CN115584638B - Aromatic microcapsule blended antibacterial cotton fiber and preparation method thereof - Google Patents
Aromatic microcapsule blended antibacterial cotton fiber and preparation method thereof Download PDFInfo
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- CN115584638B CN115584638B CN202211288980.0A CN202211288980A CN115584638B CN 115584638 B CN115584638 B CN 115584638B CN 202211288980 A CN202211288980 A CN 202211288980A CN 115584638 B CN115584638 B CN 115584638B
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- 239000003094 microcapsule Substances 0.000 title claims abstract description 71
- 125000003118 aryl group Chemical group 0.000 title claims abstract description 53
- 229920000742 Cotton Polymers 0.000 title claims abstract description 39
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 102000008186 Collagen Human genes 0.000 claims abstract description 96
- 108010035532 Collagen Proteins 0.000 claims abstract description 96
- 229920001436 collagen Polymers 0.000 claims abstract description 96
- 239000000835 fiber Substances 0.000 claims abstract description 91
- 239000000243 solution Substances 0.000 claims abstract description 49
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 46
- 239000000839 emulsion Substances 0.000 claims abstract description 36
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 35
- 238000001035 drying Methods 0.000 claims abstract description 31
- 238000002156 mixing Methods 0.000 claims abstract description 29
- 238000004132 cross linking Methods 0.000 claims abstract description 26
- 238000004061 bleaching Methods 0.000 claims abstract description 25
- 238000004043 dyeing Methods 0.000 claims abstract description 24
- 239000007788 liquid Substances 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 16
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000010041 electrostatic spinning Methods 0.000 claims abstract description 13
- 239000001301 oxygen Substances 0.000 claims abstract description 13
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 238000011065 in-situ storage Methods 0.000 claims abstract description 11
- 239000004721 Polyphenylene oxide Substances 0.000 claims abstract description 10
- 229920000570 polyether Polymers 0.000 claims abstract description 10
- 150000003242 quaternary ammonium salts Chemical class 0.000 claims abstract description 10
- SXRSQZLOMIGNAQ-UHFFFAOYSA-N Glutaraldehyde Chemical compound O=CCCCC=O SXRSQZLOMIGNAQ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000004140 cleaning Methods 0.000 claims abstract description 8
- 238000007598 dipping method Methods 0.000 claims abstract description 8
- 238000005470 impregnation Methods 0.000 claims abstract description 7
- 230000008569 process Effects 0.000 claims abstract description 7
- 239000007864 aqueous solution Substances 0.000 claims abstract description 5
- -1 polysiloxane Polymers 0.000 claims abstract description 5
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 5
- 239000007853 buffer solution Substances 0.000 claims abstract description 3
- DCAYPVUWAIABOU-UHFFFAOYSA-N hexadecane Chemical compound CCCCCCCCCCCCCCCC DCAYPVUWAIABOU-UHFFFAOYSA-N 0.000 claims description 22
- 238000003756 stirring Methods 0.000 claims description 22
- 239000000341 volatile oil Substances 0.000 claims description 20
- 239000000843 powder Substances 0.000 claims description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 239000003921 oil Substances 0.000 claims description 12
- 238000002791 soaking Methods 0.000 claims description 12
- 239000000725 suspension Substances 0.000 claims description 12
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 10
- 239000000178 monomer Substances 0.000 claims description 10
- 238000009987 spinning Methods 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 235000019441 ethanol Nutrition 0.000 claims description 9
- 239000003999 initiator Substances 0.000 claims description 8
- 230000000694 effects Effects 0.000 claims description 7
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical class [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 6
- 239000000872 buffer Substances 0.000 claims description 6
- 230000001804 emulsifying effect Effects 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 239000004094 surface-active agent Substances 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 4
- 239000002344 surface layer Substances 0.000 claims description 4
- 239000003431 cross linking reagent Substances 0.000 claims description 3
- 125000003277 amino group Chemical group 0.000 claims description 2
- 230000005540 biological transmission Effects 0.000 claims description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 2
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 abstract description 3
- 239000004753 textile Substances 0.000 abstract description 2
- 239000012071 phase Substances 0.000 description 17
- 244000178870 Lavandula angustifolia Species 0.000 description 5
- 235000010663 Lavandula angustifolia Nutrition 0.000 description 5
- 239000011162 core material Substances 0.000 description 5
- 239000001102 lavandula vera Substances 0.000 description 5
- 235000018219 lavender Nutrition 0.000 description 5
- BHTJEPVNHUUIPV-UHFFFAOYSA-N pentanedial;hydrate Chemical compound O.O=CCCCC=O BHTJEPVNHUUIPV-UHFFFAOYSA-N 0.000 description 5
- ZQTYRTSKQFQYPQ-UHFFFAOYSA-N trisiloxane Chemical class [SiH3]O[SiH2]O[SiH3] ZQTYRTSKQFQYPQ-UHFFFAOYSA-N 0.000 description 5
- 230000004075 alteration Effects 0.000 description 4
- 239000008346 aqueous phase Substances 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 239000003205 fragrance Substances 0.000 description 2
- 230000005764 inhibitory process Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 241000222122 Candida albicans Species 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 241000588724 Escherichia coli Species 0.000 description 1
- 235000010254 Jasminum officinale Nutrition 0.000 description 1
- 240000005385 Jasminum sambac Species 0.000 description 1
- 244000178231 Rosmarinus officinalis Species 0.000 description 1
- 241000191967 Staphylococcus aureus Species 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 229940095731 candida albicans Drugs 0.000 description 1
- 238000010382 chemical cross-linking Methods 0.000 description 1
- 230000003013 cytotoxicity Effects 0.000 description 1
- 231100000135 cytotoxicity Toxicity 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 102000034240 fibrous proteins Human genes 0.000 description 1
- 108091005899 fibrous proteins Proteins 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000010309 melting process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000002352 surface water Substances 0.000 description 1
- 230000037303 wrinkles Effects 0.000 description 1
Classifications
-
- 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
- D06M23/00—Treatment of fibres, threads, yarns, fabrics or fibrous goods made from such materials, characterised by the process
- D06M23/12—Processes in which the treating agent is incorporated in microcapsules
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0015—Electro-spinning characterised by the initial state of the material
- D01D5/003—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
-
- 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
- D01F4/00—Monocomponent artificial filaments or the like of proteins; Manufacture thereof
-
- D—TEXTILES; PAPER
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
- D02G3/00—Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
- D02G3/02—Yarns or threads characterised by the material or by the materials from which they are made
- D02G3/04—Blended or other yarns or threads containing components made from different materials
-
- D—TEXTILES; PAPER
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
- D02G3/00—Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
- D02G3/44—Yarns or threads characterised by the purpose for which they are designed
-
- D—TEXTILES; PAPER
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
- D02G3/00—Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
- D02G3/44—Yarns or threads characterised by the purpose for which they are designed
- D02G3/449—Yarns or threads with antibacterial properties
-
- 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
- D06M13/123—Polyaldehydes; Polyketones
-
- 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
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/53—Polyethers
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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
- D06M16/00—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
- D06P3/82—Textiles which contain different kinds of fibres
- D06P3/8204—Textiles which contain different kinds of fibres fibres of different chemical nature
- D06P3/829—Textiles which contain different kinds of fibres fibres of different chemical nature mixtures of cellulose and animalized fibres
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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
- 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
- D06M2101/06—Vegetal fibres cellulosic
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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
- 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
- D06M2101/10—Animal fibres
- D06M2101/14—Collagen fibres
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- Engineering & Computer Science (AREA)
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- Chemical & Material Sciences (AREA)
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- Mechanical Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- Microbiology (AREA)
- Animal Husbandry (AREA)
- Manufacturing & Machinery (AREA)
- Dispersion Chemistry (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Artificial Filaments (AREA)
- Chemical Treatment Of Fibers During Manufacturing Processes (AREA)
Abstract
The invention discloses an aromatic microcapsule blended antibacterial cotton fiber and a preparation method thereof, and relates to the technical field of textile, wherein the preparation method comprises the following steps: dissolving EDC and NHS in ethanol, dissolving collagen in PBS buffer solution, mixing the obtained EDC/NHS solution with the collagen solution, and carrying out electrostatic spinning to obtain collagen initial fibers; adding glutaraldehyde aqueous solution into the collagen primary fiber to carry out dipping reaction, cleaning and drying to obtain collagen fiber; preparing collagen fibers and cotton fibers into yarns through a blending process; oxygen bleaching dyeing, and adding the dyeing liquor into finishing liquor for padding finishing to obtain the finished product; wherein the finishing liquid consists of aromatic microcapsule emulsion and quaternary ammonium salt type polyether modified polysiloxane. The collagen fiber prepared by adopting the method combining in-situ crosslinking and impregnation crosslinking through the electrostatic spinning technology has the advantages of good thermal stability, good mechanical property, water resistance, comfort and skin friendliness.
Description
Technical Field
The invention relates to the technical field of textile, in particular to an aromatic microcapsule blended antibacterial cotton fiber and a preparation method thereof.
Background
Along with the improvement of living standard, the requirements of people on knitted products are not limited to the appearance and the quality, and the comfort, the environmental protection and the health care of the products are very important. The collagen has similar structure to human skin collagen, is a biological polymer substance, is white, opaque and unbranched fibrous protein, and has the effects of moistening skin, beautifying and eliminating wrinkles. Collagen solution is obtained by extracting collagen, and collagen fibers can be formed through spinning. The collagen fiber and the cotton fiber are blended to develop the mixed functional spinning thread, so that the knitwear can have the functions of comfort, skin friendliness, antibiosis and the like. However, collagen itself has many defects, such as poor mechanical properties and poor water solubility, which are difficult to meet the use requirements without modification treatment, and can be effectively improved by chemical crosslinking, but the mechanical properties, water resistance and other properties of the collagen in the prior art are still to be further improved.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides the aromatic microcapsule blended antibacterial cotton fiber and the preparation method thereof, and the collagen fiber prepared by adopting the method of combining in-situ crosslinking and impregnation crosslinking through the electrostatic spinning technology has the advantages of good thermal stability, good mechanical property, water resistance, comfort and skin friendliness.
The invention provides a preparation method of aromatic microcapsule blended antibacterial cotton fiber, which comprises the following steps:
s1, collagen fiber preparation: EDC and NHS are dissolved in ethanol to obtain EDC/NHS solution; dissolving collagen in PBS buffer solution to obtain collagen solution; mixing EDC/NHS solution and collagen solution, stirring, and carrying out electrostatic spinning to obtain collagen initial fiber; adding glutaraldehyde aqueous solution into the collagen primary fiber to carry out dipping reaction, cleaning and drying to obtain collagen fiber;
s2, blending: preparing collagen fibers and cotton fibers into yarns through a blending process;
s3, oxygen bleaching and dyeing: adding yarn into bleaching liquid for bleaching treatment, and then adding the yarn into dye for dyeing treatment;
s4, padding: padding and finishing the yarn after the oxygen bleaching and dyeing treatment, adding the yarn into finishing liquid, dipping, dehydrating and drying to obtain the aromatic microcapsule blended antibacterial cotton fiber; wherein the finishing liquid consists of aromatic microcapsule emulsion and quaternary ammonium salt type polyether modified polysiloxane.
Preferably, in S1, the molar ratio of EDC to NHS is between 2 and 4: the concentration of EDC/NHS in the 1, EDC/NHS solution is 4-7g/L; the pH of the PBS buffer=7.4, the concentration of collagen in the collagen solution is 10-14wt%; the volume percentage of EDC/NHS solution and collagen solution is 50-60:40-50.
Preferably, in S1, the voltage of electrostatic spinning is 15-18kV, the receiving distance is 15-20cm, and the solution advancing speed is 0.4-0.6mL/h.
Preferably, in S1, the concentration of glutaraldehyde aqueous solution is 0.3-0.6wt%, and the soaking reaction is carried out for 20-30min at normal temperature.
Preferably, in S2, the mass percentage of the collagen fibers and the cotton fibers in the yarn is 30-40:60-70.
Preferably, in S4, the aromatic microcapsule emulsion is obtained by dispersing an aromatic microcapsule powder in water, and the aromatic microcapsule powder is prepared as follows: dissolving surfactant SDS in deionized water to form a water phase; adding essential oil, methacrylic acid monomer and initiator into n-hexadecane, stirring and mixing to form an oil phase; mixing the water phase and the oil phase, and stirring and emulsifying to obtain emulsion; introducing nitrogen into the emulsion, heating in a water bath, and stirring for reaction to obtain microcapsule suspension; adding saturated calcium chloride emulsion into the microcapsule suspension to demulsify, filtering, washing with absolute ethyl alcohol, and drying at low temperature.
In the present invention, the essential oils include, but are not limited to, lavender essential oil, rosemary essential oil, jasmine essential oil; the conventional plant essential oil can be used.
Preferably, the mass ratio of the water phase to the oil phase is 3.8-4.2:1, a step of; the mass ratio of SDS to deionized water in the water phase is 0.8-1.2:100; in the oil phase, the mass ratio of the n-hexadecane, the essential oil, the methacrylic acid monomer and the initiator is 2-2.5:1:3-3.5:0.03-0.04.
Preferably, in the finishing liquid, the mass percentage ratio of the aromatic microcapsule emulsion to the quaternary ammonium salt polyether modified polysiloxane is 92-96:4-8; wherein the solid content of the aromatic microcapsule emulsion is 18-23%.
Preferably, the bath ratio of the pad finishing is 1:15-20, soaking at normal temperature for 8-12min, dehydrating, pre-drying at 60-65deg.C for 3-5min, and drying at 115-125deg.C.
The invention also provides the aromatic microcapsule blended antibacterial cotton fiber prepared by the method.
The beneficial effects are that: the invention prepares collagen fiber by adopting an electrostatic spinning technology and adopting a method combining in-situ crosslinking and impregnation crosslinking; firstly, EDC/NHS with good biocompatibility and slightly lower crosslinking strength is adopted as a crosslinking agent for in-situ crosslinking, and the in-situ crosslinking is carried out to promote the combination of carboxyl and amino in the molecular structure of collagen to form an amide bond, so that the regularity of collagen molecules is improved before the fiber is formed, the crosslinking effect of EDC/NHS is enhanced in the presence of ethanol, a three-dimensional crosslinking network structure is formed in the fiber, and the transmission of water molecules in the fiber is hindered; then, after the fiber is formed, glutaraldehyde with high crosslinking strength is adopted for impregnation crosslinking, so that the fiber can be well combined with amino groups in collagen molecules on the surface of the fiber, a crosslinked network is formed on the surface of the fiber through crosslinking, water molecules are prevented from entering the fiber from the surface layer of the fiber, and the water resistance of the fiber is improved. In addition, the inside of the fiber is crosslinked in situ to form a three-dimensional porous network structure, the surface layer structure is compact, the fiber has good dyeing performance, and the co-dyeing effect is better after the fiber is blended with cotton fiber for spinning. Compared with the method that the collagen fibers are directly subjected to the dipping crosslinking treatment, the method adopts different types of crosslinking agents to firstly perform in-situ crosslinking and then perform dipping crosslinking in the preparation process of the collagen fibers, so that the method has better mechanical property and water resistance, and the in-situ crosslinking increases the gaps among collagen molecules, so that the moisture regain is better, the consumption of glutaraldehyde with cytotoxicity is reduced in the preparation process, and the spinning blended cotton fibers with good thermal stability, good mechanical property, water resistance, comfort and skin friendliness are prepared.
The collagen/cotton fiber antibacterial finishing is carried out by padding and drying in aromatic microcapsule emulsion and quaternary ammonium salt polyether modified trisiloxane, and the obtained blend fiber has excellent antibacterial performance and has antibacterial rate of more than 80% on staphylococcus aureus, escherichia coli and candida albicans. In addition, the fragrance release rate of the prepared fragrance microcapsules is mainly divided into three stages: in the first stage, the core material in the microcapsule is solid below 10 ℃, and the n-hexadecane which is mutually soluble with the essential oil plays a role of a wall material to a certain extent, so that the release of the essential oil is effectively inhibited, and the release speed is low; the second stage, 10-24 ℃ is the heat absorption melting process of the core material, in this stage, the core material gradually changes from solid to liquid along with the temperature rise, the inhibition effect of the n-hexadecane on the release of the essential oil gradually weakens, and the release rate of the essential oil in the core material gradually accelerates along with the temperature rise; in the third stage, when the temperature reaches 24 ℃, the microcapsule core material is completely melted into liquid, the inhibition effect of the n-hexadecane on the release of the essential oil is basically disappeared, the release rate of the essential oil is obviously accelerated, and when the temperature is increased to 35 ℃, the release amount of the essential oil is increased slightly. The microcapsules are finished into a product.
Drawings
FIG. 1 is an SEM image of aromatic microcapsule powder prepared in example 4 of the invention.
Detailed Description
The technical scheme of the invention is described in detail through specific embodiments.
Example 1
An aromatic microcapsule blended antibacterial cotton fiber is prepared as follows:
s1, collagen fiber preparation: according to 2:1, taking EDC and NHS according to a molar ratio, dissolving the EDC and the NHS in ethanol, and preparing an EDC/NHS solution with the concentration of 4 g/L; collagen was dissolved in PBS buffer (ph=7.4) to give a collagen solution with a concentration of 10 wt%; EDC/NHS solution and collagen solution were mixed according to 50:50, mixing, stirring, carrying out electrostatic spinning, wherein the spinning voltage is 16kV, the receiving distance is 18cm, and the solution advancing speed is 0.5mL/h, so as to obtain the collagen primary fiber; adding 0.3wt% glutaraldehyde water solution into the collagen primary fiber, soaking for 20min, cleaning, and drying to obtain collagen fiber;
s2, blending: preparing collagen fibers and cotton fibers into yarns by a blending process, wherein the mass percentage of the collagen fibers and the cotton fibers in the yarns is 30:70;
s3, oxygen bleaching and dyeing: adding the yarn into bleaching liquid for bleaching treatment, and then adding the yarn into dye for dyeing treatment, wherein the dyed yarn has no chromatic aberration;
s4, padding: padding and finishing the yarn after the oxygen bleaching and dyeing treatment, and adding the yarn into finishing liquid, wherein the bath ratio is 1:15, soaking for 8min at normal temperature, dehydrating, pre-drying for 3min at 60 ℃, and then drying at 115 ℃ to obtain the aromatic microcapsule blended antibacterial cotton fiber; wherein the finishing liquid is prepared from 20% of aromatic microcapsule emulsion and quaternary ammonium salt type polyether modified trisiloxane according to 92:8 mass percent; the aromatic microcapsule emulsion is obtained by dispersing aromatic microcapsule powder into water, and the preparation of the aromatic microcapsule powder is as follows: dissolving 0.8 part of surfactant SDS in 100 parts of deionized water to form an aqueous phase; adding 1 part of lavender essential oil, 3 parts of methacrylic acid monomer and 0.03 part of initiator into 2.5 parts of n-hexadecane, and stirring and mixing to form an oil phase; the aqueous and oily phases were mixed according to 3.8:1, mixing, stirring and emulsifying to obtain emulsion; introducing nitrogen into the emulsion, heating to 60 ℃ in a water bath, and stirring for reaction for 5 hours to obtain microcapsule suspension; adding saturated calcium chloride emulsion into the microcapsule suspension to demulsify, filtering, washing with absolute ethyl alcohol, and drying at low temperature.
Example 2
An aromatic microcapsule blended antibacterial cotton fiber is prepared as follows:
s1, collagen fiber preparation: according to 3:1, taking EDC and NHS according to a molar ratio, dissolving the EDC and the NHS in ethanol, and preparing an EDC/NHS solution with the concentration of 5.5 g/L; collagen was dissolved in PBS buffer (ph=7.4) to give a collagen solution with a concentration of 12 wt%; EDC/NHS solution and collagen solution were mixed according to 60:40, mixing, stirring, carrying out electrostatic spinning, wherein the spinning voltage is 16kV, the receiving distance is 18cm, and the solution advancing speed is 0.5mL/h, so as to obtain the collagen primary fiber; adding 0.4wt% glutaraldehyde water solution into the collagen primary fiber, soaking for 20min, cleaning, and drying to obtain collagen fiber;
s2, blending: preparing collagen fibers and cotton fibers into yarns by a blending process, wherein the mass percentage of the collagen fibers and the cotton fibers in the yarns is 40:60;
s3, oxygen bleaching and dyeing: adding the yarn into bleaching liquid for bleaching treatment, and then adding the yarn into dye for dyeing treatment, wherein the dyed yarn has no chromatic aberration;
s4, padding: padding and finishing the yarn after the oxygen bleaching and dyeing treatment, and adding the yarn into finishing liquid, wherein the bath ratio is 1:17, soaking for 10min at normal temperature, dehydrating, pre-drying for 4min at 65 ℃, and drying at 120 ℃ to obtain the aromatic microcapsule blended antibacterial cotton fiber; wherein the finishing liquid is prepared from 20% of aromatic microcapsule emulsion and quaternary ammonium salt type polyether modified trisiloxane according to the following formula 94:6 mass percent; the aromatic microcapsule emulsion is obtained by dispersing aromatic microcapsule powder into water, and the preparation of the aromatic microcapsule powder is as follows: 1 part of surfactant SDS is dissolved in 100 parts of deionized water to form an aqueous phase; adding 1 part of lavender essential oil, 3.2 parts of methacrylic acid monomer and 0.03 part of initiator into 2.2 parts of n-hexadecane, and stirring and mixing to form an oil phase; the aqueous and oily phases were mixed according to 4:1, mixing, stirring and emulsifying to obtain emulsion; introducing nitrogen into the emulsion, heating to 65 ℃ in a water bath, and stirring for reacting for 5.5 hours to obtain microcapsule suspension; adding saturated calcium chloride emulsion into the microcapsule suspension to demulsify, filtering, washing with absolute ethyl alcohol, and drying at low temperature.
Example 3
An aromatic microcapsule blended antibacterial cotton fiber is prepared as follows:
s1, collagen fiber preparation: according to 4:1, taking EDC and NHS according to a molar ratio, dissolving the EDC and the NHS in ethanol, and preparing an EDC/NHS solution with the concentration of 7g/L; collagen was dissolved in PBS buffer (ph=7.4) to give a collagen solution with a concentration of 14wt%; EDC/NHS solution and collagen solution were mixed according to 60:40, mixing, stirring, carrying out electrostatic spinning, wherein the spinning voltage is 16kV, the receiving distance is 18cm, and the solution advancing speed is 0.5mL/h, so as to obtain the collagen primary fiber; adding 0.6wt% glutaraldehyde water solution into the collagen primary fiber, carrying out dipping reaction for 30min, cleaning, and drying to obtain collagen fiber;
s2, blending: preparing collagen fibers and cotton fibers into yarns by a blending process, wherein the mass percentage of the collagen fibers and the cotton fibers in the yarns is 40:60;
s3, oxygen bleaching and dyeing: adding the yarn into bleaching liquid for bleaching treatment, and then adding the yarn into dye for dyeing treatment, wherein the dyed yarn has no chromatic aberration;
s4, padding: padding and finishing the yarn after the oxygen bleaching and dyeing treatment, and adding the yarn into finishing liquid, wherein the bath ratio is 1:20, soaking for 12min at normal temperature, dehydrating, pre-drying for 5min at 65 ℃, and drying at 125 ℃ to obtain the aromatic microcapsule blended antibacterial cotton fiber; wherein the finishing liquid is prepared from 20% of aromatic microcapsule emulsion and quaternary ammonium salt type polyether modified trisiloxane according to the following steps: 4 mass percent; the aromatic microcapsule emulsion is obtained by dispersing aromatic microcapsule powder into water, and the preparation of the aromatic microcapsule powder is as follows: 1.2 parts of surfactant SDS is dissolved in 100 parts of deionized water to form an aqueous phase; 1 part of lavender essential oil, 3.5 parts of methacrylic acid monomer and 0.04 part of initiator are added into 2.5 parts of n-hexadecane, and stirred and mixed to form an oil phase; the aqueous and oily phases were combined according to 4.2:1, mixing, stirring and emulsifying to obtain emulsion; introducing nitrogen into the emulsion, heating to 70 ℃ in a water bath, and stirring for reaction for 6 hours to obtain microcapsule suspension; adding saturated calcium chloride emulsion into the microcapsule suspension to demulsify, filtering, washing with absolute ethyl alcohol, and drying at low temperature.
Example 4
An aromatic microcapsule blended antibacterial cotton fiber is prepared as follows:
s1, collagen fiber preparation: according to 2:1, taking EDC and NHS according to a molar ratio, dissolving the EDC and the NHS in ethanol, and preparing an EDC/NHS solution with the concentration of 6 g/L; collagen was dissolved in PBS buffer (ph=7.4) to give a collagen solution with a concentration of 13 wt%; EDC/NHS solution and collagen solution were mixed according to 55:45, stirring, carrying out electrostatic spinning, wherein the spinning voltage is 16kV, the receiving distance is 18cm, and the solution advancing speed is 0.5mL/h, so as to obtain the collagen primary fiber; adding 0.5wt% glutaraldehyde water solution into the collagen primary fiber, soaking and reacting for 25min, cleaning, and drying to obtain collagen fiber;
s2, blending: preparing collagen fibers and cotton fibers into yarns by a blending process, wherein the mass percentage of the collagen fibers and the cotton fibers in the yarns is 35: 65.
S3, oxygen bleaching and dyeing: adding the yarn into bleaching liquid for bleaching treatment, and then adding the yarn into dye for dyeing treatment, wherein the dyed yarn has no chromatic aberration;
s4, padding: padding and finishing the yarn after the oxygen bleaching and dyeing treatment, and adding the yarn into finishing liquid, wherein the bath ratio is 1:18, soaking for 10min at normal temperature, dehydrating, pre-drying for 5min at 65 ℃, and then drying at 120 ℃ to obtain the aromatic microcapsule blended antibacterial cotton fiber; wherein the finishing liquid is prepared from 20% of aromatic microcapsule emulsion and quaternary ammonium salt type polyether modified trisiloxane according to the following weight percentage of 95:5 mass percent; the aromatic microcapsule emulsion is obtained by dispersing aromatic microcapsule powder into water, and the preparation of the aromatic microcapsule powder is as follows: 1 part of surfactant SDS is dissolved in 100 parts of deionized water to form an aqueous phase; 1 part of lavender essential oil, 3.3 parts of methacrylic acid monomer and 0.035 part of initiator are added into 2.3 parts of n-hexadecane, and stirred and mixed to form an oil phase; the aqueous and oily phases were mixed according to 4:1, mixing, stirring and emulsifying to obtain emulsion; introducing nitrogen into the emulsion, heating to 65 ℃ in a water bath, and stirring for reaction for 6 hours to obtain microcapsule suspension; adding saturated calcium chloride emulsion into the microcapsule suspension to demulsify, filtering, washing with absolute ethyl alcohol, and drying at low temperature.
Fig. 1 is an SEM image of the aromatic microcapsule powder prepared in this example, and it can be seen from the figure that the microcapsules are spherical or ellipsoidal overall, and have a relatively regular morphology, smooth surface, and different sizes. Because the methacrylic acid monomer is slightly soluble in water, part of the methacrylic acid monomer reacts and polymerizes in the water phase, so that a 'connecting rod-shaped' bonding occurs between part of the microcapsules.
Comparative example 1
The difference compared to example 4 is only that the S1 step is different. Specific: dissolving collagen into ethanol solution to prepare collagen solution with the concentration of 5.8wt%, and carrying out electrostatic spinning, wherein the spinning voltage is 16kV, the receiving distance is 18cm, and the solution advancing speed is 0.5mL/h, so as to obtain collagen initial fibers; adding 0.7wt% glutaraldehyde water solution into the collagen primary fiber, soaking for 25min, cleaning, and drying to obtain collagen fiber
In the preparation process of the collagen fibers in examples 1 to 4 of the present invention, the collagen fibers obtained by in-situ crosslinking and impregnation crosslinking were dried, and the properties of the fibers at each stage and the properties of the collagen fibers prepared in comparative example 1 after impregnation crosslinking were examined, respectively.
1. Breaking strength: according to GB/T3916-1997, a fiber strength tester is adopted to detect the breaking strength;
2. water resistance: expressed as water absorption, immersing the fiber in deionized water for 10min, taking out, removing surface water, calculating the increased mass of the fiber, wherein the water absorption=the increased mass of the fiber/the initial mass of the fiber is 100%;
3. moisture regain: expressed as the moisture regain, the fibers were placed in an oven at 25 ℃ and 70 ℃ for 24 hours, taken out, dried at 100 ℃ and the mass of fiber reduction before and after drying calculated as moisture regain = mass of fiber reduction/mass of fiber after drying 100%.
The detection results are shown in Table 1.
TABLE 1 collagen fiber Performance data prepared in examples 1-4 and comparative example 1
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.
Claims (4)
1. The preparation method of the aromatic microcapsule blended antibacterial cotton fiber is characterized by comprising the following steps of:
s1, collagen fiber preparation: EDC and NHS are dissolved in ethanol to obtain EDC/NHS solution; dissolving collagen in PBS buffer solution to obtain collagen solution; mixing EDC/NHS solution and collagen solution, stirring, and carrying out electrostatic spinning to obtain collagen initial fiber; adding glutaraldehyde aqueous solution into the collagen primary fiber to carry out dipping reaction, cleaning and drying to obtain collagen fiber;
s2, blending: preparing collagen fibers and cotton fibers into yarns through a blending process;
s3, oxygen bleaching and dyeing: adding yarn into bleaching liquid for bleaching treatment, and then adding the yarn into dye for dyeing treatment;
s4, padding: padding and finishing the yarn after the oxygen bleaching and dyeing treatment, adding the yarn into finishing liquid, dipping, dehydrating and drying to obtain the aromatic microcapsule blended antibacterial cotton fiber; wherein the finishing liquid consists of aromatic microcapsule emulsion and quaternary ammonium salt type polyether modified polysiloxane;
in S1, the molar ratio of EDC to NHS is 2-4: the concentration of EDC/NHS in the 1, EDC/NHS solution is 4-7g/L; the pH of the PBS buffer=7.4, the concentration of collagen in the collagen solution is 10-14wt%; the volume percentage of EDC/NHS solution and collagen solution is 50-60:40-50 parts; the voltage of electrostatic spinning is 15-18kV, the receiving distance is 15-20cm, and the solution advancing speed is 0.4-0.6mL/h; the concentration of glutaraldehyde aqueous solution is 0.3-0.6wt%, and the soaking reaction is carried out for 20-30min at normal temperature;
in-situ crosslinking is carried out by adopting EDC/NHS as a crosslinking agent, so that carboxyl and amino in the molecular structure of the collagen are promoted to combine to form an amide bond, the regularity of collagen molecules is improved before the fiber is formed, the crosslinking effect of EDC/NHS is enhanced in the presence of ethanol, a three-dimensional crosslinked network structure is formed in the fiber, and the transmission of water molecules in the fiber is hindered; then, after the fiber is molded, glutaraldehyde with high crosslinking strength is adopted for impregnation crosslinking, so that the fiber can be well combined with amino groups in collagen molecules on the surface of the fiber, a crosslinked network is formed on the surface of the fiber through crosslinking, water molecules are prevented from entering the fiber from the surface layer of the fiber, and the water resistance of the fiber is improved; in addition, the inside of the fiber is crosslinked in situ to form a three-dimensional porous network structure, the surface layer structure is compact, the fiber has good dyeing performance, and the co-dyeing effect is better after the fiber is blended with cotton fiber for spinning;
in S2, the mass percentage of the collagen fiber and the cotton fiber in the yarn is 30-40:60-70 parts;
the mass ratio of the water phase to the oil phase is 3.8-4.2:1, a step of; the mass ratio of SDS to deionized water in the water phase is 0.8-1.2:100; in the oil phase, the mass ratio of the n-hexadecane, the essential oil, the methacrylic acid monomer and the initiator is 2-2.5:1:3-3.5:0.03-0.04;
in S4, the aromatic microcapsule emulsion is obtained by dispersing an aromatic microcapsule powder in water, and the aromatic microcapsule powder is prepared as follows: dissolving surfactant SDS in deionized water to form a water phase; adding essential oil, methacrylic acid monomer and initiator into n-hexadecane, stirring and mixing to form an oil phase; mixing the water phase and the oil phase, and stirring and emulsifying to obtain emulsion; introducing nitrogen into the emulsion, heating in a water bath, and stirring for reaction to obtain microcapsule suspension; adding saturated calcium chloride emulsion into the microcapsule suspension to demulsify, filtering, washing with absolute ethyl alcohol, and drying at low temperature.
2. The preparation method of the aromatic microcapsule blended antibacterial cotton fiber according to claim 1, wherein the mass ratio of the aromatic microcapsule emulsion to the quaternary ammonium salt polyether modified polysiloxane in the finishing liquid is 92-96:4-8; wherein the solid content of the aromatic microcapsule emulsion is 18-23%.
3. The method for preparing the aromatic microcapsule blended antibacterial cotton fiber according to claim 2, wherein the bath ratio of padding finishing is 1:15-20, soaking at normal temperature for 8-12min, dehydrating, pre-drying at 60-65deg.C for 3-5min, and drying at 115-125deg.C.
4. An aromatic microcapsule blended antibacterial cotton fiber prepared by the method of claim 3.
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