CN114571807A - Multilayer composite medical fabric and preparation method thereof - Google Patents

Multilayer composite medical fabric and preparation method thereof Download PDF

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Publication number
CN114571807A
CN114571807A CN202210314138.3A CN202210314138A CN114571807A CN 114571807 A CN114571807 A CN 114571807A CN 202210314138 A CN202210314138 A CN 202210314138A CN 114571807 A CN114571807 A CN 114571807A
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CN
China
Prior art keywords
mass
fabric
cotton fibers
multilayer composite
layer
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN202210314138.3A
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Chinese (zh)
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CN114571807B (en
Inventor
王伟历
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Xiamen Meirun Medical Technology Co ltd
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Individual
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Priority to CN202210314138.3A priority Critical patent/CN114571807B/en
Priority to CN202310496399.6A priority patent/CN116691085A/en
Publication of CN114571807A publication Critical patent/CN114571807A/en
Application granted granted Critical
Publication of CN114571807B publication Critical patent/CN114571807B/en
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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
    • B32B5/02—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
    • B32B5/022—Non-woven fabric
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B33/00—Layered products characterised by particular properties or particular surface features, e.g. particular surface coatings; Layered products designed for particular purposes not covered by another single class
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/06—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the heating method
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/10—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the pressing technique, e.g. using action of vacuum or fluid pressure
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B38/00—Ancillary operations in connection with laminating processes
    • B32B38/0008—Electrical discharge treatment, e.g. corona, plasma treatment; wave energy or particle radiation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B38/00—Ancillary operations in connection with laminating processes
    • B32B38/08—Impregnating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B38/00—Ancillary operations in connection with laminating processes
    • B32B38/16—Drying; Softening; Cleaning
    • B32B38/162—Cleaning
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B38/00—Ancillary operations in connection with laminating processes
    • B32B38/16—Drying; Softening; Cleaning
    • B32B38/164—Drying
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B32B5/02—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
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    • B32B5/24—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer
    • B32B5/26—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer another layer next to it also being fibrous or filamentary
    • B32B5/262—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer another layer next to it also being fibrous or filamentary characterised by one fibrous or filamentary layer being a woven fabric layer
    • B32B5/263—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer another layer next to it also being fibrous or filamentary characterised by one fibrous or filamentary layer being a woven fabric layer next to one or more woven fabric layers
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    • B32B5/22—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed
    • B32B5/24—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer
    • B32B5/26—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer another layer next to it also being fibrous or filamentary
    • B32B5/265—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer another layer next to it also being fibrous or filamentary characterised by one fibrous or filamentary layer being a non-woven fabric layer
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
    • B32B5/22—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed
    • B32B5/24—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer
    • B32B5/26—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer another layer next to it also being fibrous or filamentary
    • B32B5/275—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer another layer next to it also being fibrous or filamentary characterised by one woven fabric layer next to a non-woven fabric layer
    • 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
    • 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
    • D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
    • D01D5/0092—Electro-spinning characterised by the electro-spinning apparatus characterised by the electrical field, e.g. combined with a magnetic fields, using biased or alternating fields
    • 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
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
    • D01F6/74—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polycondensates of cyclic compounds, e.g. polyimides, polybenzimidazoles
    • D—TEXTILES; PAPER
    • D03—WEAVING
    • D03D—WOVEN FABRICS; METHODS OF WEAVING; LOOMS
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    • D03D15/20—Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used characterised by the material of the fibres or filaments constituting the yarns or threads
    • D03D15/208—Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used characterised by the material of the fibres or filaments constituting the yarns or threads cellulose-based
    • D03D15/217—Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used characterised by the material of the fibres or filaments constituting the yarns or threads cellulose-based natural from plants, e.g. cotton
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    • D03D15/283—Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used characterised by the material of the fibres or filaments constituting the yarns or threads synthetic polymer-based, e.g. polyamide or polyester fibres
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
    • D06B3/00—Passing of textile materials through liquids, gases or vapours to effect treatment, e.g. washing, dyeing, bleaching, sizing, impregnating
    • D06B3/10—Passing of textile materials through liquids, gases or vapours to effect treatment, e.g. washing, dyeing, bleaching, sizing, impregnating of fabrics
    • 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
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    • D06M10/025—Corona discharge or low temperature plasma
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    • D06M11/07—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 halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof
    • D06M11/30—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 halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof with oxides of halogens, oxyacids of halogens or their salts, e.g. with perchlorates
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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    • D06M11/32—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 oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
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    • B32B2307/582—Tearability
    • B32B2307/5825—Tear resistant
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/70—Other properties
    • B32B2307/714—Inert, i.e. inert to chemical degradation, corrosion
    • B32B2307/7145—Rot proof, resistant to bacteria, mildew, mould, fungi
    • 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
    • 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
    • D06M2101/16—Synthetic fibres, other than mineral fibres
    • D06M2101/18—Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/20—Polyalkenes, polymers or copolymers of compounds with alkenyl groups bonded to aromatic groups

Abstract

The invention discloses a multilayer composite medical fabric and a preparation method thereof, and relates to the technical field of textiles. The multilayer composite medical fabric comprises a skin-friendly layer, a crosslinking layer and a protective layer from inside to outside; the skin-friendly layer is a modified cotton fiber fabric; the crosslinking layer is a crosslinked polyimide fabric; the protective layer is a polypropylene non-woven fabric subjected to plasma treatment, the polypropylene non-woven fabric subjected to plasma treatment has improved surface hydrophilicity and can be connected with the crosslinking layer; the modified cotton fiber enables the skin-friendly layer to have antibacterial property; the cross-linked layer is prepared by electrostatic spinning of polyimide with a cross-linked structure inside, so that the fracture toughness of the multilayer composite medical fabric is enhanced.

Description

Multilayer composite medical fabric and preparation method thereof
Technical Field
The invention relates to the technical field of fabrics, in particular to a multilayer composite medical fabric and a preparation method thereof.
Background
With the development of times, people have higher and higher requirements on fabrics, and the fabrics capable of meeting the requirements of consumers are developed and play an increasingly important role in the field of fabric production. The existing single-layer structure textile fabric cannot meet daily requirements of people, particularly has little effect on the aspects of water resistance and air permeability, and is particularly medical fabric.
The cotton fabric has the characteristics of natural fibers, is soft in hand feeling and comfortable to wear, but has the defects of poor oxidation resistance and no antibacterial property. Therefore, the preparation of the multilayer composite medical fabric by taking the cotton fiber fabric as the base material has excellent antibacterial property and fracture toughness.
Disclosure of Invention
The invention aims to provide a multilayer composite medical fabric and a preparation method thereof, and aims to solve the problems in the background technology.
A multilayer composite medical fabric comprises a skin-friendly layer, a cross-linking layer and a protective layer from inside to outside; the skin-friendly layer is a modified cotton fiber fabric; the crosslinking layer is a crosslinked polyimide fabric; the protective layer is polypropylene non-woven fabric subjected to plasma treatment.
Preferably, the modified cotton fiber is prepared by grafting modified chitosan on aldehyde cotton fiber and then reacting with hydrazine hydrate.
Preferably, the cross-linked polyimide fabric is prepared by blending 2, 2' -bis (3, 4-dicarboxyphenyl) hexafluoropropane tetracarboxylic dianhydride and 3, 5-bis (2-trifluoromethyl-4-aminophenoxy) phenol to prepare an electrostatic spinning solution, performing electrostatic spinning to prepare polyimide fibers, and weaving the polyimide fibers into the fabric.
Preferably, the preparation method of the multilayer composite medical fabric comprises the following steps: preparing a skin-friendly layer, preparing a cross-linking layer, preparing a protective layer and preparing a multilayer composite medical fabric.
Preferably, the preparation method of the multilayer composite medical fabric comprises the following specific steps:
(1) dispersing aldehyde cotton fibers in deionized water with the mass of 5-10 times that of the aldehyde cotton fibers, adding modified chitosan with the mass of 0.4-0.6 time that of the aldehyde cotton fibers, stirring at 50-100 rpm, dropwise adding a saturated sodium carbonate solution with the mass of 2-3 times that of the aldehyde cotton fibers, continuing stirring after dropwise adding, reacting for 8-12 hours, fishing out, washing for 3-5 times with deionized water, transferring to absolute ethyl alcohol with the mass of 5-10 times that of the aldehyde cotton fibers, adding hydrazine hydrate with the mass of 0.25-0.3 time that of the aldehyde cotton fibers, continuing stirring for reacting for 3-5 hours, fishing out, washing for 5-8 times with deionized water, and drying in an oven at 40-60 ℃ for 6-8 hours to obtain modified cotton fibers; the modified cotton fiber is subjected to double twisting, spinning and weaving to obtain the modified cotton fiber with the gram weight of 80-120 g/m2The skin-friendly layer of (a);
(2) mixing 3, 5-bis (2-trifluoromethyl-4-aminophenoxy) phenol and dimethylformamide according to the mass ratio of 1: 5-1: 8, adding 2,2 '-bis (3, 4-dicarboxyphenyl) hexafluoropropane tetracarboxylic dianhydride every 10-12 min after fully dissolving, controlling the feeding time to be 1.5-2 h, and the mass ratio of the 2, 2' -bis (3, 4-dicarboxyphenyl) hexafluoropropane tetracarboxylic dianhydride to the 3, 5-bis (2-trifluoromethyl-4-aminophenoxy) phenol to be 1: 1-1.12: 1, stirring and homogenizing for 4-6 h at 50-100 rpm after feeding is finished to prepare an electrostatic spinning solution, carrying out electrostatic spinning to prepare a crosslinked polyimide fiber, carrying out double twisting and spinning on the crosslinked polyimide fiber, after weaving, the gram weight is 40-60 g/m.2The crosslinked layer of (a);
(3) the gram weight is 30 to 60g/m2Soaking the polypropylene non-woven fabric in absolute ethyl alcohol, fishing out and drying after 24-28 h, soaking in acetone, ultrasonically washing for 20-40 min at 40-60 kHz, fishing out, washing for 3-5 times by using deionized water, and drying in an oven at 40-60 ℃ to constant weight to obtain a pretreated polypropylene non-woven fabric; suspending the pretreated polypropylene nonwoven fabric in a plasma apparatusVacuumizing the treatment cavity to 5-10 Pa, introducing oxygen to the vacuum degree of 15-30 Pa, and performing plasma treatment at 80-100W for 4-6 min to obtain a protective layer;
(4) and sequentially placing the skin-friendly layer, the crosslinking layer and the protective layer, pressing by using a hot press at the pressing temperature of 150-180 ℃, and cutting to obtain the multilayer composite medical fabric.
Preferably, in the step (1): the preparation method of the aldehyde group cotton fiber comprises the following steps: soaking cotton fibers in a sodium hydroxide solution with the mass fraction of 18-20% and the mass of 20-30 times of that of the cotton fibers at room temperature, taking out after reacting for 2-4 h, washing with deionized water for 5-8 times, soaking in a potassium periodate solution with the mass fraction of 5-10% and the mass of 40-50 times of that of the cotton fibers, taking out after reacting for 4-6 h in a dark place, transferring to glycerol with the mass of 10-20 times of that of the cotton fibers, taking out after reacting for 1-2 h, washing with deionized water for 5-8 times, and drying to constant weight to obtain the aldehyde-based cotton fibers.
Preferably, in the step (1): the preparation method of the modified chitosan comprises the following steps: mixing chitosan and N-methyl pyrrolidone according to the mass ratio of 1: 20-1: 30 in a nitrogen atmosphere, dropwise adding an N-methyl pyrrolidone solution of chlorobutyryl chloride with the mass fraction of 2-5% which is 2-3 times that of chitosan at the speed of 1-2 ml/min, reacting for 3-5 h, concentrating until no precipitate is generated after washing with diethyl ether, washing with methanol for 3-5 times, adding 2,4, 6-tris (4-hydroxyphenyl) pyridine with the mass of 1.5-1.8 times that of chitosan, stirring and reacting for 72-78 h at 50-100 rpm, concentrating to obtain a precipitate, washing with diethyl ether and methanol for 3-5 times in sequence, and drying to constant weight to obtain the modified chitosan.
Preferably, the preparation method of the 2,4, 6-tris (4-hydroxyphenyl) pyridine comprises the following steps: mixing 4-hydroxyphenylformaldehyde, 4-hydroxyacetophenone, ammonium acetate and glacial acetic acid according to the mass ratio of 1:2:3: 4.5-1: 2.2:3.5:5, heating to 80-90 ℃, carrying out reflux reaction for 3-5 h, cooling to room temperature, adding an acetic acid solution with the mass fraction of 50-60% which is 8-10 times that of 4-hydroxyphenylformaldehyde, carrying out precipitation, stirring at 100-200 rpm for 10-15 min, filtering, recrystallizing with absolute ethyl alcohol, and finally drying at 65-70 ℃ for 12h under vacuum to obtain the 2,4, 6-tris (4-hydroxyphenyl) pyridine.
Preferably, in the step (2): the preparation method of the 3, 5-bis (2-trifluoromethyl-4-aminophenoxy) phenol comprises the following steps: mixing phloroglucinol, 3-trifluoromethyl-4-chloronitrobenzene and sewage potassium carbonate according to the mass ratio of 3:11: 4-3: 11.3-4.2, adding toluene which is 3.2-3.4 times of the mass of phloroglucinol and N, N-dimethylformamide which is 16-18 times of the mass of phloroglucinol, heating to 115-120 ℃, stirring and reacting for 5-5.5 hours at 100-200 rpm, heating to 150-155 ℃, continuing to react for 8-9 hours, cooling to room temperature, washing for 3-5 times with deionized water, adding iron powder which is 3.1-3.3 times of the mass of phloroglucinol, adding a mixed solvent which is 16-18 times of the mass of phloroglucinol, wherein the mass ratio of acetone, ethanol and deionized water in the mixed solvent is 1:1:1, heating to 80-100 ℃ in a nitrogen atmosphere, stirring and refluxing for 5-6 hours at 50-100 rpm, adding sodium hydroxide which is 0.08-0.1 time of the mass of phloroglucinol, continuing to stir for 5-8 minutes, and filtering while the mixture is hot, then carrying out reduced pressure distillation, and recrystallizing by using water and absolute ethyl alcohol to obtain the 3, 5-bis (2-trifluoromethyl-4-aminophenoxy) phenol.
Preferably, during electrostatic spinning, the distance from the injector to the aluminum foil is 15-20 cm, the injection speed of the spinning solution is 0.24-0.5 mL/h, the relative humidity is 5-10%, the temperature is 40-60 ℃, and the voltage of two electrodes is 15-35 kV.
Compared with the prior art, the invention has the following beneficial effects:
the multilayer composite medical fabric comprises a skin-friendly layer, a crosslinking layer and a protective layer from inside to outside; the skin-friendly layer is a modified cotton fiber fabric; the crosslinking layer is a crosslinked polyimide fabric; the protective layer is a polypropylene non-woven fabric subjected to plasma treatment, the polypropylene non-woven fabric subjected to plasma treatment has improved surface hydrophilicity and can be connected with the crosslinking layer;
the modified cotton fiber is prepared by grafting modified chitosan on aldehyde cotton fiber and then reacting with hydrazine hydrate; the modified chitosan is prepared by reacting chitosan with 2,4, 6-tri (4-hydroxyphenyl) pyridine, and a large amount of hydroxyl is introduced while introducing the pyridine; performing alkali treatment on cotton fibers, oxidizing hydroxyl on the cotton fibers into aldehyde groups, reacting the hydroxyl on the modified chitosan with the aldehyde groups to form acetal, reacting with hydrazine hydrate to form Schiff base, polymerizing the modified chitosan on the surfaces of the cotton fibers, and enabling the skin-friendly layer to have antibacterial property;
the cross-linked polyimide fabric is prepared by blending 2, 2' -bis (3, 4-dicarboxyphenyl) hexafluoropropane tetracarboxylic dianhydride and 3, 5-bis (2-trifluoromethyl-4-aminophenoxy) phenol to prepare an electrostatic spinning solution, carrying out electrostatic spinning to prepare polyimide fibers, and weaving the polyimide fibers into the fabric; 2,2 '-bis (3, 4-dicarboxyphenyl) hexafluoropropane tetracarboxylic dianhydride and 3, 5-bis (2-trifluoromethyl-4-aminophenoxy) phenol are blended to form crosslinked polyimide, the residual phenol reacts with carboxylic acid in a polyimide side chain to form ester groups and can also react with carboxyl to form polyimide with an internal crosslinked structure, the strength and the fracture toughness of a crosslinked layer are enhanced, meanwhile, polyimide prepared from the 2, 2' -bis (3, 4-dicarboxyphenyl) hexafluoropropane tetracarboxylic dianhydride and the 3, 5-bis (2-trifluoromethyl-4-aminophenoxy) phenol has a microporous structure and can be adsorbed between two layers when being pressed with a skin-friendly layer and a protective layer, so that the interlayer connection is tight, and the fracture toughness of the fabric is enhanced.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In order to more clearly illustrate the method provided by the present invention, the following examples are used to illustrate the method for testing the indexes of the multilayered composite medical fabric prepared in the examples and the comparative examples as follows:
and (3) antibacterial property: the antibacterial property test of the multilayer composite medical fabrics prepared in the examples and the comparative examples is carried out according to GB/T20944.3.
Fracture toughness: the multi-layer composite medical fabrics prepared in the examples and the comparative examples were subjected to tensile strength test with reference to B/T3923.1.
Example 1
A preparation method of a multilayer composite medical fabric comprises the following steps:
(1) soaking cotton fibers in a sodium hydroxide solution with the mass fraction of 18 percent which is 20 times of the mass of the cotton fibers at room temperature, taking out after reacting for 2 hours, washing with deionized water for 5 times, soaking in a potassium periodate solution with the mass fraction of 5 percent which is 40 times of the mass of the cotton fibers, taking out after reacting in a dark place for 4 hours, transferring to glycerol with the mass of 10 times of the mass of the cotton fibers, taking out after reacting for 1 hour, washing with deionized water for 5 times, and drying to constant weight to obtain aldehyde cotton fibers; mixing 4-hydroxyphenylformaldehyde, 4-hydroxyacetophenone, ammonium acetate and glacial acetic acid according to the mass ratio of 1:2:3:4.5, heating to 80 ℃, carrying out reflux reaction for 3h, cooling to room temperature, adding an acetic acid solution with the mass fraction of 50 percent being 8 times of that of the 4-hydroxyphenylformaldehyde, carrying out precipitation, stirring at 100rpm for 10min, filtering, recrystallizing by using absolute ethyl alcohol, and finally drying at 65 ℃ in vacuum for 12h to obtain 2,4, 6-tris (4-hydroxyphenyl) pyridine; mixing chitosan and N-methyl pyrrolidone according to a mass ratio of 1:20 in a nitrogen atmosphere, dripping N-methyl pyrrolidone solution of chlorobutyryl chloride with the mass fraction of 2 times that of 2 percent of the chitosan at a speed of 1ml/min, reacting for 3 hours, concentrating until no precipitate is generated after washing with diethyl ether, washing with methanol for 3 times, adding 2,4, 6-tris (4-hydroxyphenyl) pyridine with the mass of 1.5 times that of the chitosan, stirring and reacting for 72 hours at 50rpm, concentrating to obtain a precipitate, washing with diethyl ether and methanol for 3 times in sequence, and drying to constant weight to obtain modified chitosan;
(2) dispersing aldehyde cotton fibers in deionized water with the mass 5 times that of the aldehyde cotton fibers, adding modified chitosan with the mass 0.4 time that of the aldehyde cotton fibers, stirring at 50rpm, dropwise adding saturated sodium carbonate solution with the mass 2 times that of the aldehyde cotton fibers, continuing stirring after dropwise adding, reacting for 8 hours, fishing out, washing with deionized water for 3 times, transferring to absolute ethyl alcohol with the mass 5 times that of the aldehyde cotton fibers, adding hydrazine hydrate with the mass 0.25 time that of the aldehyde cotton fibers, continuing stirring for reaction for 3 hours, fishing out, washing with deionized water for 5 times, and drying in a drying oven at 40 ℃ for 6 hours to obtain modified cotton fibers; the modified cotton fiber is subjected to double twisting, spinning and weaving to obtain the modified cotton fiber with the gram weight of 80g/m2The skin-friendly layer of (a);
(3) mixing phloroglucinol, 3-trifluoromethyl-4-chloronitrobenzene and sewage potassium carbonate according to the mass ratio of 3:11:4, adding toluene accounting for 3.2 times of the mass of phloroglucinol and N, N-dimethylformamide accounting for 16 times of the mass of phloroglucinol, heating to 115 ℃, stirring at 100rpm for 5 hours, heating to 150 ℃, continuing to react for 8 hours, cooling to room temperature, washing with deionized water for 3 times, adding iron powder accounting for 3.1 times of the mass of phloroglucinol, adding a mixed solvent accounting for 16 times of the mass of phloroglucinol, wherein the mass ratio of acetone, ethanol and deionized water in the mixed solvent is 1:1:1, heating to 80 ℃ under the nitrogen atmosphere, stirring and refluxing for 5 hours at 50rpm, adding sodium hydroxide accounting for 0.08 times of the mass of phloroglucinol, continuously stirring for 5 minutes, filtering while hot, performing reduced pressure distillation, and recrystallizing with water and anhydrous ethanol, to prepare 3, 5-bis (2-trifluoromethyl-4-aminophenoxy) phenol;
(4) mixing 3, 5-bis (2-trifluoromethyl-4-aminophenoxy) phenol and dimethylformamide according to the mass ratio of 1:5, adding 2,2 '-bis (3, 4-dicarboxyphenyl) hexafluoropropane tetracarboxylic dianhydride every 10min after fully dissolving, controlling the mass ratio of 2, 2' -bis (3, 4-dicarboxyphenyl) hexafluoropropane tetracarboxylic dianhydride to 3, 5-bis (2-trifluoromethyl-4-aminophenoxy) phenol to be 1:1, stirring and homogenizing for 4h at 50rpm after the addition is finished to prepare electrostatic spinning solution, carrying out electrostatic spinning, wherein the distance from an injector to an aluminum foil is 15cm, the injection speed of the spinning solution is 0.24mL/h, the relative humidity is 5%, the temperature is 40 ℃, and the bipolar voltage is 15kV, preparing the crosslinked polyimide fiber, and preparing the crosslinked polyimide fiber with the gram weight of 40g/m after double twisting, spinning and weaving2The crosslinked layer of (a);
(5) the gram weight is 30g/m2Soaking the polypropylene non-woven fabric in absolute ethyl alcohol, fishing out and airing after 24 hours, soaking in acetone, ultrasonically washing for 20min at 40kHz, fishing out, washing for 3 times by using deionized water, and drying in an oven at 40 ℃ to constant weight to obtain a pretreated polypropylene non-woven fabric; suspending the pretreated polypropylene non-woven fabric in a treatment cavity of a plasma instrument, vacuumizing to 5Pa, introducing oxygen to reach a vacuum degree of 15Pa, and performing plasma treatment at 90W for 4min to obtain a protective layer;
(6) and sequentially placing the skin-friendly layer, the crosslinking layer and the protective layer, pressing by using a hot press at the pressing temperature of 150 ℃, and cutting to obtain the multilayer composite medical fabric.
Example 2
A preparation method of a multilayer composite medical fabric comprises the following steps:
(1) soaking cotton fibers in a sodium hydroxide solution with the mass fraction of 19 percent, which is 25 times that of the cotton fibers, at room temperature, taking out after reacting for 3h, washing the cotton fibers with deionized water for 6 times, soaking the cotton fibers in a potassium periodate solution with the mass fraction of 8 percent, reacting in a dark place for 5h, taking out, transferring the cotton fibers to glycerol with the mass fraction of 15 times that of the cotton fibers, taking out after reacting for 1h, washing the cotton fibers with deionized water for 6 times, and drying the cotton fibers to constant weight to obtain aldehyde-based cotton fibers; mixing 4-hydroxyphenylformaldehyde, 4-hydroxyacetophenone, ammonium acetate and glacial acetic acid according to the mass ratio of 1:2:3.2:4.8, heating to 85 ℃, carrying out reflux reaction for 4h, cooling to room temperature, adding an acetic acid solution with the mass fraction of 55 percent being 9 times of that of the 4-hydroxyphenylformaldehyde, carrying out precipitation, stirring at 150rpm for 13min, filtering, recrystallizing by absolute ethyl alcohol, and finally drying at 68 ℃ in vacuum for 12h to obtain 2,4, 6-tris (4-hydroxyphenyl) pyridine; mixing chitosan and N-methyl pyrrolidone according to a mass ratio of 1:25 in a nitrogen atmosphere, dripping N-methyl pyrrolidone solution of chlorobutyryl chloride with the mass fraction of 3 percent, which is 2 times of the mass of chitosan, at a speed of 1ml/min, reacting for 4 hours, concentrating until no precipitate is generated after washing with diethyl ether, washing with methanol for 4 times, adding 2,4, 6-tris (4-hydroxyphenyl) pyridine with the mass of 1.6 times of the mass of chitosan, stirring and reacting for 75 hours at 80rpm, concentrating to obtain a precipitate, washing with diethyl ether and methanol for 4 times in sequence, and drying to constant weight to obtain modified chitosan;
(2) dispersing aldehyde cotton fibers in deionized water with the mass of 8 times that of the aldehyde cotton fibers, adding modified chitosan with the mass of 0.5 time that of the aldehyde cotton fibers, stirring at 80rpm, dropwise adding saturated sodium carbonate solution with the mass of 2-3 times that of the aldehyde cotton fibers, continuing stirring after dropwise adding, reacting for 10 hours, taking out, washing for 4 times by using deionized water, transferring to absolute ethyl alcohol with the mass of 8 times that of the aldehyde cotton fibers, adding hydrazine hydrate with the mass of 0.28 time that of the aldehyde cotton fibers, continuing stirring for reacting for 4 hours, taking out and taking outWashing with deionized water for 6 times, and drying in oven at 50 deg.C for 7 hr to obtain modified cotton fiber; the modified cotton fiber is subjected to double twisting, spinning and weaving to obtain the modified cotton fiber with the gram weight of 100g/m2The skin-friendly layer of (a);
(3) mixing phloroglucinol, 3-trifluoromethyl-4-chloronitrobenzene and sewage potassium carbonate according to the mass ratio of 3:11.2:4.1, adding toluene which is 3.3 times of the mass of phloroglucinol and N, N-dimethylformamide which is 17 times of the mass of phloroglucinol, heating to 118 ℃, stirring and reacting for 5 hours at 150rpm, heating to 153 ℃, continuing to react for 8 hours, cooling to room temperature, washing with deionized water for 4 times, adding iron powder which is 3.2 times of the mass of phloroglucinol, adding a mixed solvent which is 17 times of the mass of phloroglucinol, wherein the mass ratio of acetone, ethanol and deionized water in the mixed solvent is 1:1:1, heating to 90 ℃ under the nitrogen atmosphere, stirring and refluxing for 5 hours at 70rpm, adding sodium hydroxide which is 0.09 times of the mass of phloroglucinol, continuing to stir for 6 minutes, filtering while hot, then carrying out reduced pressure distillation, and carrying out recrystallization by using water and absolute ethanol, to prepare 3, 5-bis (2-trifluoromethyl-4-aminophenoxy) phenol;
(4) mixing 3, 5-bis (2-trifluoromethyl-4-aminophenoxy) phenol and dimethylformamide according to the mass ratio of 1:6, adding 2,2 '-bis (3, 4-dicarboxyphenyl) hexafluoropropane tetracarboxylic dianhydride every 11min after fully dissolving, controlling the mass ratio of the 2, 2' -bis (3, 4-dicarboxyphenyl) hexafluoropropane tetracarboxylic dianhydride to the 3, 5-bis (2-trifluoromethyl-4-aminophenoxy) phenol to be 1.1:1, stirring and homogenizing for 5h at 70rpm after the addition is finished to prepare electrostatic spinning solution, carrying out electrostatic spinning, wherein the distance from an injector to an aluminum foil is 18cm, the injection speed of the spinning solution is 0.4mL/h, the relative humidity is 8%, the temperature is 50 ℃, and the bipolar voltage is 25kV, preparing the crosslinked polyimide fiber, and preparing the crosslinked polyimide fiber into the crosslinked polyimide fiber with the gram weight of 50g/m after double twisting, spinning and weaving2The crosslinked layer of (a);
(5) the gram weight is 40g/m2Soaking the polypropylene non-woven fabric in absolute ethyl alcohol, fishing out and drying after 26h, soaking in acetone, performing ultrasonic washing for 40min at 50kHz, fishing out, washing with deionized water for 4 times, and drying in an oven at 50 ℃ to constant weight to obtain a pretreated polypropylene non-woven fabric; will be pre-treatedSuspending the polypropylene non-woven fabric in a treatment cavity of a plasma instrument, vacuumizing to 8Pa, introducing oxygen to the vacuum degree of 20Pa, and performing plasma treatment at 90W for 5min to obtain a protective layer;
(6) sequentially placing the skin-friendly layer, the crosslinking layer and the protective layer, pressing by using a hot press at 165 ℃, and cutting to obtain the multilayer composite medical fabric.
Example 3
A preparation method of a multilayer composite medical fabric comprises the following steps:
(1) soaking cotton fibers in a sodium hydroxide solution with the mass fraction of 20% which is 30 times that of the cotton fibers at room temperature, taking out after reacting for 4h, washing with deionized water for 8 times, soaking in a potassium periodate solution with the mass fraction of 10% which is 50 times that of the cotton fibers, taking out after reacting for 6h in a dark place, transferring to glycerol with the mass fraction of 20 times that of the cotton fibers, taking out after reacting for 2h, washing with deionized water for 8 times, and drying to constant weight to obtain aldehyde-based cotton fibers; mixing 4-hydroxyphenylformaldehyde, 4-hydroxyacetophenone, ammonium acetate and glacial acetic acid according to the mass ratio of 1:2.2:3.5:5, heating to 90 ℃, carrying out reflux reaction for 5 hours, cooling to room temperature, adding an acetic acid solution with the mass fraction of 60 percent being 10 times of that of the 4-hydroxyphenylformaldehyde, carrying out precipitation, stirring at 200rpm for 10-15 min, filtering, recrystallizing by using absolute ethyl alcohol, and finally drying at 70 ℃ in vacuum for 12 hours to prepare 2,4, 6-tris (4-hydroxyphenyl) pyridine; mixing chitosan and N-methyl pyrrolidone according to a mass ratio of 1:30 in a nitrogen atmosphere, dripping N-methyl pyrrolidone solution of chlorobutyryl chloride with the mass fraction of 5% which is 3 times that of chitosan at a speed of 2ml/min, reacting for 3-5 h, concentrating until no precipitate is generated after washing with diethyl ether, washing with methanol for 5 times, adding 2,4, 6-tris (4-hydroxyphenyl) pyridine with the mass of 1.8 times that of chitosan, stirring at 100rpm for reaction for 78h, concentrating to obtain a precipitate, washing with diethyl ether and methanol for 5 times in sequence, and drying to constant weight to obtain modified chitosan;
(2) dispersing aldehyde cotton fiber in deionized water with the mass of 10 times that of the aldehyde cotton fiber, adding modified chitosan with the mass of 0.6 time that of the aldehyde cotton fiber, stirring at 100rpm, and dropwise adding saturated chitosan with the mass of 3 times that of the aldehyde cotton fiberContinuously stirring the sodium carbonate solution after the dropwise adding is finished, reacting for 12h, fishing out, washing for 5 times by using deionized water, transferring the sodium carbonate solution into absolute ethyl alcohol with the mass of 10 times that of the aldehyde cotton fibers, adding hydrazine hydrate with the mass of 0.3 time that of the aldehyde cotton fibers, continuously stirring and reacting for 5h, fishing out, washing for 8 times by using deionized water, and drying for 8h in a drying oven at 60 ℃ to obtain modified cotton fibers; the modified cotton fiber is subjected to double twisting, spinning and weaving to obtain the modified cotton fiber with the gram weight of 120g/m2The skin-friendly layer of (a);
(3) mixing phloroglucinol, 3-trifluoromethyl-4-chloronitrobenzene and sewage potassium carbonate according to the mass ratio of 3:11: 4-3: 11.3-4.2, adding toluene which is 3.4 times of the mass of phloroglucinol and N, N-dimethylformamide which is 16-18 times of the mass of phloroglucinol, heating to 120 ℃, stirring and reacting for 5.5 hours at 200rpm, heating to 155 ℃, continuing to react for 9 hours, cooling to room temperature, washing for 5 times with deionized water, adding iron powder which is 3.3 times of the mass of phloroglucinol, adding a mixed solvent which is 18 times of the mass of phloroglucinol, wherein the mass ratio of acetone, ethanol and deionized water in the mixed solvent is 1:1:1, heating to 100 ℃ under the nitrogen atmosphere, stirring and refluxing for 6 hours at 100rpm, adding sodium hydroxide which is 0.1 time of the mass of phloroglucinol, continuing to stir for 8 minutes, then filtering while hot, then carrying out reduced pressure distillation, and carrying out recrystallization by using water and absolute ethanol, to prepare 3, 5-bis (2-trifluoromethyl-4-aminophenoxy) phenol;
(4) mixing 3, 5-bis (2-trifluoromethyl-4-aminophenoxy) phenol and dimethylformamide according to the mass ratio of 1:8, adding 2,2 '-bis (3, 4-dicarboxyphenyl) hexafluoropropane tetracarboxylic dianhydride every 12min after fully dissolving, controlling the mass ratio of 2h to 2, 2' -bis (3, 4-dicarboxyphenyl) hexafluoropropane tetracarboxylic dianhydride to 3, 5-bis (2-trifluoromethyl-4-aminophenoxy) phenol to be 1.12:1, stirring and homogenizing for 6h at 100rpm after the addition is finished to prepare electrostatic spinning solution, carrying out electrostatic spinning, wherein the distance from an injector to an aluminum foil is 20cm, the injection speed of the spinning solution is 0.5mL/h, the relative humidity is 10%, the temperature is 60 ℃, and the bipolar voltage is 35kV, preparing the crosslinked polyimide fiber, and preparing the crosslinked polyimide fiber with the gram weight of 60g/m after double twisting, spinning and weaving2The crosslinked layer of (a);
(5) the gram weight is 60g/m2Soaking the polypropylene non-woven fabric in absolute ethyl alcohol, fishing out and drying after 28h, soaking in acetone, performing ultrasonic washing for 40min at 60kHz, fishing out, washing for 5 times by using deionized water, and drying in an oven at 60 ℃ to constant weight to obtain a pretreated polypropylene non-woven fabric; suspending the pretreated polypropylene non-woven fabric in a treatment cavity of a plasma instrument, vacuumizing to 10Pa, introducing oxygen to a vacuum degree of 30Pa, and performing plasma treatment at 100W for 6min to obtain a protective layer;
(6) and sequentially placing the skin-friendly layer, the crosslinking layer and the protective layer, pressing by using a hot press at the pressing temperature of 180 ℃, and cutting to obtain the multilayer composite medical fabric.
Comparative example 1
The formulation of comparative example 1 was the same as that of example 2. The preparation method of the multilayer composite medical fabric is different from the preparation method of the example 2 only in the difference of the step (2), and the step (2) is modified as follows: (2) dispersing aldehyde cotton fibers in deionized water with the mass 8 times that of the aldehyde cotton fibers, adding modified chitosan with the mass 0.5 time that of the aldehyde cotton fibers, stirring at 80rpm, dropwise adding a saturated sodium carbonate solution with the mass 2-3 times that of the aldehyde cotton fibers, continuing stirring after dropwise adding, reacting for 10 hours, taking out, washing for 4 times by using the deionized water, and drying for 7 hours in an oven at 50 ℃ to obtain the modified cotton fibers; the modified cotton fiber is subjected to double twisting, spinning and weaving to obtain the modified cotton fiber with the gram weight of 100g/m2The skin-friendly layer of (1).
Comparative example 2
Comparative example 2 was formulated in the same manner as in example 2. The preparation method of the multilayer composite medical fabric is different from the example 2 only in that the treatment of the step (1) is not carried out, and the step (2) is modified as follows: dispersing aldehyde cotton fibers in deionized water with the mass of 8 times that of the aldehyde cotton fibers, adding chitosan with the mass of 0.5 time that of the aldehyde cotton fibers, stirring at 80rpm, dropwise adding saturated sodium carbonate solution with the mass of 2-3 times that of the aldehyde cotton fibers, continuing stirring after dropwise adding, reacting for 10 hours, fishing out, washing with deionized water for 4 times, transferring to absolute ethyl alcohol with the mass of 8 times that of the aldehyde cotton fibers, adding hydrazine hydrate with the mass of 0.28 time that of the aldehyde cotton fibers, continuing stirring for reacting for 4 hours, fishing out, washing with deionized water for 6 times, placing in a drying oven, and drying in a drying ovenDrying at 50 ℃ for 7h to obtain modified cotton fibers; the modified cotton fiber is subjected to double twisting, spinning and weaving to obtain the modified cotton fiber with the gram weight of 100g/m2The skin-friendly layer of (1).
Comparative example 3
The formulation of comparative example 3 was the same as that of example 2. The preparation method of the multilayer composite medical fabric is different from the preparation method of the example 2 only in the steps (1) and (2), and the steps (1) and (2) are modified as follows: (1) soaking cotton fibers in a sodium hydroxide solution with the mass fraction of 19 percent, which is 25 times that of the cotton fibers, at room temperature, taking out after reacting for 3h, washing the cotton fibers with deionized water for 6 times, soaking the cotton fibers in a potassium periodate solution with the mass fraction of 8 percent, reacting in a dark place for 5h, taking out, transferring the cotton fibers to glycerol with the mass fraction of 15 times that of the cotton fibers, taking out after reacting for 1h, washing the cotton fibers with deionized water for 6 times, and drying the cotton fibers to constant weight to obtain modified cotton fibers; (2) the modified cotton fiber is subjected to double twisting, spinning and weaving to obtain the modified cotton fiber with the gram weight of 100g/m2The skin-friendly layer of (1).
Comparative example 4
The formulation of comparative example 4 was the same as example 2. The preparation method of the multilayer composite medical fabric is different from the example 2 only in that the treatment of the step (3) is not carried out, and the step (4) is modified as follows: mixing p-phenylenediamine and dimethylformamide according to the mass ratio of 1:6, fully dissolving, adding 2,2 '-bis (3, 4-dicarboxyphenyl) hexafluoropropane tetracarboxylic dianhydride every 11min, controlling the feeding time to be 1.5h, controlling the mass ratio of the 2, 2' -bis (3, 4-dicarboxyphenyl) hexafluoropropane tetracarboxylic dianhydride to the p-phenylenediamine to be 1.1:1, stirring and homogenizing for 5h at 70rpm after feeding is finished, preparing an electrostatic spinning solution, carrying out electrostatic spinning, wherein the distance from an injector to an aluminum foil is 18cm, the injection speed of the spinning solution is 0.4mL/h, the relative humidity is 8%, the temperature is 50 ℃, the bipolar voltage is 25kV, preparing crosslinked polyimide fibers, and after double twisting, spinning and weaving the crosslinked polyimide fibers, preparing the cross-linked polyimide fibers with the gram weight of 50g/m2The crosslinked layer of (1).
Comparative example 5
The formulation of comparative example 5 was the same as example 2. The preparation method of the multilayer composite medical fabric is different from the embodiment 2 only in the difference of the step (4), and the step (4) is modified as follows: mixing 3, 5-di (2-trifluoromethyl)Mixing base-4-aminophenoxy) phenol and dimethylformamide according to the mass ratio of 1:6, adding pyromellitic dianhydride every 11min after fully dissolving, controlling the feeding time to be 1.5h, the mass ratio of the pyromellitic dianhydride to the 3, 5-bis (2-trifluoromethyl-4-aminophenoxy) phenol to be 1.1:1, stirring and homogenizing for 5h at 70rpm after feeding is finished, preparing electrostatic spinning solution, carrying out electrostatic spinning, wherein the distance from an injector to an aluminum foil is 18cm, the speed of the spinning solution is 0.4mL/h, the relative humidity is 8%, the injection temperature is 50 ℃, the bipolar voltage is 25kV, preparing crosslinked polyimide fibers, and preparing the crosslinked polyimide fibers by carrying out double twisting, spinning and weaving to obtain the crosslinked polyimide fibers with the gram weight of 50g/m2Cross-linked layer of
Effect example 1
Table 1 below shows the results of performance analysis of the multi-layer composite medical fabrics using examples 1, 2, and 3 of the present invention and comparative examples 1, 2, 3,4, and 5.
TABLE 1
Antibacterial ratio (%) Elongation at Break (%)
Example 1 95.9 38.4
Example 2 94.3 37.2
Example 3 96.8 36.9
Comparative example 1 78.2 35.7
Comparative example 2 54.3 36.1
Comparative example 3 21.4 37.3
Comparative example 4 94.0 25.4
Comparative example 5 93.7 21.6
Compared with the experimental data of the comparative examples and the examples in the table 1, it can be obviously found that the antibacterial property and the fracture toughness of the multilayer composite medical fabrics prepared in the examples 1, 2 and 3 are better;
from the comparison of experimental data of examples 1, 2 and 3 and comparative examples 1, 2 and 3, it can be seen that, when preparing modified cotton fibers, chitosan grafted on aldehyde-based cotton fibers reacts with 2,4, 6-tris (4-hydroxyphenyl) pyridine to prepare modified chitosan, then the modified chitosan reacts with hydrazine hydrate, a great amount of hydroxyl is introduced while introducing pyridine, the hydroxyl on the modified chitosan reacts with aldehyde groups on the cotton fibers to form acetal, and then the acetal reacts with hydrazine hydrate to form Schiff base, and the modified chitosan is polymerized on the surfaces of the cotton fibers, so that the skin-friendly layer has excellent antibacterial property; from the comparison of experimental data of examples 1, 2, 3 and comparative examples 4 and 5, it can be found that the polyimide fiber is prepared by blending 2, 2' -bis (3, 4-dicarboxyphenyl) hexafluoropropane tetracarboxylic dianhydride with 3, 5-bis (2-trifluoromethyl-4-aminophenoxy) phenol to prepare an electrospinning solution, and then the electrospinning solution is used for electrospinning, and the crosslinked polyimide fabric is prepared by weaving the fabric to be used as a crosslinked layer, so that not only the polyimide with a crosslinked structure inside is formed, and the strength and the fracture toughness of the crosslinked layer are enhanced, but also the crosslinked polyimide fabric has a microporous structure, and when the crosslinked polyimide fabric is pressed with a skin-friendly layer and a protective layer, the polyimide fabric can be adsorbed between the two layers, so that the interlayer connection is tight, and the fracture toughness of the fabric is enhanced.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.

Claims (10)

1. A multilayer composite medical fabric comprises a skin-friendly layer, a cross-linking layer and a protective layer from inside to outside; the fabric is characterized in that the skin-friendly layer is a modified cotton fiber fabric; the crosslinking layer is a crosslinked polyimide fabric; the protective layer is polypropylene non-woven fabric subjected to plasma treatment.
2. The multilayer composite medical fabric as claimed in claim 1, wherein the modified cotton fiber is prepared by grafting modified chitosan onto an aldehyde cotton fiber and then reacting with hydrazine hydrate.
3. The multilayer composite medical fabric according to claim 1, wherein the crosslinked polyimide fabric is prepared by blending 2, 2' -bis (3, 4-dicarboxyphenyl) hexafluoropropane tetracarboxylic dianhydride and 3, 5-bis (2-trifluoromethyl-4-aminophenoxy) phenol to prepare an electrospinning solution, performing electrospinning to prepare polyimide fibers, and weaving the polyimide fibers into the fabric.
4. A preparation method of a multilayer composite medical fabric is characterized by comprising the following steps: preparing a skin-friendly layer, preparing a cross-linking layer, preparing a protective layer and preparing a multilayer composite medical fabric.
5. The preparation method of the multilayer composite medical fabric according to claim 4, which is characterized by comprising the following specific steps of:
(1) dispersing aldehyde cotton fibers in deionized water with the mass of 5-10 times that of the aldehyde cotton fibers, adding modified chitosan with the mass of 0.4-0.6 time that of the aldehyde cotton fibers, stirring at 50-100 rpm, dropwise adding a saturated sodium carbonate solution with the mass of 2-3 times that of the aldehyde cotton fibers, continuing stirring after dropwise adding, reacting for 8-12 hours, fishing out, washing for 3-5 times with deionized water, transferring to absolute ethyl alcohol with the mass of 5-10 times that of the aldehyde cotton fibers, adding hydrazine hydrate with the mass of 0.25-0.3 time that of the aldehyde cotton fibers, continuing stirring for reacting for 3-5 hours, fishing out, washing for 5-8 times with deionized water, and drying in an oven at 40-60 ℃ for 6-8 hours to obtain modified cotton fibers; the modified cotton fiber is subjected to double twisting, spinning and weaving to obtain the modified cotton fiber with the gram weight of 80-120 g/m2The skin-friendly layer of (a);
(2) mixing 3, 5-bis (2-trifluoromethyl-4-aminophenoxy) phenol and dimethylformamide according to the mass ratio of 1: 5-1: 8, adding 2,2 '-bis (3, 4-dicarboxyphenyl) hexafluoropropane tetracarboxylic dianhydride every 10-12 min after fully dissolving, controlling the feeding time to be 1.5-2 h, and the mass ratio of the 2, 2' -bis (3, 4-dicarboxyphenyl) hexafluoropropane tetracarboxylic dianhydride to the 3, 5-bis (2-trifluoromethyl-4-aminophenoxy) phenol to be 1: 1-1.12: 1, stirring and homogenizing for 4-6 h at 50-100 rpm after feeding is finished to prepare an electrostatic spinning solution, carrying out electrostatic spinning to prepare a crosslinked polyimide fiber, carrying out double twisting and spinning on the crosslinked polyimide fiber, after weaving, the gram weight is 40-60 g/m.2The crosslinked layer of (a);
(3) the gram weight is 30 to 60g/m2Soaking the polypropylene non-woven fabric in absolute ethyl alcohol, fishing out after 24-28 h, and airingDrying, soaking in acetone, performing ultrasonic washing at 40-60 kHz for 20-40 min, taking out, washing with deionized water for 3-5 times, and drying in an oven at 40-60 ℃ to constant weight to obtain a pretreated polypropylene non-woven fabric; suspending the pretreated polypropylene non-woven fabric in a treatment cavity of a plasma instrument, vacuumizing to 5-10 Pa, introducing oxygen to reach a vacuum degree of 15-30 Pa, and performing plasma treatment at 80-100W for 4-6 min to obtain a protective layer;
(4) and sequentially placing the skin-friendly layer, the crosslinking layer and the protective layer, pressing by using a hot press at the pressing temperature of 150-180 ℃, and cutting to obtain the multilayer composite medical fabric.
6. The method for preparing the multilayer composite medical fabric as claimed in claim 5, wherein in the step (1): the preparation method of the aldehyde group cotton fiber comprises the following steps: soaking cotton fibers in a sodium hydroxide solution with the mass fraction of 18-20% and the mass of 20-30 times of that of the cotton fibers at room temperature, taking out after reacting for 2-4 h, washing with deionized water for 5-8 times, soaking in a potassium periodate solution with the mass fraction of 5-10% and the mass of 40-50 times of that of the cotton fibers, taking out after reacting for 4-6 h in a dark place, transferring to glycerol with the mass of 10-20 times of that of the cotton fibers, taking out after reacting for 1-2 h, washing with deionized water for 5-8 times, and drying to constant weight to obtain the aldehyde-based cotton fibers.
7. The method for preparing the multilayer composite medical fabric according to claim 5, wherein in the step (1): the preparation method of the modified chitosan comprises the following steps: mixing chitosan and N-methyl pyrrolidone according to the mass ratio of 1: 20-1: 30 in a nitrogen atmosphere, dropwise adding an N-methyl pyrrolidone solution of chlorobutyryl chloride with the mass fraction of 2-5% which is 2-3 times that of chitosan at the speed of 1-2 ml/min, reacting for 3-5 h, concentrating until no precipitate is generated after washing with diethyl ether, washing with methanol for 3-5 times, adding 2,4, 6-tris (4-hydroxyphenyl) pyridine with the mass of 1.5-1.8 times that of chitosan, stirring and reacting for 72-78 h at 50-100 rpm, concentrating to obtain a precipitate, washing with diethyl ether and methanol for 3-5 times in sequence, and drying to constant weight to obtain the modified chitosan.
8. The preparation method of the multilayer composite medical fabric according to claim 7, wherein the preparation method of the 2,4, 6-tris (4-hydroxyphenyl) pyridine comprises the following steps: mixing and heating 4-hydroxyphenylformaldehyde, 4-hydroxyacetophenone, ammonium acetate and glacial acetic acid according to the mass ratio of 1:2:3: 4.5-1: 2.2:3.5:5 to 80-90 ℃, carrying out reflux reaction for 3-5 h, cooling to room temperature, adding an acetic acid solution with the mass fraction of 50-60% which is 8-10 times that of 4-hydroxyphenylformaldehyde to carry out precipitation, stirring at 100-200 rpm for 10-15 min, filtering, recrystallizing with absolute ethanol, and finally drying at 65-70 ℃ for 12h under vacuum to obtain the 2,4, 6-tris (4-hydroxyphenyl) pyridine.
9. The method for preparing the multilayer composite medical fabric according to claim 7, wherein in the step (2): the preparation method of the 3, 5-bis (2-trifluoromethyl-4-aminophenoxy) phenol comprises the following steps: mixing phloroglucinol, 3-trifluoromethyl-4-chloronitrobenzene and sewage potassium carbonate according to the mass ratio of 3:11: 4-3: 11.3-4.2, adding toluene which is 3.2-3.4 times of the mass of phloroglucinol and N, N-dimethylformamide which is 16-18 times of the mass of phloroglucinol, heating to 115-120 ℃, stirring and reacting for 5-5.5 hours at 100-200 rpm, heating to 150-155 ℃, continuing to react for 8-9 hours, cooling to room temperature, washing for 3-5 times with deionized water, adding iron powder which is 3.1-3.3 times of the mass of phloroglucinol, adding a mixed solvent which is 16-18 times of the mass of phloroglucinol, wherein the mass ratio of acetone, ethanol and deionized water in the mixed solvent is 1:1:1, heating to 80-100 ℃ in a nitrogen atmosphere, stirring and refluxing for 5-6 hours at 50-100 rpm, adding sodium hydroxide which is 0.08-0.1 time of the mass of phloroglucinol, continuing to stir for 5-8 minutes, and filtering while the mixture is hot, then carrying out reduced pressure distillation, and recrystallizing by using water and absolute ethyl alcohol to obtain the 3, 5-bis (2-trifluoromethyl-4-aminophenoxy) phenol.
10. The method for preparing the multilayer composite medical fabric according to claim 6, wherein in the step (3): during electrostatic spinning, the distance between an injector and an aluminum foil is 15-20 cm, the injection speed of the spinning solution is 0.24-0.5 mL/h, the relative humidity is 5-10%, the temperature is 40-60 ℃, and the bipolar voltage is 15-35 kV.
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