CN106012092A - Multifunctional protein fiber and preparation method thereof - Google Patents

Multifunctional protein fiber and preparation method thereof Download PDF

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Publication number
CN106012092A
CN106012092A CN201610641350.5A CN201610641350A CN106012092A CN 106012092 A CN106012092 A CN 106012092A CN 201610641350 A CN201610641350 A CN 201610641350A CN 106012092 A CN106012092 A CN 106012092A
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fiber
protein fiber
multifunctional protein
parts
spinning
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CN106012092B (en
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翁冰雄
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Guangdong Anzhiban Industry Co., Ltd.
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翁冰雄
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Priority to CN201711261763.1A priority patent/CN107955995B/en
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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/02Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from cellulose, cellulose derivatives, or proteins
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/10Other agents for modifying properties
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/10Other agents for modifying properties
    • D01F1/103Agents inhibiting growth of microorganisms
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/04Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
    • D01F8/10Conjugated, 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
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/18Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from other substances
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00Treating 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
    • D06M11/51Treating 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
    • D06M11/55Treating 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
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10Treating 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
    • D06M13/12Aldehydes; Ketones
    • D06M13/127Mono-aldehydes, e.g. formaldehyde; Monoketones
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/02Natural fibres, other than mineral fibres
    • D06M2101/04Vegetal fibres

Abstract

The invention discloses a multifunctional protein fiber and a preparation technology thereof. The preparation technology comprises adding natural additives with functions of antibiosis, mildew resistance, mosquito and insect prevention and cooling into main fiber raw materials such as soybean protein, polyvinyl alcohol (PVA) and carboxymethyl chitosan to obtain a spinning stock solution with a plurality of functions, preparing a fiber semi-finished product from the spinning stock solution through a wet spinning technology and carrying out finishing so that mechanical properties of the protein fiber are improved and the multifunctional protein fiber with excellent mechanical properties is obtained. The multifunctional protein fiber and the preparation technology solve the problem that the common protein fiber on the market has a single function, is produced by complex processes, has no lasting effects and has a high production cost. The multifunctional protein fiber has effects of softness, skin adaptability, moisture absorption, humidity elimination, antibiosis, mildew resistance, mosquito repellency, insect prevention and skin cooling and has a good market prospect.

Description

A kind of multifunctional protein fiber and preparation method thereof
Technical field
The present invention relates to technical field of textile industry, particularly relate to a kind of with soybean protein, polyvinyl alcohol for the most former Multifunctional protein fiber of material and preparation method thereof.
Background technology
Along with the increase of world population, the demand of fiber is gradually risen by people, it is contemplated that to the year two thousand fifty, fiber total Demand will reach 0.9-1 hundred million tons.Along with raising and the development of science and technology of people's living standard, clothing are knitted by people Thing is had higher requirement.At present natural fiber is ventilative etc. with its natural environmental-protective, comfortable feel harmless to skin, moisture absorption Advantage enjoys consumers.
The material protein of preparing of azelon takes from milk, Semen arachidis hypogaeae, corn and soybean etc. more.Containing abundant in Semen sojae atricolor Protein, and with low cost, therefore soybean protein becomes the primary raw material of azelon.It is soft that soybean fiber has feel The advantages such as gloss sliding, bright, moisture absorption, wet guilding are good.
Occur in that a lot of patent in terms of soybean fiber processing technology, such as, patent " a kind of compound egg at present White fiber and preparation method thereof " (application number: 201110073928.9) describes collagen protein, soybean protein and polyethylene Alcohol mixing, modification by copolymerization, the method preparing compound protein fiber, improve the mechanical property of simple proteins fiber.Patent " Semen sojae atricolor Azelon and preparation method thereof " (application number: 201110110949.3) describes employing chemical method soybean protein is entered Row modification, thus strengthen the acid-fast alkali-proof of soybean fiber.Patent " a kind of electrostatic spinning prepared containing azelon Method " (application number: 201310264109.1) describe employing method of electrostatic spinning azelon spinning technique is improved, make Protein-contg polymer solution carries out electrospinning in the atmosphere of cross-linking agent and water, it is to avoid the cross-linking reaction shadow to Electrospun profile Ring.
But, only rest on the aspect of performance how changing azelon now concerning the preparation of azelon, prepare Azelon function singleness, it is impossible to meet the demand of refrigerant to summer clothes, mosquito-proof, the anti-demodicid mite of people etc.;It addition, azelon The shortcomings such as fiber prepared by cross-linking polyvinyl alcohol in use exists easy bacteria-developing and causes the use time short, and hydrothermal is low.Logical Cross at the fiber prepared by the multifunctional fibre preparation method of fiber surface coating functions material easily along with washing times Increase functional decrease fast.Therefore, the soybean protein viscose rayon with anti-microbial property is possible not only to meet people to medicated clothing The research of anti-microbial property, the life-span for medicated clothing itself also has important function, and can be with soybean fiber and polyethylene The selection of the additive that alcohol copolymerization plays antibacterial action is most important, uses in the patent of Application No. 201310327891.7 Antimicrobial component be nanometer silver, in wearing process, silver ion can diffuse out and be unfavorable for human body skin and health care of body.
Summary of the invention
In order to overcome above-mentioned deficiency of the prior art, the invention provides a kind of multifunctional protein fiber and preparation side thereof Method, to overcome azelon function singleness, does not possess Vermins-proof and mosquito-driving function, does not possess disinfecting and sterilizing functions and PVA and albumen The problem of fiber copolymerization not hydrothermal.
In order to realize the purpose of the present invention, the technical solution used in the present invention is as follows:
A kind of multifunctional protein fiber, including the raw material of following weight portion:
Soybean protein 30 parts-35 parts, polyvinyl alcohol 50 parts-55 parts, functional additive 4 parts-5 parts, carboxymethyl chitosan 10 Part-15 parts, calcium gluconate 3 parts-6 parts;
Wherein, described functional additive includes the effective raw material of following mass parts:
Berberine 1.2-1.5 part, Aloe extract 1.0-1.2 part, natural anophelifuge 0.6-0.8 part, Mentholum 0.8 part, Bamboo charcoal micropowder 0.4 part-0.7 part.
The present invention also has a following additional technical feature:
Preferably, purity >=95% of soybean protein, the degree of polymerization of polyvinyl alcohol is 2000-3000, described polyvinyl alcohol Alcoholysis degree more than 99%.
Preferably, purity >=95% of soybean protein.
Preferably, described soybean protein is to extract from soybean meal, main with a diameter of 5-20um in Semen sojae atricolor Albumen spheroid exist.
The present invention also provides for the preparation method of above-mentioned multifunctional protein fiber, specifically includes following steps:
Prepared by A aftergrowth albumen spinning base fluid: soybean protein is dissolved in water, the quality of described water be 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 so that it is dissolve all Even, it is warming up to 80-100 DEG C, regulation pH value, to 8-9, adds polyvinyl alcohol, makes soybean protein, carboxymethyl chitosan in high-speed stirred Sugar and polyvinyl alcohol fully dissolve mix homogeneously, and the speed of described high-speed stirred is 250-300 revolutions per second;
Prepared by B functional additive: add berberine, bamboo charcoal micropowder, Aloe extract, natural anophelifuge, Herba Menthae in water Stir after brain, dispersant, functional additive, the quality of described water is the effective raw material of described functional additive 4-6 times;
Prepared by C spinning solution: functional additive step B obtained adds in the spinning base fluid in step A, and stirring is all Even;Regulation pH value is 5-7, and adds initiator, temperature be 50-60 DEG C reaction 6-10 hour after, add calcium gluconate, stir Mixing uniformly, through filtration, standing and defoaming, make spinning solution, wherein initiator is Ammonium persulfate., benzoyl peroxide or cerous nitrate Ammonium or its combination in any;
D spinning technique: spinning solution step C obtained uses wet spinning technology, sprays through spinneret, spinning head A diameter of 0.1mm~0.4mm, spinneret spouting velocity is 15-17m/min, then through drawing-off, dry, heat-setting process, prepares half Finished fiber;
E postfinishing process: Semifinished fibre step D obtained carries out hydroformylation process, processes 20-40 minute time, control Hydroformylation temperature processed is 70-80 DEG C, hydroformylation time pH value be 4~6, obtain multifunctional protein fiber through washing, be dried, oiling.
Preferably, described dispersant model is SP-724, HT-5168 and carbon black dispersant mixes according to 2:2:1, institute With dispersant manufacturer predominantly: Bo Cheng Chemical Co., Ltd. of Guangdong city, Guangdong Heng Yu Chemical Co., Ltd..
Preferably, the addition of described dispersant is the 0.5%-1% of water quality.
Preferably, described initiator is the 0.15%~4% of soybean protein quality mark..
Preferably, the quality of described water is soybean protein and the 5.4%-22% of polyvinyl alcohol gross mass.
Preferably, the mass ratio of soybean protein described in step A and polyvinyl alcohol is 1:2.
Preferably, regulation acid used by pH value described in step A and step C is hydrochloric acid, sulphuric acid, acetic acid, polyacrylic acid, anti-bad One or more in hematic acid;Regulation alkali used by pH value is in sodium hydroxide, potassium hydroxide and disodiumedetate One or more.
Preferably, natural anophelifuge described in step B is that Cypress ethereal oil and Herba Lysimachiae foenum-graeci quintessence oil are according to the mixing of 1:1 mass ratio Becoming, Cypress ethereal oil and Herba Lysimachiae foenum-graeci quintessence oil are commercial.
Preferably, Aloe extract described in step B is with fresh Somalia Aloe as raw material, after cleaning, pulverizing, adds For the alcohol reflux that mass fraction is 50-70% 2-3 hour of fresh Somalia Aloe quality 4-6 times, concentrated spray is done Dry form.
Preferably, initiator amount described in step C is the 0.15%~4% of soybean protein quality.
Preferably, hydroformylation described in step E processes hydroformylation liquid used and is formed by formaldehyde, sulphuric acid, sodium sulfate and soft water are compounding, first Aldehyde is 26 ± 1g/L, and sulfuric acid content is 220 ± 4g/L, and sodium sulphate content is 72 ± 2g/L.
Preferably, described 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, Herba Menthae Brain and bamboo charcoal micropowder composition, Aloe extract has good disinfecting and sterilizing functions;Natural anophelifuge is Cypress ethereal oil and smokes clothing Grass quintessence oil mixes according to one to one mass ratio, and raw material is natural, is conducive to improving fibroid while solving anophelifuge problem Energy;Mentholum has refrigerant function, but also has sterilizing function;Bamboo-charcoal particles has elimination abnormal flavour, moisture absorption mildew-resistant, antibacterial drives Worm function;Raw material can be blended, and by additive granule size, the impact of group, the mechanical property of azelon can be by shadow Ringing, raw material is different, and its mixing with additive also can affect the mechanical property of azelon, the method for the present invention testing big On the basis of amount material, obtain this material combination.
Compared with prior art, the invention has the beneficial effects as follows:
The multifunctional protein fiber of the present invention has the multiple merits such as moisture absorption is ventilative, antibacterial and mouldproof, mosquito-proof insect protected, refrigerant skin smoothing Can, the problem solving current soybean fiber function singleness, the functional additive employed in the present invention is natural adding Add agent, abundance, with low cost, harmless, and there is health care;
The multifunctional protein fiber of the present invention passes through crosslinked carboxymethyl chitosan and calcium gluconate, adds molecular structure steady Qualitative, solve the shortcoming that fiber hydrothermal prepared by azelon cross-linking polyvinyl alcohol present in prior art is low, energy Hydrothermal from the prior art 100 DEG C are brought up to 147 DEG C;
Multifunctional protein fiber function prepared by the present invention is lasting, and the fabric made will not be along 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.
Detailed description of the invention
Below in conjunction with instantiation, the invention will be further described, but embodiments of the present invention do not limit 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, Mentholum 80g, bamboo Charcoal micropowder 70g), water volume.
Prepare multifunctional protein fiber:
Prepared by aftergrowth albumen spinning base fluid: soybean protein is dissolved in 48kg water, uses temperature-controllable heater, rises Temperature to 60-80 DEG C, be stirred continuously middle addition carboxymethyl chitosan so that it is be uniformly dissolved, be warming up to 80 DEG C, by add hydrochloric acid and Sodium hydroxide regulation pH value, to 8, adds polyvinyl alcohol, makes soybean protein, carboxymethyl chitosan and polyvinyl alcohol in high-speed stirred Fully dissolving mix homogeneously, the speed of described high-speed stirred is 250 revolutions per seconds;
(2) prepared by functional additive: add berberine, Aloe extract, natural anophelifuge, Mentholum, bamboo in 2kg water Charcoal micropowder, dispersant SP-724200g, stir and can obtain functional additive solution, the most natural anophelifuge be Cypress ethereal oil and Herba Lysimachiae foenum-graeci quintessence oil mixes according to one to one mass ratio, and Aloe extract is with fresh Somalia Aloe as raw material, through washing Only, being dried the moisture removing Aloe surface, after pulverizing, the mass fraction being incorporated as fresh Somalia Aloe quality 5 times is 50- The alcohol reflux of 70% 2.5 hours, reclaims ethanol, and concentrated spray is dried and forms;
(3) prepared by spinning solution: functional additive step (2) obtained adds in the spinning base fluid in step (1), stirs Mix uniformly;Regulation pH value be 5, and add protein quality 3% Ammonium persulfate., make soybean protein, carboxymethyl chitosan and Polyvinyl alcohol produce polyreaction, temperature be 60 DEG C reaction 10 hours after, add calcium gluconate, stir, through filter, quiet Put vacuum defoamation, make spinning solution;
(4) spinning technique: spinning solution step (3) obtained uses wet spinning technology, sprays through spinneret, is adopted With a diameter of 0.3mm of spinning head, spinneret spouting velocity be 16m/min again through drawing-off, be dried, heat-setting process, prepare half Finished fiber;
(5) postfinishing process: formaldehyde, sulphuric acid, sodium sulfate and soft water are re-dubbed hydroformylation liquid, make content of formaldehyde be 26 ± 1g/L, sulfuric acid content is 220 ± 4g/L, and sodium sulphate content is 72 ± 2g/L, and the Semifinished fibre that step (4) obtains is carried out aldehyde Change processes, and processes 30 minutes time, and controlling hydroformylation temperature is 80 DEG C, obtains multifunctional protein through steps such as washing, be dried, oil Fiber.
The present embodiment has carried out the mechanical property of anti-microbial property, repelling effect and fiber and has surveyed this multifunctional protein fiber Examination.
The test of the anti-microbial property of azelon uses Japanese Industrial Standards JIS L1902:2008 to carry out.
The method that the repelling effect test of azelon is taked is as follows:
(1) mosquito collected is imported to A room and the B room of mosquito-proof measure of merit case, makes the number base of mosquito in two Room This holding is consistent;Take equivalent 100% the salt water yield in culture dish as bait, be respectively placed in A room and the lower floor of B room;
(2) mosquito is under the attraction of salt, after a while, when on the gauze that mosquito falls within A room and B room or arbitrarily disperseing When two is indoor, the fiber without mosquito-proof effect being put in the upper strata of A room drawer, as comparison, mosquito-proof regenerated celulose fibre is put Enter the upper strata of B room drawer;Baffle plate about closing, observes the active situation of mosquito;
(3) after a few minutes, open the baffle plate between two Room, observe mosquito activity direction, treat that the land situation of mosquito is the most steady Regularly, the mosquito sum of two indoor is recorded.The different mosquito-proof regenerated celulose fibre of anophelifuge content is calculated according to equation below Anophelifuge rate, the mosquito-proof effect of this fiber is evaluated.
Its computing formula is: anophelifuge rate=(two mosquito sum-B room, Room mosquito populations)/two Room 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: embodiment 1 test result
Embodiment 2
Weigh raw material: soybean protein 3.5kg, polyvinyl alcohol (DP=3000) 5kg, carboxymethyl chitosan 1.5kg, glucose Acid calcium 0.4kg, functional additive 0.5kg (berberine 150g, Aloe extract 120g, natural anophelifuge 80g, Mentholum 80g, Bamboo charcoal micropowder 70g), water volume.
(1) prepared by aftergrowth albumen spinning base fluid: soybean protein is dissolved in 50kg water, uses temperature-controllable heating Device, is warming up to 60 DEG C, is stirred continuously middle addition carboxymethyl chitosan so that it is be uniformly dissolved, is warming up to 100 DEG C, by adding salt Acid and sodium hydroxide regulation pH value, to 8, add polyvinyl alcohol, make soybean protein, carboxymethyl chitosan and poly-second in high-speed stirred Enol fully dissolves mix homogeneously, and the speed of described high-speed stirred is 250 revolutions per seconds;
(2) prepared by functional additive: add berberine, Aloe extract, natural anophelifuge, Mentholum, bamboo charcoal in water Micropowder, dispersant HT-5168300g, stir and can obtain functional additive solution, the most natural anophelifuge be Cypress ethereal oil and Herba Lysimachiae foenum-graeci quintessence oil mixes according to one to one mass ratio, and Aloe extract is with fresh Somalia Aloe as raw material, through washing Only, being dried the moisture removing Aloe surface, after pulverizing, the mass fraction being incorporated as fresh Somalia Aloe quality 5 times is 50- The alcohol reflux of 70% 2.5 hours, reclaims ethanol, and concentrated spray is dried and forms;
(3) prepared by spinning solution: functional additive step (2) obtained adds in the spinning base fluid in step (1), stirs Mix uniformly;Regulation pH value be 6, and add protein quality 3% Ammonium persulfate., make soybean protein, carboxymethyl chitosan and Polyvinyl alcohol produce polyreaction, temperature be 55 DEG C reaction 8 hours after, add calcium gluconate, stir, through filter, quiet Put vacuum defoamation, make spinning solution;
(4) spinning technique: spinning solution step (3) obtained uses wet spinning technology, sprays through spinneret, is adopted With a diameter of 0.3mm of spinning head, spinneret spouting velocity be 16m/min again through drawing-off, be dried, heat-setting process, prepare half Finished fiber;
(5) postfinishing process: formaldehyde, sulphuric acid, sodium sulfate and soft water are re-dubbed hydroformylation liquid, making content of formaldehyde is 26g/L, Sulfuric acid content is 220g/L, and sodium sulphate content is 72g/L, and the Semifinished fibre that step (4) obtains is carried out hydroformylation process, processes 30 minutes time, controlling hydroformylation temperature is 80 DEG C, obtains multifunctional protein fiber through steps such as washing, be dried, oil.
The present embodiment and embodiment 1 use method of the same race that this multifunctional protein fiber is carried out anti-microbial property, repelling effect And the Mechanics Performance Testing of fiber, gained test result such as table 2 below.
Table 2: embodiment 2 test result
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, Mentholum 80g, bamboo Charcoal micropowder 40g), water volume.
Prepare multifunctional protein fiber:
(1) prepared by aftergrowth albumen spinning base fluid: soybean protein is dissolved in 60kg water, uses temperature-controllable heating Device, is warming up to 80 DEG C, is stirred continuously middle addition carboxymethyl chitosan so that it is be uniformly dissolved, is warming up to 90 DEG C, by adding hydrochloric acid With sodium hydroxide regulation pH value to 9, high-speed stirred adds polyvinyl alcohol, makes soybean protein, carboxymethyl chitosan and polyethylene Alcohol fully dissolves mix homogeneously, and the speed of described high-speed stirred is 300 revolutions per seconds;
(2) prepared by functional additive: add berberine, Aloe extract, natural anophelifuge, Mentholum, bamboo charcoal in water Micropowder, dispersant SP-724200g, stir and can obtain functional additive solution, and the most natural anophelifuge is Cypress ethereal oil and smokes Clothing grass quintessence oil mixes according to one to one mass ratio, and Aloe extract is with fresh Somalia Aloe as raw material, through cleaning, Being dried the moisture removing Aloe surface, after pulverizing, the mass fraction being incorporated as fresh Somalia Aloe quality 5 times is 50-70% Alcohol reflux 2.5 hours, reclaim ethanol, concentrated spray is dried and forms;
(3) prepared by spinning solution: functional additive step (2) obtained adds in the spinning base fluid in step (1), stirs Mix uniformly;Regulation pH value be 6, and add protein quality 3% benzoyl peroxide, make soybean protein, carboxymethyl chitosan Sugar and polyvinyl alcohol produce polyreaction, temperature be 55 DEG C reaction 8 hours after, add calcium gluconate, stir, pass through Filter, standing vacuum defoamation, make spinning solution;
(4) spinning technique: spinning solution step (3) obtained uses wet spinning technology, sprays through spinneret, is adopted With a diameter of 0.3mm of spinning head, spinneret spouting velocity be 16m/min again through drawing-off, be dried, heat-setting process, prepare half Finished fiber;
(5) postfinishing process: formaldehyde, sulphuric acid, sodium sulfate and soft water are re-dubbed hydroformylation liquid, make content of formaldehyde be 26 ± 1g/L, sulfuric acid content is 220 ± 4g/L, and sodium sulphate content is 72 ± 2g/L.The Semifinished fibre that step (4) obtains is carried out aldehyde Change processes, and processes 30 minutes time, and controlling hydroformylation temperature is 80 DEG C, obtains multifunctional protein through steps such as washing, be dried, oil Fiber.
The present embodiment and embodiment 1 use method of the same race that this multifunctional protein fiber is carried out anti-microbial property, repelling effect 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, is spun into pure fibers cloth and carries out antibiotic property detection, gained test knot Fruit is such as table 3 below.After the pure cloth being spun into is washed 30 times, then survey its antibiotic property, wherein, cloth is placed in roller washing machine Rotate 30 minutes and calculate washing once, anti-microbial property such as table 4 after washing 30 times.
Table 3: embodiment 3 test result
Table 4 embodiment 3 washes 30 anti-microbial properties afterwards
Wherein, the method for antibacterial detection according to the detection method in embodiment 1 is, antibacterial value is 2.7, and sterilizing value is 1.3。
Function Persistence study:
Experimental technique: the cloth after the fiber of embodiment 1, embodiment 2 and embodiment 3 gained is used that same technique is pure spinning Material, washes, and washing times is 30 times, and the method for washing is calculated once for fabric is placed in washing machine washing for 30 minutes.Point Not carrying out the Mechanics Performance Testing of anti-microbial property, repelling effect and fiber, detection method and embodiment 1 use method of the same race. The result such as table 5 obtained;
Table 5: comparative example 1,2,3 test result
Washing times has impact somewhat, impact effect to the intensity of azelon, wet breaking strength, dry elongation at break Not quite.The biocidal property of multifunctional protein fiber, bactericidal properties, repelling effect can subtract along with the increase of washing times Weak.
Comparative example 1
The present embodiment compared with Example 1, does not uses carboxymethyl chitosan and calcium gluconate, and other is the most identical.
Comparative example 2
The present embodiment compared with Example 1, does not uses carboxymethyl chitosan, and other is the most identical.
By embodiment 1-3, comparative example 1-2 gained fiber carries out hydrothermal detection, and embodiment 1 softening point in water 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 polysaccharide and calcium gluconate can improve the hydrothermal of azelon.
The above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art For Yuan, under the premise without departing from the principles of the invention, it is also possible to make some improvements and modifications, these improvements and modifications also should It is considered as protection scope of the present invention.

Claims (9)

1. a multifunctional protein fiber, it is characterised in that: include the raw material of following weight portion:
Soybean protein 30 parts-35 parts, polyvinyl alcohol 50 parts-55 parts, functional additive 4 parts-5 parts, carboxymethyl chitosan 10 parts- 15 parts, calcium gluconate 3 parts-6 parts;
Wherein, described functional additive includes the effective raw material of following mass parts:
Berberine 1.2-1.5 part, Aloe extract 1.0-1.2 part, natural anophelifuge 0.6-0.8 part, Mentholum 0.8 part, bamboo charcoal Micropowder 0.4 part-0.7 part.
Multifunctional protein fiber the most according to claim 1, it is characterised in that purity >=95% of soybean protein, polyethylene The degree of polymerization of alcohol is 2000-3000, and the alcoholysis degree of described 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:
Prepared by A aftergrowth albumen spinning base fluid: soybean protein is dissolved in water, and the quality of described 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 so that it is be uniformly dissolved, and rises Temperature is to 80-100 DEG C, and regulation pH value, to 8-9, adds polyvinyl alcohol in high-speed stirred, make soybean protein, carboxymethyl chitosan and gather Vinyl alcohol fully dissolves mix homogeneously, and the speed of described high-speed stirred is 250-300 revolutions per second;
Prepared by B functional additive: add berberine, bamboo charcoal micropowder, Aloe extract, natural anophelifuge, Mentholum in water, divide Stir after powder, functional additive, the quality of described water is the 4-6 of the effective raw material of described functional additive Times;
Prepared by C spinning solution: functional additive step B obtained adds in the spinning base fluid in step A, stirs;Adjust Joint pH value is 5-7, and adds initiator, after temperature is 50-60 DEG C of reaction 6-10 hour, adds calcium gluconate, and stirring is all Even, through filtration, standing and defoaming, make spinning solution, wherein initiator is Ammonium persulfate., benzoyl peroxide or ammonium ceric nitrate;
D spinning technique: spinning solution step C obtained uses wet spinning technology, sprays through spinneret, the diameter of spinning head For 0.1mm~0.4mm, spinneret spouting velocity is 15-17m/min, then through drawing-off, dry, heat-setting process, prepares semi-finished product Fiber;
E postfinishing process: Semifinished fibre step D obtained carries out hydroformylation process, processes 20-40 minute time, controls aldehyde Change temperature be 70-80 DEG C, hydroformylation time pH value be 4~6, obtain multifunctional protein fiber through washing, be dried, oiling.
The preparation method of multifunctional protein fiber the most according to claim 3, it is characterised in that Semen sojae atricolor egg described in step A White and polyvinyl alcohol mass ratio is 1:2.
The preparation method of multifunctional protein fiber the most according to claim 3, it is characterised in that described in step A and step C Regulation acid used by pH value is one or more in hydrochloric acid, sulphuric acid, acetic acid, polyacrylic acid, ascorbic acid;Used by regulation pH value Alkali be one or more in sodium hydroxide, potassium hydroxide and disodiumedetate.
The preparation method of multifunctional protein fiber the most according to claim 3, it is characterised in that natural anti-described in step B Mosquito agent is Cypress ethereal oil and Herba Lysimachiae foenum-graeci quintessence oil mixes according to 1:1 mass ratio.
The preparation method of multifunctional protein fiber the most according to claim 3, it is characterised in that described in step B, Aloe carries Taking thing is with fresh Somalia Aloe as raw material, after cleaning, pulverizing, is incorporated as the matter of fresh Somalia Aloe quality 4-6 times Amount mark is alcohol reflux 2-3 hour of 50-70%, and concentrated spray is dried and forms.
The preparation method of multifunctional protein fiber the most according to claim 3, it is characterised in that initiator described in step C Consumption is the 0.15%~4% of soybean protein quality.
The preparation method of multifunctional protein fiber the most according to claim 3, it is characterised in that at hydroformylation described in step E Reason hydroformylation liquid used is formed by formaldehyde, sulphuric acid, sodium sulfate and soft water are compounding, and content of formaldehyde is 26 ± 1g/L, and sulfuric acid content is 220 ± 4g/L, sodium sulphate content is 72 ± 2g/L.
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