CN114889263A - Medical high-performance fiber composite material and preparation method thereof - Google Patents
Medical high-performance fiber composite material and preparation method thereof Download PDFInfo
- Publication number
- CN114889263A CN114889263A CN202210704367.6A CN202210704367A CN114889263A CN 114889263 A CN114889263 A CN 114889263A CN 202210704367 A CN202210704367 A CN 202210704367A CN 114889263 A CN114889263 A CN 114889263A
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- CN
- China
- Prior art keywords
- composite material
- spunlace
- waterproof
- fiber composite
- under
- 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.)
- Pending
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- 239000002131 composite material Substances 0.000 title claims abstract description 81
- 229920006253 high performance fiber Polymers 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title claims abstract description 37
- 239000004744 fabric Substances 0.000 claims abstract description 81
- CSHWQDPOILHKBI-UHFFFAOYSA-N peryrene Natural products C1=CC(C2=CC=CC=3C2=C2C=CC=3)=C3C2=CC=CC3=C1 CSHWQDPOILHKBI-UHFFFAOYSA-N 0.000 claims abstract description 45
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 33
- 238000002156 mixing Methods 0.000 claims abstract description 32
- KLMPLIAOJUSKMQ-UHFFFAOYSA-N CC(CCC(C=C)=C=O)=C=O Chemical compound CC(CCC(C=C)=C=O)=C=O KLMPLIAOJUSKMQ-UHFFFAOYSA-N 0.000 claims abstract description 29
- 238000001179 sorption measurement Methods 0.000 claims abstract description 23
- -1 benzimidazole compound Chemical class 0.000 claims abstract description 17
- BKOOJFVKBBKUBH-UHFFFAOYSA-N NC(C(N)=C(C=C1)Br)=C1C1=CC(C(C=CC(Br)=C2N)=C2N)=CC(C(C=CC(Br)=C2N)=C2N)=C1 Chemical compound NC(C(N)=C(C=C1)Br)=C1C1=CC(C(C=CC(Br)=C2N)=C2N)=CC(C(C=CC(Br)=C2N)=C2N)=C1 BKOOJFVKBBKUBH-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000000889 atomisation Methods 0.000 claims abstract description 13
- 125000002080 perylenyl group Chemical group C1(=CC=C2C=CC=C3C4=CC=CC5=CC=CC(C1=C23)=C45)* 0.000 claims abstract description 12
- 229920003043 Cellulose fiber Polymers 0.000 claims abstract description 11
- JDQLUYWHCUWSJE-UHFFFAOYSA-N methanolate;titanium(3+) Chemical compound [Ti+3].[O-]C.[O-]C.[O-]C JDQLUYWHCUWSJE-UHFFFAOYSA-N 0.000 claims abstract description 11
- 230000000243 photosynthetic effect Effects 0.000 claims abstract description 10
- 229920002972 Acrylic fiber Polymers 0.000 claims abstract description 9
- 125000005395 methacrylic acid group Chemical group 0.000 claims abstract description 9
- 239000013317 conjugated microporous polymer Substances 0.000 claims abstract description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 48
- 238000003756 stirring Methods 0.000 claims description 45
- 238000001816 cooling Methods 0.000 claims description 33
- 238000007664 blowing Methods 0.000 claims description 32
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 30
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 26
- 238000001291 vacuum drying Methods 0.000 claims description 26
- 238000009987 spinning Methods 0.000 claims description 23
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 22
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 22
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 20
- 238000001914 filtration Methods 0.000 claims description 18
- 239000004594 Masterbatch (MB) Substances 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 15
- 238000005406 washing Methods 0.000 claims description 15
- 239000000835 fiber Substances 0.000 claims description 14
- 238000005096 rolling process Methods 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 13
- 229910052757 nitrogen Inorganic materials 0.000 claims description 13
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 13
- JIPHTMBKXJMSKY-UHFFFAOYSA-N 3-aminoprop-1-en-2-ol Chemical group NCC(O)=C JIPHTMBKXJMSKY-UHFFFAOYSA-N 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 11
- 229910021641 deionized water Inorganic materials 0.000 claims description 11
- 238000005286 illumination Methods 0.000 claims description 11
- NFHFRUOZVGFOOS-UHFFFAOYSA-N palladium;triphenylphosphane Chemical compound [Pd].C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 NFHFRUOZVGFOOS-UHFFFAOYSA-N 0.000 claims description 10
- 230000008569 process Effects 0.000 claims description 10
- 238000009960 carding Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- IUKPWYDLDSUYIB-UHFFFAOYSA-N 3-tert-butyl-2-pyridin-2-ylpyridine Chemical compound CC(C)(C)C1=CC=CN=C1C1=CC=CC=N1 IUKPWYDLDSUYIB-UHFFFAOYSA-N 0.000 claims description 7
- KTYAQHYBYRVCGD-UHFFFAOYSA-N [Ir].COC1=CC=CCCCC1 Chemical class [Ir].COC1=CC=CCCCC1 KTYAQHYBYRVCGD-UHFFFAOYSA-N 0.000 claims description 7
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 claims description 7
- IPWKHHSGDUIRAH-UHFFFAOYSA-N bis(pinacolato)diboron Chemical compound O1C(C)(C)C(C)(C)OB1B1OC(C)(C)C(C)(C)O1 IPWKHHSGDUIRAH-UHFFFAOYSA-N 0.000 claims description 6
- 238000001723 curing Methods 0.000 claims description 6
- 239000001307 helium Substances 0.000 claims description 6
- 229910052734 helium Inorganic materials 0.000 claims description 6
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 6
- 238000000944 Soxhlet extraction Methods 0.000 claims description 5
- 238000007710 freezing Methods 0.000 claims description 5
- 230000008014 freezing Effects 0.000 claims description 5
- 238000010992 reflux Methods 0.000 claims description 5
- 238000010030 laminating Methods 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract description 12
- 230000000844 anti-bacterial effect Effects 0.000 abstract description 7
- 239000004408 titanium dioxide Substances 0.000 abstract description 6
- 238000003475 lamination Methods 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 20
- 239000000203 mixture Substances 0.000 description 11
- 239000000463 material Substances 0.000 description 8
- ZGEGCLOFRBLKSE-UHFFFAOYSA-N methylene hexane Natural products CCCCCC=C ZGEGCLOFRBLKSE-UHFFFAOYSA-N 0.000 description 8
- 230000002265 prevention Effects 0.000 description 5
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 4
- 238000001125 extrusion Methods 0.000 description 4
- 230000001681 protective effect Effects 0.000 description 4
- 238000010561 standard procedure Methods 0.000 description 4
- 125000003277 amino group Chemical group 0.000 description 3
- 239000004750 melt-blown nonwoven Substances 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- 239000004745 nonwoven fabric Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- CERQOIWHTDAKMF-UHFFFAOYSA-M methacrylate group Chemical group C(C(=C)C)(=O)[O-] CERQOIWHTDAKMF-UHFFFAOYSA-M 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 2
- BBEAQIROQSPTKN-UHFFFAOYSA-N pyrene Chemical compound C1=CC=C2C=CC3=CC=CC4=CC=C1C2=C43 BBEAQIROQSPTKN-UHFFFAOYSA-N 0.000 description 2
- 238000004659 sterilization and disinfection Methods 0.000 description 2
- 238000010257 thawing Methods 0.000 description 2
- BMIBJCFFZPYJHF-UHFFFAOYSA-N 2-methoxy-5-methyl-3-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)pyridine Chemical compound COC1=NC=C(C)C=C1B1OC(C)(C)C(C)(C)O1 BMIBJCFFZPYJHF-UHFFFAOYSA-N 0.000 description 1
- 206010019345 Heat stroke Diseases 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000003385 bacteriostatic effect Effects 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- VBXDEEVJTYBRJJ-UHFFFAOYSA-N diboronic acid Chemical compound OBOBO VBXDEEVJTYBRJJ-UHFFFAOYSA-N 0.000 description 1
- 239000011363 dried mixture Substances 0.000 description 1
- GVEPBJHOBDJJJI-UHFFFAOYSA-N fluoranthrene Natural products C1=CC(C2=CC=CC=C22)=C3C2=CC=CC3=C1 GVEPBJHOBDJJJI-UHFFFAOYSA-N 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- OKPYIWASQZGASP-UHFFFAOYSA-N n-(2-hydroxypropyl)-2-methylprop-2-enamide Chemical compound CC(O)CNC(=O)C(C)=C OKPYIWASQZGASP-UHFFFAOYSA-N 0.000 description 1
- 125000000449 nitro group Chemical group [O-][N+](*)=O 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- 239000013618 particulate matter Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920000128 polypyrrole Polymers 0.000 description 1
- 230000033764 rhythmic process Effects 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 210000004243 sweat Anatomy 0.000 description 1
- LOJPEGWUHVRGBN-UHFFFAOYSA-J tetrachlorotitanium;triethylalumane Chemical compound [Cl-].[Cl-].[Cl-].[Cl-].[Ti+4].CC[Al](CC)CC LOJPEGWUHVRGBN-UHFFFAOYSA-J 0.000 description 1
Classifications
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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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- A—HUMAN NECESSITIES
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- A41D31/04—Materials specially adapted for outerwear characterised by special function or use
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- A—HUMAN NECESSITIES
- A41—WEARING APPAREL
- A41D—OUTERWEAR; PROTECTIVE GARMENTS; ACCESSORIES
- A41D31/00—Materials specially adapted for outerwear
- A41D31/04—Materials specially adapted for outerwear characterised by special function or use
- A41D31/10—Impermeable to liquids, e.g. waterproof; Liquid-repellent
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- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
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- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
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- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
- D04H1/4382—Stretched reticular film fibres; Composite fibres; Mixed fibres; Ultrafine fibres; Fibres for artificial leather
- D04H1/43825—Composite fibres
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- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
- D04H1/4382—Stretched reticular film fibres; Composite fibres; Mixed fibres; Ultrafine fibres; Fibres for artificial leather
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- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
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- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
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- B32B2307/00—Properties of the layers or laminate
- B32B2307/70—Other properties
- B32B2307/726—Permeability to liquids, absorption
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- B32B2535/00—Medical equipment, e.g. bandage, prostheses, catheter
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- Physics & Mathematics (AREA)
- Fluid Mechanics (AREA)
- Manufacturing & Machinery (AREA)
- Nonwoven Fabrics (AREA)
Abstract
The invention discloses a medical high-performance fiber composite material and a preparation method thereof, and relates to the technical field of composite materials. The preparation method comprises the steps of mixing 1, 7-dinitro-6, 12-diacrylic acid perylene with 1,3, 5-tris (2, 3-diamino-4-bromophenyl) benzene to form perylene-based conjugated microporous polymer and benzimidazole compound, and preparing waterproof spunlace fabric; then, poly 3-amino-2-hydroxyl acrylic fiber and methacrylic trimethoxy titanium are mixed and melt-blown to form an N- (2-hydroxypropyl) methacrylamide compound and a titanium dioxide network, so as to obtain superfine melt-blown fabric with high adsorption function; and finally, laying the cellulose fiber spunlace cloth serving as an inner layer, the superfine high-adsorption function meltblown cloth serving as an intermediate layer and the waterproof spunlace cloth serving as an outer layer, and carrying out photosynthetic atomization lamination by using 3, 6-dicarbonyl heptene to obtain the medical high-performance fiber composite material with good antibacterial property, water resistance, peeling resistance and tensile strength.
Description
Technical Field
The invention relates to the technical field of composite materials, in particular to a medical high-performance fiber composite material and a preparation method thereof.
Background
From 2019 to the present, the occurrence of epidemic situation has great influence on the economic development and social stability of countries in the world. Meanwhile, the rhythm and stability of the daily life of people are greatly influenced. Therefore, epidemic prevention materials such as disposable masks, protective clothing, disinfection wet tissues and the like play an important role in the period. However, due to technical barriers, the quality and comfort of a large amount of epidemic prevention materials are poor, and the phenomena that medical workers are suffocated with sweat and even heatstroke shock by wearing protective clothing, the epidemic prevention materials are easy to damage and the like often occur.
The spunlace nonwoven fabric and the melt-blown nonwoven fabric are applied to the preparation of disposable masks, protective clothing, disinfection wet tissues and other epidemic prevention materials in a large number due to some specific functions, and play a great role in epidemic prevention and control. However, although the spunlace nonwoven fabric has the advantages of cleanness, air permeability, softness, skin friendliness, various processability and the like, and is widely applied to the fields of sanitary materials, wiping materials, medical supplies and the like, the spunlace nonwoven fabric serving as a protective material has insufficient water resistance and antibacterial property; although the melt-blown non-woven fabric has the advantages of high air permeability, high shielding, high particulate matter filtering efficiency and the like, the melt-blown non-woven fabric is widely applied to the fields of medical treatment and filtration. But the strength and tensile strength of the material are poor.
The present invention addresses these problems by preparing a medical high performance fiber composite.
Disclosure of Invention
The invention aims to provide a medical high-performance fiber composite material and a preparation method thereof, and aims to solve the problems in the prior art.
In order to solve the technical problems, the invention provides the following technical scheme:
a medical high-performance fiber composite material comprises an inner layer, a middle layer and an outer layer; the medical high-performance fiber composite material is prepared by unreeling an inner layer, a middle layer and an outer layer and then carrying out a photosynthetic atomization laminating process, wherein the outer layer is provided with a perylene-based conjugated microporous polymer, and the middle layer is provided with an N- (2-hydroxypropyl) methacrylamide compound; the photosynthetic atomization bonding process is characterized in that atomized 3, 6-dicarbonyl heptene is introduced under the illumination condition, and the composite material after unreeling and layering is bonded.
Further, the inner layer is a cellulose fiber spunlace; the middle layer is superfine high-adsorption function melt-blown cloth; the superfine melt-blown fabric with the high adsorption function is obtained by mixing and melt-blowing poly 3-amino-2-hydroxyl acrylic fiber and methacrylic trimethoxy titanium.
Further, the outer layer is a waterproof spunlace cloth layer; the waterproof spunlace fabric is obtained by mixing and spinning pretreated 1, 7-dinitro-6, 12-diacrylic acid perylene and 1,3, 5-tri (2, 3-diamino-4-bromophenyl) benzene and carrying out spunlace.
Further, the preparation method of the pretreated 1, 7-dinitro-6, 12-diacrylic acid perylene comprises the following steps: under the protection of nitrogen, 1, 7-dinitro-6, 12-diacrylic acid perylene, diboron pinacol ester, methoxyl (cyclooctadiene) iridium dimer, tert-butyl-2, 2' -bipyridine and anhydrous tetrahydrofuran are mixed according to a predetermined mass ratio, heated and stirred for reaction, and the pretreated 1, 7-dinitro-6, 12-diacrylic acid perylene is obtained.
Further, the preparation method of the medical high-performance fiber composite material comprises the following preparation steps:
(1) mixing the pretreated 1, 7-dinitro-6, 12-diacrylic acid perylene with 1,3, 5-tris (2, 3-diamino-4-bromophenyl) benzene to obtain a waterproof spunlace master batch; spinning, opening and mixing, carding, cross lapping, spunlacing and drying the waterproof spunlace master batch to prepare the waterproof spunlace cloth;
(2) preparing superfine high-adsorption-function melt-blown fabric: mixing and melt-blowing the poly 3-amino-2-hydroxyl acrylic fiber and the methacrylate trimethoxy titanium to prepare superfine melt-blown fabric with high adsorption function;
(3) unreeling and layering a cellulose fiber spunlace fabric serving as an inner layer, an ultrafine high-adsorption-function meltblown fabric serving as an intermediate layer and a waterproof spunlace fabric serving as an outer layer to prepare a composite material;
(4) and under the illumination condition, introducing atomized 3, 6-dicarbonyl heptene, and attaching the composite material to prepare the medical high-performance fiber composite material.
Further, the preparation method of the medical high-performance fiber composite material comprises the following preparation steps:
(1) under the protection of nitrogen, pre-treated 1, 7-dinitro-6, 12-diacrylic acid perylene, 1,3, 5-tris (2, 3-diamino-4-bromophenyl) benzene, tetrakis (triphenylphosphine) palladium, dimethylformamide and potassium carbonate solution are mixed according to the mass ratio of 1: 0.0009: 0.00001: 0.025: 0.005 to 1: 0.001: 0.00003: 0.035: 0.0055, stirring at 800-1000 r/min for 20-30 min, then performing freeze-thaw cycle for 2-4 times under the conditions that the freezing temperature is-15 to-13 ℃ and the dissolving temperature is 4-6 ℃, then continuously stirring for 46-50 h at 149-151 ℃, naturally cooling to room temperature, filtering, washing for 1-3 times with deionized water, methanol, chloroform and acetone in sequence, putting into a Soxhlet extraction device, adding pretreated 1, 7-dinitro-6, 12-diacrylic acid-based perylene in an amount of 7-7.2 times of anhydrous tetrahydrofuran, stirring for 70-74 h at 79-81 ℃ at the same stirring speed, and then performing vacuum drying for 22-26 h at 10-20 pa and 69-71 ℃ to obtain the waterproof spunlace master batch; putting the waterproof spunlace fabric master batch into a spinning box at the temperature of 150-160 ℃, spinning by using a screw extruder provided with a spinneret plate with the aperture of 0.5-1.5 mm under the conditions of the spinning speed of 600-800 m/min at the temperature of 230-260 ℃, and carrying out side-blowing, cooling and curing for 30-40 min under the conditions of the temperature of 14-20 ℃, the humidity of 25-30% and the wind speed of 0.8-1.5 m/s, and then carrying out opening, mixing, carding and cross lapping to obtain a waterproof spunlace fabric fiber web; then controlling the spunlace pressure to be 50-70 x 10 5 Pa, the density of the water needles is 14-18/cm, the diameter of the water needles is 80-120 mu m, net conveying spunlace is carried out at the net conveying speed of 0.3-0.5 m/min, and then vacuum drying is carried out for 2-3 h at the temperature of 30-50 ℃ under the condition of 10-20 Pa to prepare the waterproof spunlace fabric with the thickness of 0.3-0.5 mm;
(2) under the protection of helium, mixing poly 3-amino-2-hydroxy propylene fiber and dimethylformamide according to the mass ratio of 1: 6-1: 8, mixing, stirring for 20-30 min at 800-1000 r/min, putting into an oil bath kettle at 70-80 ℃, refluxing for 3-4 h at the same stirring speed, then dripping methacrylic trimethoxy titanium with the mass of 1.2-1.4 times of that of the poly 3-amino-2-hydroxy propylene fiber at 70-80 drops/min, continuously stirring for 3-4 h, naturally cooling to room temperature, filtering, vacuum drying for 5-6 h at 10-20 pa and 30-50 ℃, then washing for 1-3 times by using deionized water, methanol, chloroform and acetone sequentially, vacuum drying for 3-4 h at the same pressure and temperature, naturally cooling to room temperature, then putting into a melt-blowing device, adjusting the receiving distance to 38-42 cm, extruding frequency to 1.5-2.5 Hz, hot air temperature to 245-255 ℃ for melt-blowing, controlling the electret voltage to 38-42 kV and the electret distance to 2.5-3.5 cm for electret 0.8-1.2 min, preparing superfine high-adsorption-function melt-blown cloth with the thickness of 0.8-1.2 mm;
(3) unreeling and layering a cellulose fiber spunlace cloth with the thickness of 0.3-0.5 mm as an inner layer, an ultrafine high-adsorption function meltblown cloth as an intermediate layer and a waterproof spunlace cloth as an outer layer to prepare a composite material;
(4) placing the composite material in a closed space under the illumination condition of 550-650 lx, vacuumizing under the condition of 10-20 pa, introducing atomized 3, 6-dicarbonyl heptene at the speed of 0.10-0.15 m/s for 5-6 h, rolling for 2-3 times under the conditions of rolling speed of 123-260 m/min, roller spacing of 1.4-2.9 mm and pressure of 0.25-0.35 MPa, and vacuum drying at 10-20 pa and 30-40 ℃ for 2-3 h to prepare the medical high-performance fiber composite material.
Further, the preparation method of the pretreated 1, 7-dinitro-6, 12-diacrylic acid perylene in the step (1) comprises the following steps: under the protection of nitrogen, 1, 7-dinitro-6, 12-diacrylic acid perylene, diboron pinacol ester, methoxyl (cyclooctadiene) iridium dimer, tert-butyl-2, 2' -bipyridine and anhydrous tetrahydrofuran are mixed according to the mass ratio of 1: 4.4: 0.026: 0.021: 7-1: 4.5: 0.027: 0.022: 7.2, stirring at 800-1000 r/min for 20-30 min, heating to 79-81 ℃ at the speed of 1-3 ℃/min, continuing stirring for 14-18 h, naturally cooling to room temperature, filtering, washing with methanol for 3-5 times, placing into an oven at 30-40 ℃ for drying for 1-2 h, and naturally cooling to room temperature to obtain the pretreated 1, 7-dinitro-6, 12-diacrylic acid perylene.
Further, the mass fraction of the potassium carbonate solution in the step (1) is 18-22%.
Further, the rotating speed of a condensing screen roller of the melt-blowing device in the step (2) is 92-96 m/min, the aperture of a melt-blowing die head is 5-7 mu m, the temperature of the die head is 221-225 ℃, and the pressure of hot air is 0.21-0.23 MPa.
Further, the atomized 3, 6-dicarbonyl heptene in the step (4) is prepared by the following method: under the ultrasonic condition of 1.65 MHz-1.75 MHz, carrying out ultrasonic atomization on 3, 6-dicarbonyl heptene for 6-7 h, heating to 38-40 ℃ at the speed of 1-2 ℃/min for 1-2 h, and then preserving heat for later use to prepare atomized 3, 6-dicarbonyl heptene.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, the cellulose fiber spunlace fabric is used as an inner layer, the superfine high-adsorption function meltblown fabric is used as an intermediate layer, and the waterproof spunlace fabric is layered as an outer layer to obtain the composite material; then carrying out a photosynthetic atomization laminating process on the composite material by using 3, 6-dicarbonyl heptene to obtain a medical high-performance fiber composite material; wherein the superfine melt-blown fabric with high adsorption function is obtained by mixing and melt-blowing poly 3-amino-2-hydroxyl acrylic fiber and methacrylic trimethoxy titanium; the waterproof spunlace fabric is obtained by mixing, spinning and spunlacing 1, 7-dinitro-6, 12-diacrylic acid perylene and 1,3, 5-tri (2, 3-diamino-4-bromophenyl) benzene.
Firstly, 1, 7-dinitro-6, 12-diacrylic acid perylene and 1,3, 5-tri (2, 3-diamino-4-bromophenyl) benzene are mixed, spun and spunlaced to obtain waterproof spunlace cloth, and 2, 5, 8 and 11 sites of 1, 7-dinitro-6, 12-diacrylic acid pyrene have stronger activity and are substituted by 1,3, 5-tri (2, 3-diamino-4-bromophenyl) benzene to form perylene conjugated microporous polymer, so that the adsorption performance of the waterproof spunlace cloth is enhanced; carboxyl in the 1, 7-dinitro-6, 12-diacrylic acid perylene reacts with two adjacent amino groups in the 1,3, 5-tri (2, 3-diamino-4-bromophenyl) benzene to form a benzimidazole compound, so that the antibacterial performance of the waterproof spunlace fabric is enhanced.
Secondly, mixing and melt-blowing the poly 3-amino-2-hydroxyl acrylic fiber and the methacrylate group trimethoxy titanium to obtain superfine melt-blown cloth with high adsorption function, wherein carboxyl of the methacrylate group trimethoxy titanium reacts with amino on the poly 3-amino-2-hydroxyl acrylic fiber for crosslinking to generate an N- (2-hydroxypropyl) methacrylamide compound; methyl polymerization of the methacrylate trimethoxy titanium is removed under the action of hydroxyl of the poly 3-amino-2-hydroxyl acrylic fiber to form a titanium dioxide network, so that the tensile strength of the superfine high-adsorption function melt-blown fabric is increased; then, carrying out a photosynthetic atomization lamination process on the composite material by using 3, 6-dicarbonyl heptene to obtain a medical high-performance fiber composite material, wherein the perylene-based conjugated microporous polymer photocatalytically reduces nitro groups in the outer layer to form amino groups, and 3, 6-dicarbonyl heptene microdroplets are deposited on the outer layer to react with the amino groups and rapidly polymerize to form a convex micro-nano structure, so that the waterproofness of the medical high-performance fiber composite material is enhanced; the N- (2-hydroxypropyl) methacrylamide compound in the middle layer contacts with high-temperature 3, 6-dicarbonyl heptene microdroplets to be rapidly contracted, so that an olefin bond is exposed on the surface of the middle layer to be polymerized with the 3, 6-dicarbonyl heptene, amino on the surface of the outer layer reacts with two carbonyl groups in the 3, 6-dicarbonyl heptene to form a ring and is polymerized to form conductive polypyrrole, a perylene-based conjugated microporous polymer and a titanium dioxide network form a heterojunction, light energy is converted into electric energy to form micro-current, hydroxyl on the outer surface of the inner layer is oxidized to form carboxyl, the carboxyl reacts with N- (2-hydroxypropyl) methacrylamide to be crosslinked, the middle layer and the inner layer are firmly attached together, and the stripping resistance of the medical high-performance fiber composite material 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 describe the method in detail, and the method for testing each index of the medical high-performance fiber composite material prepared in the following examples is as follows:
and (3) antibacterial property: the medical high-performance fiber composite material prepared by the same mass example and the comparative example is tested for bacteriostasis rate according to the GB/T20944.3 standard method.
Water resistance: the medical high-performance fiber composite materials prepared by the same mass of the examples and the comparative examples are tested for water resistance according to a GB/T4745 standard method for testing a contact angle.
Peeling resistance: the medical high-performance fiber composite material prepared by the embodiment and the comparative example with the same length and width is tested for the peel strength according to the GB/T8808 standard method.
Tensile strength: the tensile strength of the medical high-performance fiber composite material prepared by taking the same length and width of the example and the comparative example is measured according to the GB/T2418.3 standard method.
Example 1
A preparation method of a medical high-performance fiber composite material comprises the following preparation steps:
(1) under the protection of nitrogen, 1, 7-dinitro-6, 12-diacrylic acid perylene, diboron pinacol ester, methoxyl (cyclooctadiene) iridium dimer, tert-butyl-2, 2' -bipyridine and anhydrous tetrahydrofuran are mixed according to the mass ratio of 1: 4.4: 0.026: 0.021: 7, mixing, stirring for 20min at the speed of 800r/min, heating to 79 ℃ at the speed of 1 ℃/min, continuously stirring for 14h, then naturally cooling to room temperature, cleaning for 3 times by using methanol after filtering, placing into a 30 ℃ oven to be dried for 1h, and naturally cooling to room temperature to obtain the pretreated 1, 7-dinitro-6, 12-diacrylic acid perylene; under the protection of nitrogen, pretreated 1, 7-dinitro-6, 12-diacrylic acid perylene, 1,3, 5-tris (2, 3-diamino-4-bromophenyl) benzene, tetrakis (triphenylphosphine) palladium, dimethylformamide and a potassium carbonate solution with the mass fraction of 18 percent are mixed according to the mass ratio of 1: 0.0009: 0.00001: 0.025: 0.005 mixing, stirring for 20min at 800r/min, then performing freeze-thaw cycle for 2 times at the freezing temperature of-15 ℃ and the dissolving temperature of 4 ℃, then continuing stirring for 46h at 149 ℃, naturally cooling to room temperature, filtering, washing for 1 time by sequentially using deionized water, methanol, chloroform and acetone, putting into a Soxhlet extraction device, adding anhydrous tetrahydrofuran which is 7 times of the mass of the pretreated 1, 7-dinitro-6, 12-diacrylic acid perylene, stirring for 70h at the same stirring speed at 79 ℃, and then performing vacuum drying for 22h at 10pa and 69 ℃ to obtain the waterproof spunlace master batch; putting the waterproof spunlace fabric master batch into a spinning box at 150 ℃, spinning by using a screw extruder provided with a spinneret plate with the aperture of 0.5mm under the conditions of 230 ℃ and the spinning speed of 600m/min, cooling and curing for 30min by side air blowing under the conditions of 14 ℃, the humidity of 25 percent and the air speed of 0.8m/s, and then opening, mixing, carding and cross lapping to obtain a waterproof spunlace fabric web; then controlling the water jet pressure to 50 x 10 5 Pa, the density of the water needle is 14/cm, the diameter of the water needle is 80 mu m, andcarrying out net conveying spunlace at a net conveying speed of 0.3m/min, and then carrying out vacuum drying at 10pa and 30 ℃ for 2h to prepare waterproof spunlace cloth with the thickness of 0.3 mm;
(2) under the protection of helium, mixing poly 3-amino-2-hydroxy propylene fiber and dimethylformamide according to the mass ratio of 1: 6 mixing, stirring at 800r/min for 20min, placing in a 70 ℃ oil bath, refluxing at the same stirring speed for 3h, then dripping 1.2 times of methacrylic trimethoxy titanium with the mass of the 3-amino-2-hydroxy propylene fiber at 70 drops/min, continuing stirring for 3h, naturally cooling to room temperature, filtering, vacuum drying at 10pa and 30 ℃ for 5h, washing with deionized water, methanol, chloroform and acetone for 1 time, vacuum drying at the same pressure and temperature for 3h, naturally cooling to room temperature, placing in a melt-blowing device with a condensing net roller rotating speed of 92m/min, a melt-blowing die head aperture of 5 μm, a die head temperature of 221 ℃ and a hot air pressure of 0.21MPa, adjusting the receiving distance to 38cm, the extrusion frequency to 1.5Hz, the hot air temperature to 245 ℃ for melt-blowing, and controlling the electret voltage to 38kV, Performing electret for 0.8min at an electret distance of 2.5cm to obtain superfine melt-blown cloth with high adsorption function and thickness of 0.8 mm;
(3) unreeling and layering a cellulose fiber spunlace cloth with the thickness of 0.3mm as an inner layer, an ultrafine high-adsorption function meltblown cloth as an intermediate layer and a waterproof spunlace cloth as an outer layer to prepare a composite material;
(4) ultrasonically atomizing 3, 6-dicarbonyl heptene for 6h under the ultrasonic condition of 1.65MHz, heating to 38 ℃ at the speed of 1 ℃/min, keeping the temperature for later use, and preparing atomized 3, 6-dicarbonyl heptene; placing the composite material in a closed space under 550lx illumination, vacuumizing under 10pa, introducing atomized 3, 6-dicarbonyl heptylene for 5h at the speed of 0.10 m/s, rolling for 2 times under the conditions of the rolling speed of 123m/min, the roller spacing of 1.4mm and the pressure of 0.25MPa, and vacuum-drying for 2h at 10pa and 30 ℃ to prepare the medical high-performance fiber composite material.
Example 2
A preparation method of a medical high-performance fiber composite material comprises the following preparation steps:
(1) under the protection of nitrogen, 1, 7-dinitro6, 12-diacrylate perylene, diboronic acid pinacol ester, methoxyl (cyclooctadiene) iridium dimer, tert-butyl-2, 2' -bipyridine and anhydrous tetrahydrofuran in a mass ratio of 1: 4.45: 0.0265: 0.0215: 7.1, stirring at 900r/min for 25min, heating to 80 ℃ at 2 ℃/min, continuing stirring for 16h, then naturally cooling to room temperature, filtering, washing with methanol for 4 times, placing in a 35 ℃ oven for drying for 1.5h, and naturally cooling to room temperature to obtain the pretreated 1, 7-dinitro-6, 12-diacrylic perylene; under the protection of nitrogen, pretreated 1, 7-dinitro-6, 12-diacrylic acid perylene, 1,3, 5-tris (2, 3-diamino-4-bromophenyl) benzene, tetrakis (triphenylphosphine) palladium, dimethylformamide and 20 mass percent potassium carbonate solution are mixed according to the mass ratio of 1: 0.00095: 0.00002: 0.03: 0.00525, stirring at 900r/min for 25min, freezing and thawing at-14 deg.C and 5 deg.C for 3 times, further stirring at 150 deg.C for 48h, naturally cooling to room temperature, filtering, sequentially washing with deionized water, methanol, chloroform and acetone for 2 times, placing into a Soxhlet extraction device, adding pretreated 1, 7-dinitro-6, 12-diacrylic acid perylene (7.1 times of anhydrous tetrahydrofuran), stirring at 80 deg.C for 72h, and vacuum drying at 15pa and 70 deg.C for 24h to obtain waterproof spunlace masterbatch; putting the waterproof spunlace fabric master batch into a spinning box at 155 ℃, spinning by using a screw extruder with a spinneret plate with the aperture of 1mm under the conditions of 245 ℃ and 700m/min spinning speed, cooling and curing for 35min by side air blowing under the conditions of 17 ℃, 27.5% of humidity and 1.15m/s of wind speed, and then opening, mixing, carding and cross lapping to obtain a waterproof spunlace fabric web; and then controlling the spunlace pressure to 60 x 10 5 Pa, the density of the water needles is 16/cm, the diameter of the water needles is 100 mu m, net conveying and spunlacing are carried out at the net conveying speed of 0.4m/min, and then vacuum drying is carried out for 2.5 hours at the temperature of 40 ℃ at 15Pa to prepare waterproof spunlace cloth with the thickness of 0.4 mm;
(2) under the protection of helium, mixing poly 3-amino-2-hydroxy propylene fiber and dimethylformamide according to the mass ratio of 1: 7 mixing, stirring for 25min at 900r/min, placing in a 75 ℃ oil bath, refluxing for 3.5h at the same stirring speed, then dripping methacrylic trimethoxy titanium with 1.3 times of the mass of the poly 3-amino-2-hydroxy propylene fiber at 75 drops/min, continuing stirring for 3.5h, naturally cooling to room temperature, filtering, vacuum drying for 5.5h at 15pa and 40 ℃, then washing for 2 times with deionized water, methanol, chloroform and acetone in sequence, vacuum drying for 3.5h at the same pressure and temperature, naturally cooling to room temperature, then placing in a melt-blowing device with a condensing net roller rotating speed of 94m/min, a melt-blowing die head aperture of 6 μm, a die head temperature of 223 ℃ and a hot air pressure of 0.22MPa, adjusting the receiving distance to 40cm, an extrusion frequency to 2Hz, a hot air temperature to 250 ℃ for melt-blowing, and controlling the standing voltage of 40kV, the static voltage of 40kV, Performing electret for 1min at an electret distance of 3cm to prepare superfine melt-blown fabric with high adsorption function and thickness of 1 mm;
(3) unreeling and layering a cellulose fiber spunlace cloth with the thickness of 0.4mm as an inner layer, an ultrafine high-adsorption function meltblown cloth as an intermediate layer and a waterproof spunlace cloth as an outer layer to prepare a composite material;
(4) ultrasonically atomizing 3, 6-dicarbonyl heptene for 6.5h under the ultrasonic condition of 1.7MHz, heating to 39 ℃ at the speed of 1.5 ℃/min for 1.5h, and preserving heat for later use to prepare atomized 3, 6-dicarbonyl heptene; placing the composite material in a closed space under the condition of 600lx illumination, vacuumizing under the condition of 15pa, introducing atomized 3, 6-dicarbonyl heptylene for 5.5h at the speed of 0.125 m/s, rolling for 2 times under the conditions of 191m/min rolling speed, 2.15mm roll spacing and 0.3Mpa pressure, and vacuum drying for 2.5h at the temperature of 15pa and 35 ℃ to prepare the medical high-performance fiber composite material.
Example 3
A preparation method of a medical high-performance fiber composite material comprises the following preparation steps:
(1) under the protection of nitrogen, 1, 7-dinitro-6, 12-diacrylic acid perylene, diboron pinacol ester, methoxyl (cyclooctadiene) iridium dimer, tert-butyl-2, 2' -bipyridine and anhydrous tetrahydrofuran are mixed according to the mass ratio of 1: 4.5: 0.027: 0.022: 7.2 mixing, stirring at 1000r/min for 30min, heating to 81 ℃ at 3 ℃/min, continuing stirring for 18h, then naturally cooling to room temperature, filtering, washing with methanol for 5 times, placing into a 40 ℃ oven to bake for 2h, naturally cooling to room temperature to obtain the pretreated 1, 7-dinitro-6, 12-diacrylic acid radicalA perylene; under the protection of nitrogen, pretreated 1, 7-dinitro-6, 12-diacrylic acid perylene, 1,3, 5-tris (2, 3-diamino-4-bromophenyl) benzene, tetrakis (triphenylphosphine) palladium, dimethylformamide and a potassium carbonate solution with the mass fraction of 22 percent are mixed according to the mass ratio of 1: 0.001: 0.00003: 0.035: 0.0055, stirring at 1000r/min for 30min, then freezing and thawing at-13 ℃ and 6 ℃ for 4 times, then continuously stirring at 151 ℃ for 50h, naturally cooling to room temperature, filtering, sequentially washing with deionized water, methanol, chloroform and acetone for 3 times, placing into a Soxhlet extraction device, adding anhydrous tetrahydrofuran (7.2 times the mass of the pretreated 1, 7-dinitro-6, 12-diacrylic acid perylene), stirring at 81 ℃ for 74h at the same stirring speed, and then vacuum drying at 20pa and 71 ℃ for 26h to obtain the waterproof spunlace masterbatch; putting the waterproof spunlace fabric master batch into a spinning box at 160 ℃, spinning by using a screw extruder provided with a spinneret plate with the aperture of 1.5mm under the conditions of 260 ℃ and 800m/min of spinning speed, cooling and curing for 40min by side air blowing under the conditions of 20 ℃, 30% of humidity and 1.5m/s of wind speed, and then opening, mixing, carding and cross lapping to obtain a waterproof spunlace fabric web; then controlling the water jet pressure to 70 x 10 5 Pa, the density of the water needles is 18/cm, the diameter of the water needles is 120 mu m, net conveying and spunlacing are carried out at the net conveying speed of 0.5m/min, and then vacuum drying is carried out for 3 hours at the temperature of 50 ℃ at 20Pa to prepare waterproof spunlace cloth with the thickness of 0.5 mm;
(2) under the protection of helium, mixing poly 3-amino-2-hydroxy propylene fiber and dimethylformamide according to the mass ratio of 1: 8, stirring the mixture for 30min at 1000r/min, putting the mixture into an oil bath kettle at 80 ℃, refluxing the mixture for 4h at the same stirring speed, then dripping methacrylic trimethoxy titanium with the mass 1.4 times that of the poly 3-amino-2-hydroxyl propylene fiber into the mixture at 80 drops/min, continuously stirring the mixture for 4h, naturally cooling the mixture to room temperature, filtering the mixture, drying the mixture in vacuum for 6h at 20pa and 50 ℃, washing the dried mixture for 3 times by using deionized water, methanol, chloroform and acetone in sequence, drying the mixture in vacuum for 4h at the same pressure and temperature, naturally cooling the mixture to room temperature, putting the mixture into a melt-blowing device with a condensing net roller, the rotating speed of the condensing net roller being 96m/min, the aperture of a melt-blowing die head being 7 mu m, the temperature of the die head being 225 ℃ and the hot air pressure being 0.23MPa, adjusting the receiving distance to 42cm, the extrusion frequency to 2.5Hz, the hot air temperature to 255 ℃ for melt-blowing, and controlling the electret voltage to be 42kV, Performing electret for 1.2min at an electret distance of 3.5cm to obtain superfine melt-blown cloth with high adsorption function and thickness of 1.2 mm;
(3) unreeling and layering a cellulose fiber spunlace cloth with the thickness of 0.5mm as an inner layer, an ultrafine high-adsorption function meltblown cloth as an intermediate layer and a waterproof spunlace cloth as an outer layer to prepare a composite material;
(4) ultrasonically atomizing 3, 6-dicarbonyl heptene for 7h under the ultrasonic condition of 1.75MHz, heating to 40 ℃ at the speed of 2 ℃/min, keeping the temperature for later use, and preparing atomized 3, 6-dicarbonyl heptene; placing the composite material in a closed space under 650lx illumination, vacuumizing under 20pa, introducing atomized 3, 6-dicarbonyl heptylene for 6h at the speed of 0.15 m/s, rolling for 3 times under the conditions of the rolling speed of 260m/min, the roller spacing of 2.9mm and the pressure of 0.35Mpa, and vacuum-drying for 3h at 20pa and 40 ℃ to prepare the medical high-performance fiber composite material.
Comparative example 1
The preparation method of the medical high-performance fiber composite material in the comparative example 1 is different from that of the example 2 only in the difference of the step (1), and the step (1) is modified as follows: under the protection of nitrogen, 1, 7-dinitro-6, 12-diacrylic acid perylene and titanium tetrachloride-triethyl aluminum are mixed according to the mass ratio of 1: 0.0215, stirring at 900r/min for 25min, heating to 80 ℃ at 2 ℃/min, continuing stirring for 16h, naturally cooling to room temperature, filtering, washing with methanol for 4 times, placing into a 35 ℃ oven, drying for 1.5h, and naturally cooling to room temperature to obtain the waterproof spunlace fabric master batch; putting the waterproof spunlace fabric master batch into a spinning box at 155 ℃, spinning by using a screw extruder with a spinneret plate with the aperture of 1mm under the conditions of 245 ℃ and 700m/min spinning speed, cooling and curing for 35min by side air blowing under the conditions of 17 ℃, 27.5% of humidity and 1.15m/s of wind speed, and then opening, mixing, carding and cross lapping to obtain a waterproof spunlace fabric web; then controlling the water jet pressure to be 60 x 10 5 Pa, the density of the water needles is 16/cm, the diameter of the water needles is 100 mu m, net conveying and spunlacing are carried out at the net conveying speed of 0.4m/min, and then vacuum drying is carried out for 2.5h at the temperature of 40 ℃ at 15Pa to prepare the waterproof spunlace cloth with the thickness of 0.4 mm. The rest of the preparation steps are the same as example 2.
Comparative example 2
Comparative example 2 the preparation method of the high-performance fiber composite for chinese medical use is different from that of example 2 only in the difference of step (2), and the step (2) is modified as follows: under the protection of helium, the poly 3-amino-2-hydroxyl propylene fiber is dried under vacuum at 15pa and 40 ℃ for 5.5h, washed by deionized water and acetone for 2 times in sequence, dried under the same pressure and temperature for 3.5h, naturally cooled to room temperature, then placed into a melt-blowing device with a condensing net roller rotating speed of 94m/min, a melt-blowing die head aperture of 6 mu m, a die head temperature of 223 ℃ and a hot air pressure of 0.22MPa, the receiving distance is adjusted to 40cm, the extrusion frequency is adjusted to 2Hz, the hot air temperature is adjusted to 250 ℃ for melt-blowing, the electret voltage is controlled to 40kV, the electret distance is controlled to 3cm for 1min, and the superfine high-adsorption function melt-blown fabric with the thickness of 1mm is prepared. The rest of the preparation steps are the same as example 2.
Comparative example 3
The preparation method of the medical high-performance fiber composite material in the comparative example 3 is different from that of the example 2 only in the difference of the step (4), and the step (4) is modified as follows: ultrasonically atomizing heptene for 6.5h under the ultrasonic condition of 1.7MHz, heating to 39 ℃ at the speed of 1.5 ℃/min for 1.5h, and preserving heat for later use to prepare atomized heptene; placing the composite material in a closed space under the condition of 600lx illumination, vacuumizing under the condition of 15pa, introducing atomized heptene at the speed of 0.125 m/s for 5.5h, rolling for 2 times under the conditions of 191m/min rolling speed, 2.15mm roll spacing and 0.3MPa pressure, and vacuum-drying at 15pa and 35 ℃ for 2.5h to prepare the medical high-performance fiber composite material. The rest of the preparation steps are the same as example 2.
Comparative example 4
The preparation method of the medical high-performance fiber composite material in the comparative example 4 is different from that of the example 2 only in the difference of the step (4), and the step (4) is modified as follows: ultrasonically atomizing 3, 6-dicarbonyl heptene for 6.5h under the ultrasonic condition of 1.7MHz, heating to 39 ℃ at the speed of 1.5 ℃/min for 1.5h, and preserving heat for later use to prepare atomized 3, 6-dicarbonyl heptene; putting the composite material into a closed space, vacuumizing under the condition of 15pa, introducing atomized 3, 6-dicarbonyl heptylene for 5.5h at the speed of 0.125 m/s, rolling for 2 times under the conditions of 191m/min rolling speed, 2.15mm roll spacing and 0.3Mpa pressure, and vacuum-drying for 2.5h at the temperature of 15pa and 35 ℃ to prepare the medical high-performance fiber composite material. The rest of the preparation steps are the same as example 2.
Examples of effects
Table 1 below shows the analysis results of the antibacterial property, the waterproof property, the peeling resistance and the tensile strength of the medical high performance fiber composite material prepared by examples 1 to 3 of the present invention and comparative examples 1 to 4.
TABLE 1
| [0001] | [0002]Peel strength/(N/m) | [0003]Bacteriostatic ratio (%) | [0004]Contact angle (°) | [0005]Tensile Strength/(MPa) |
| [0006]Example 1 | [0007] 20.88 | [0008] 99.86 | [0009] 116.5 | [0010] 1.5 |
| [0011]Example 2 | [0012] 20.89 | [0013] 99.89 | [0014] 116.9 | [0015] 1.6 |
| [0016]Example 3 | [0017] 20.87 | [0018] 99.87 | [0019] 116.8 | [0020] 1.4 |
| [0021]Comparative example 1 | [0022] 7.86 | [0023] 80.2 | [0024] 116.6 | [0025] 1.5 |
| [0026]Comparative example 2 | [0027] 17.88 | [0028] 99.84 | [0029] 116.3 | [0030] 0.9 |
| [0031]Comparative example 3 | [0032] 20.86 | [0033] 99.32 | [0034] 52.3 | [0035] 1.6 |
| [0036]Comparative example 4 | [0037] 10.26 | [0038] 99.97 | [0039] 86.3 | [0040] 1.3 |
From table 1, it can be seen that the medical high-performance fiber composite materials prepared in examples 1, 2 and 3 have good antibacterial property, water resistance, peeling resistance and tensile strength; from the comparison of the experimental data of the examples 1, 2 and 3 and the comparative example 1, it can be found that the waterproof spunlace fabric prepared by only using 1, 7-dinitro-6, 12-diacrylic acid-based perylene cannot form perylene-based conjugated microporous polymer and benzimidazole compound, and after the subsequent layering, the composite material is subjected to the photosynthetic atomization attaching process by using 3, 6-dicarbonyl heptene, and a heterojunction cannot be formed with a titanium dioxide network, so that the stripping resistance and the antibacterial property of the medical high-performance fiber composite material are weak; from the experimental data of examples 1, 2,3 and comparative example 2, it can be found that, when only poly 3-amino-2-hydroxy propylene fiber is used to prepare superfine high-adsorption function melt-blown fabric, N- (2-hydroxypropyl) methacrylamide compound and titanium dioxide network cannot be formed, and after subsequent layering, the composite material is subjected to a photosynthetic atomization laminating process by using 3, 6-dicarbonyl heptene, heterojunction with the titanium dioxide network cannot be formed, so that the medical high-performance fiber composite material has low tensile strength and weak peeling resistance; experimental data of examples 1, 2 and 3 and comparative examples 3 and 4 show that a convex micro-nano structure cannot be formed by carrying out a photosynthetic atomization bonding process on the composite material by utilizing heptene, and the prepared medical high-performance fiber composite material is weak in water resistance; under the non-illumination condition, the composite material is subjected to an atomization and lamination process by using 3, 6-dicarbonyl heptylene, a convex micro-nano structure and micro-current cannot be formed, and the prepared medical high-performance fiber composite material is weak in water resistance and peeling resistance.
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 medical high-performance fiber composite material is characterized by comprising an inner layer, a middle layer and an outer layer; the medical high-performance fiber composite material is prepared by unreeling an inner layer, a middle layer and an outer layer and then carrying out a photosynthetic atomization laminating process, wherein the outer layer is provided with a perylene-based conjugated microporous polymer, and the middle layer is provided with an N- (2-hydroxypropyl) methacrylamide compound; the photosynthetic atomization bonding process comprises the steps of introducing atomized 3, 6-dicarbonyl heptene under the illumination condition, and bonding the composite material after unreeling and layering.
2. The medical high-performance fiber composite material as claimed in claim 1, wherein the inner layer is a cellulose fiber spunlace; the middle layer is superfine high-adsorption function melt-blown cloth; the superfine melt-blown fabric with the high adsorption function is obtained by mixing and melt-blowing poly 3-amino-2-hydroxyl acrylic fiber and methacrylic trimethoxy titanium.
3. The medical high-performance fiber composite material as claimed in claim 1, wherein the outer layer is a waterproof spunlace cloth layer; the waterproof spunlace fabric is obtained by mixing and spinning pretreated 1, 7-dinitro-6, 12-diacrylic acid perylene and 1,3, 5-tri (2, 3-diamino-4-bromophenyl) benzene and carrying out spunlace.
4. The medical high-performance fiber composite material as claimed in claim 3, wherein the preparation method of the pretreated 1, 7-dinitro-6, 12-diacrylic acid perylene is as follows: under the protection of nitrogen, 1, 7-dinitro-6, 12-diacrylic acid perylene, diboron pinacol ester, methoxyl (cyclooctadiene) iridium dimer, tert-butyl-2, 2' -bipyridine and anhydrous tetrahydrofuran are mixed according to a predetermined mass ratio, heated and stirred for reaction, and the pretreated 1, 7-dinitro-6, 12-diacrylic acid perylene is obtained.
5. The preparation method of the medical high-performance fiber composite material is characterized by comprising the following preparation steps:
(1) mixing the pretreated 1, 7-dinitro-6, 12-diacrylic acid perylene with 1,3, 5-tris (2, 3-diamino-4-bromophenyl) benzene to obtain a waterproof spunlace master batch; spinning, opening and mixing, carding, cross lapping, spunlacing and drying the waterproof spunlace master batch to prepare the waterproof spunlace cloth;
(2) preparing superfine high-adsorption-function melt-blown fabric: mixing and melt-blowing the poly 3-amino-2-hydroxyl acrylic fiber and the methacrylate trimethoxy titanium to prepare superfine melt-blown fabric with high adsorption function;
(3) unreeling and layering a cellulose fiber spunlace fabric serving as an inner layer, an ultrafine high-adsorption-function meltblown fabric serving as an intermediate layer and a waterproof spunlace fabric serving as an outer layer to prepare a composite material;
(4) and under the illumination condition, introducing atomized 3, 6-dicarbonyl heptene, and attaching the composite material to prepare the medical high-performance fiber composite material.
6. The preparation method of the medical high-performance fiber composite material according to claim 5, wherein the preparation method of the medical high-performance fiber composite material comprises the following preparation steps:
(1) under the protection of nitrogen, pre-treated 1, 7-dinitro-6, 12-diacrylic acid perylene, 1,3, 5-tris (2, 3-diamino-4-bromophenyl) benzene, tetrakis (triphenylphosphine) palladium, dimethylformamide and potassium carbonate solution are mixed according to the mass ratio of 1: 0.0009: 0.00001: 0.025: 0.005-1: 0.001: 0.00003: 0.035: 0.0055, stirring at 800-1000 r/min for 20-30 min, then performing freeze-thaw cycle for 2-4 times under the conditions that the freezing temperature is-15 to-13 ℃ and the dissolving temperature is 4-6 ℃, then continuously stirring for 46-50 h at 149-151 ℃, naturally cooling to room temperature, filtering, washing for 1-3 times by using deionized water, methanol, chloroform and acetone in sequence, putting into a Soxhlet extraction device, and adding pretreated 1, 7-dinitro-6, 12-diacrylic acid-based perylene of which the mass is 7-7.2 times that of anhydrous tetrahydro-peryleneStirring furan at 79-81 ℃ for 70-74 h at the same stirring speed, and then performing vacuum drying at 10-20 pa and 69-71 ℃ for 22-26 h to obtain waterproof spunlace fabric master batches; putting the waterproof spunlace fabric master batch into a spinning box at the temperature of 150-160 ℃, spinning by using a screw extruder provided with a spinneret plate with the aperture of 0.5-1.5 mm under the conditions of the spinning speed of 600-800 m/min at the temperature of 230-260 ℃, and carrying out side-blowing, cooling and curing for 30-40 min under the conditions of the temperature of 14-20 ℃, the humidity of 25-30% and the wind speed of 0.8-1.5 m/s, and then carrying out opening, mixing, carding and cross lapping to obtain a waterproof spunlace fabric fiber web; then controlling the spunlace pressure to be 50-70 x 10 5 Pa, the density of the water needles is 14-18/cm, the diameter of the water needles is 80-120 mu m, net conveying spunlace is carried out at the net conveying speed of 0.3-0.5 m/min, and then vacuum drying is carried out for 2-3 h at the temperature of 30-50 ℃ under the condition of 10-20 Pa to prepare the waterproof spunlace fabric with the thickness of 0.3-0.5 mm;
(2) under the protection of helium, mixing poly 3-amino-2-hydroxy propylene fiber and dimethylformamide according to the mass ratio of 1: 6-1: 8, mixing, stirring for 20-30 min at 800-1000 r/min, putting into an oil bath kettle at 70-80 ℃, refluxing for 3-4 h at the same stirring speed, then dripping methacrylic trimethoxy titanium with the mass of 1.2-1.4 times of that of the poly 3-amino-2-hydroxy propylene fiber at 70-80 drops/min, continuously stirring for 3-4 h, naturally cooling to room temperature, filtering, vacuum drying for 5-6 h at 10-20 pa and 30-50 ℃, then washing for 1-3 times by using deionized water, methanol, chloroform and acetone sequentially, vacuum drying for 3-4 h at the same pressure and temperature, naturally cooling to room temperature, then putting into a melt-blowing device, adjusting the receiving distance to 38-42 cm, extruding frequency to 1.5-2.5 Hz, hot air temperature to 245-255 ℃ for melt-blowing, controlling the electret voltage to 38-42 kV and the electret distance to 2.5-3.5 cm for electret 0.8-1.2 min, preparing superfine high-adsorption-function melt-blown cloth with the thickness of 0.8-1.2 mm;
(3) unreeling and layering a cellulose fiber spunlace cloth with the thickness of 0.3-0.5 mm as an inner layer, an ultrafine high-adsorption function meltblown cloth as an intermediate layer and a waterproof spunlace cloth as an outer layer to prepare a composite material;
(4) placing the composite material in a closed space under the illumination condition of 550-650 lx, vacuumizing under the condition of 10-20 pa, introducing atomized 3, 6-dicarbonyl heptene at the speed of 0.10-0.15 m/s for 5-6 h, rolling for 2-3 times under the conditions of rolling speed of 123-260 m/min, roller spacing of 1.4-2.9 mm and pressure of 0.25-0.35 MPa, and vacuum drying at 10-20 pa and 30-40 ℃ for 2-3 h to prepare the medical high-performance fiber composite material.
7. The preparation method of the medical high-performance fiber composite material as claimed in claim 6, wherein the preparation method of the pretreated 1, 7-dinitro-6, 12-diacrylic acid-based perylene in the step (1) is as follows: under the protection of nitrogen, 1, 7-dinitro-6, 12-diacrylic acid perylene, diboron pinacol ester, methoxyl (cyclooctadiene) iridium dimer, tert-butyl-2, 2' -bipyridine and anhydrous tetrahydrofuran are mixed according to the mass ratio of 1: 4.4: 0.026: 0.021: 7-1: 4.5: 0.027: 0.022: 7.2, stirring at 800-1000 r/min for 20-30 min, heating to 79-81 ℃ at the speed of 1-3 ℃/min, continuing stirring for 14-18 h, naturally cooling to room temperature, filtering, washing with methanol for 3-5 times, placing into an oven at 30-40 ℃ for drying for 1-2 h, and naturally cooling to room temperature to obtain the pretreated 1, 7-dinitro-6, 12-diacrylic acid perylene.
8. The preparation method of the medical high-performance fiber composite material according to claim 7, wherein the mass fraction of the potassium carbonate solution in the step (1) is 18-22%.
9. The preparation method of the medical high-performance fiber composite material as claimed in claim 8, wherein the rotation speed of a condensing screen roller of the melt-blowing device in the step (2) is 92-96 m/min, the aperture of a melt-blowing die head is 5-7 μm, the temperature of the die head is 221-225 ℃, and the pressure of hot air is 0.21-0.23 MPa.
10. The method for preparing the medical high-performance fiber composite material as claimed in claim 9, wherein the atomized 3, 6-dicarbonyl heptene in the step (4) is prepared by the following steps: under the ultrasonic condition of 1.65 MHz-1.75 MHz, carrying out ultrasonic atomization on 3, 6-dicarbonyl heptene for 6-7 h, heating to 38-40 ℃ at the speed of 1-2 ℃/min for 1-2 h, and then preserving heat for later use to prepare atomized 3, 6-dicarbonyl heptene.
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