berberine, aloe extract, natural anophelifuge, menthol, bamboo charcoal
Micro mist, dispersant SP-724 200g, functional additive solution can be obtained by stirring, wherein natural anophelifuge be Cypress ethereal oil and
Lavender mixes according to one to one mass ratio, and aloe extract is using fresh Somalia aloe as raw material, through washing
Only the moisture for removing aloe surface, is dried, after crushing, the mass fraction for being incorporated as fresh 5 times of Somalia aloe quality is 50-
70% alcohol reflux is extracted 2.5 hours, reclaims ethanol, and concentrated spray is dried and formed；
(3) prepared by spinning solution：The functional additive that step (2) is obtained is added in the spinning base fluid in step (1), is stirred
Mix uniformly；It is 6 to adjust pH value, and adds 3% benzoyl peroxide of protein quality, makes soybean protein, carboxymethyl chitosan
Sugar and polyvinyl alcohol produce polymerisation, after temperature is reacted 8 hours for 55 DEG C, add calcium gluconate, stir, pass through
Filter, vacuum defoamation is stood, spinning solution is made；
(4) spinning technique：The spinning solution that step (3) is obtained uses wet spinning technology, sprays, is adopted through spinneret
With a diameter of 0.3mm of spinning head, spinneret spouting velocity be 16m/min again through drawing-off, drying, heat-setting process, be made half
Finished fiber；
(5) postfinishing process：Formaldehyde, sulfuric acid, sodium sulphate and soft water are re-dubbed hydroformylation liquid, make content of formaldehyde for 26 ±
1g/L, sulfuric acid content are 220 ± 4g/L, and sodium sulphate content is 72 ± 2g/L.The Semifinished fibre that step (4) is obtained carries out aldehyde
Change is handled, and 30 minutes processing times, control hydroformylation temperature as 80 DEG C, and through washing, drying, the step such as oil obtains multifunctional protein
Fiber.
The present embodiment carries out anti-microbial property, repelling effect using method of the same race with embodiment 1 to the multifunctional protein fiber
And the Mechanics Performance Testing of fiber, gained test result such as table 3 below.The detection method of antibiotic property is with reference to national standard AATCC-
The method of 100 antibacterial textile performance detections, during detection, pure fibers are spun into cloth and carry out antibiotic property detection, gained test knot
Fruit such as table 3 below.The pure cloth being spun into is washed 30 times and then surveys its antibiotic property, wherein, cloth is placed in roller washing machine
Rotation calculates washing once in 30 minutes, anti-microbial property such as table 4 after washing 30 times.
Table 3：The test result of embodiment 3
Anti-microbial property after the embodiment 3 of table 4 is washed 30 times
Wherein, the method for antibacterial detection property is that antibacterial value is 2.7, and sterilizing value is according to the detection method in embodiment 1
1.3。
Function Persistence study：
Experimental method：The fiber of embodiment 1, embodiment 2 and the gained of embodiment 3 is used to the cloth after the same pure spinning of technique
Material, is washed, and washing times are 30 times, and the method for washing is calculated once for fabric is placed in washing machine to wash 30 minutes.Point
Not carry out anti-microbial property, repelling effect and fiber Mechanics Performance Testing, detection method and embodiment 1 use method of the same race.
The result of acquisition such as table 5；
Table 5：The test result of comparative example 1,2,3
Washing times have influence somewhat, impact effect to the intensity of azelon, wet breaking strength, dry elongation at break
Less.Biocidal property, bactericidal properties, the repelling effect of multifunctional protein fiber can somewhat subtract with the increase of washing times
It is weak.
Comparative example 1
Compared with Example 1, carboxymethyl chitosan and calcium gluconate, other all sames are not used in the present embodiment.
Comparative example 2
Compared with Example 1, carboxymethyl chitosan, other all sames are not used in the present embodiment.
By embodiment 1-3, fiber obtained by comparative example 1-2 carries out hydrothermal detection, and the softening point in water of embodiment 1 is 146
DEG C, embodiment 2 is 142 DEG C, and embodiment 3 is 145 DEG C, and comparative example 1 is 107 DEG C, and comparative example 2 is 110 DEG C.Understand, carboxymethyl shell
The addition of glycan and calcium gluconate can improve the hydrothermal of azelon.
Described above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (9)
- A kind of 1. multifunctional protein fiber, it is characterised in that：Include the raw material of following parts by weight：30 parts -35 parts of soybean protein, 50 parts -55 parts of polyvinyl alcohol, 4 parts -5 parts of functional additive, 10 part -15 of carboxymethyl chitosan Part, 3 parts -6 parts of calcium gluconate；Wherein, the functional additive includes the effective raw material of following mass parts：Berberine 1.2-1.5 parts, aloe extract 1.0-1.2 parts, natural anophelifuge 0.6-0.8 parts, 0.8 part of menthol, bamboo charcoal 0.4 part -0.7 part of micro mist.
- 2. multifunctional protein fiber according to claim 1, it is characterised in that purity >=95% of soybean protein, poly- second The degree of polymerization of enol is 2000-3000, and the alcoholysis degree of the polyvinyl alcohol is more than 99%.
- 3. the preparation method of the multifunctional protein fiber described in claim 1 or 2, it is characterised in that specifically include following steps：It is prepared by A aftergrowth albumen spinning base fluid：Soybean protein is dissolved in water, the quality of the water is soybean protein and poly- second 6-7.5 times of enol gross mass, is warming up to 60-80 DEG C, is stirred continuously middle addition carboxymethyl chitosan, is uniformly dissolved it, rises Temperature is to 80-100 DEG C, regulation pH value to 8-9, and polyvinyl alcohol is added in high-speed stirred, makes soybean protein, carboxymethyl chitosan and gathers Vinyl alcohol fully dissolves well mixed, and the speed of the high-speed stirred is 250-300 revolutions per seconds；It is prepared by B functional additives：Xiang Shuizhong add berberine, bamboo charcoal micropowder, aloe extract, natural anophelifuge, menthol, point Stirred after powder, you can obtain functional additive, the quality of the water is the 4-6 of the effective raw material of the functional additive Times；It is prepared by C spinning solutions：The functional additive that step B is obtained is added in the spinning base fluid in step A, is stirred；Adjust Section pH value is 5-7, and adds initiator, after temperature is 50-60 DEG C of reaction 6-10 hour, adds calcium gluconate, stirring is equal It is even, filtered, standing and defoaming, spinning solution is made, wherein initiator is ammonium persulfate, benzoyl peroxide or ammonium ceric nitrate；D spinning techniques：The spinning solution that step C is obtained uses wet spinning technology, is sprayed through spinneret, the diameter of spinning head For 0.1mm~0.4mm, spinneret spouting velocity is 15-17m/min, then through drawing-off, drying, heat-setting process, semi-finished product are made Fiber；E postfinishing process：The Semifinished fibre that step D is obtained carries out hydroformylation processing, minute processing time 20-40, controls aldehyde Change temperature be 70-80 DEG C, hydroformylation when pH value be 4~6, through washing, drying, oiling to obtain multifunctional protein fiber.
- 4. the preparation method of multifunctional protein fiber according to claim 3, it is characterised in that soybean egg described in step A White and polyvinyl alcohol mass ratio is 1：2.
- 5. the preparation method of multifunctional protein fiber according to claim 3, it is characterised in that described in step A and step C The acid adjusted used in pH value is hydrochloric acid, the one or more in sulfuric acid, acetic acid；The alkali adjusted used in pH value is sodium hydroxide, hydrogen One or more in potassium oxide and disodium ethylene diamine tetraacetate.
- 6. the preparation method of multifunctional protein fiber according to claim 3, it is characterised in that naturally prevent described in step B Mosquito agent is Cypress ethereal oil and Lavender according to 1:1 mass ratio mixes.
- 7. the preparation method of multifunctional protein fiber according to claim 3, it is characterised in that aloe described in step B carries It is using fresh Somalia aloe as raw material to take thing, after cleaning, crushing, is incorporated as the matter of fresh 4-6 times of Somalia aloe quality Measure the alcohol reflux that fraction is 50-70% and extract 2-3 hours, concentrated spray is dried and formed.
- 8. the preparation method of multifunctional protein fiber according to claim 3, it is characterised in that initiator described in step C Dosage is the 0.15%~4% of soybean protein quality.
- 9. the preparation method of multifunctional protein fiber according to claim 3, it is characterised in that described in step E at hydroformylation Hydroformylation liquid used in reason is formed by formaldehyde, sulfuric acid, sodium sulphate and soft water compounding, and content of formaldehyde is 26 ± 1g/L, sulfuric acid content 220 ± 4g/L, sodium sulphate content are 72 ± 2g/L.
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| CN112779644B (en) * | 2020-12-24 | 2022-06-07 | 陕西元丰纺织技术研究有限公司 | Temperature-adjusting antibacterial mosquito-proof yarn and fabric and preparation method thereof |
| CN113150488B (en) * | 2021-04-20 | 2022-12-13 | 白坤玉 | Clothes hanger with mosquito repelling effect and preparation method thereof |
| CN114521629A (en) * | 2021-12-25 | 2022-05-24 | 北京天第食圣食品有限公司 | Raw wet noodles and preparation method thereof |
| CN116019965B (en) * | 2023-03-27 | 2023-05-30 | 江苏亨瑞生物医药科技有限公司 | Collagen film dressing and preparation method thereof |
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| CN1285376A (en) * | 2000-09-19 | 2001-02-28 | 武汉大学 | Process for preparation of water-proof and heat-resistant plastic soybean protein film |
| CN102534859A (en) * | 2011-12-23 | 2012-07-04 | 上海全宇生物科技遂平有限公司 | Manufacturing method of soybean protein and polyvinyl alcohol polymerized fiber |
| CN103388195A (en) * | 2013-07-31 | 2013-11-13 | 韩晓根 | Production method of antibacterial soybean protein fiber and product of antibacterial soybean protein fiber |
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| CN102174720B (en) * | 2011-03-25 | 2014-02-12 | 上海全宇生物科技遂平有限公司 | Compound protein fiber and preparation method thereof |
| CN102345186A (en) * | 2011-08-02 | 2012-02-08 | 苏州东胜化纤纺织有限公司 | Novel soybean protein synthetic fiber and preparation method |
| CN102797072B (en) * | 2012-07-27 | 2014-07-16 | 安徽绿朋实业有限公司 | Novel vinylon-based home textile fiber and preparation method thereof |
| CN103194818B (en) * | 2013-04-25 | 2014-12-17 | 南京信息工程大学 | Soybean protein and PVA (Polyvinyl Alcohol) blend fiber as well as preparation method and applications thereof |
| CN104372439B (en) * | 2014-11-10 | 2016-06-29 | 广东安之伴实业有限公司 | Bio-based protein composite fiber and preparation method thereof |
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| CN1285376A (en) * | 2000-09-19 | 2001-02-28 | 武汉大学 | Process for preparation of water-proof and heat-resistant plastic soybean protein film |
| CN102534859A (en) * | 2011-12-23 | 2012-07-04 | 上海全宇生物科技遂平有限公司 | Manufacturing method of soybean protein and polyvinyl alcohol polymerized fiber |
| CN103388195A (en) * | 2013-07-31 | 2013-11-13 | 韩晓根 | Production method of antibacterial soybean protein fiber and product of antibacterial soybean protein fiber |
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