CN114921950A - 一种轻质吸波面料及其制备方法 - Google Patents
一种轻质吸波面料及其制备方法 Download PDFInfo
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- CN114921950A CN114921950A CN202210624918.8A CN202210624918A CN114921950A CN 114921950 A CN114921950 A CN 114921950A CN 202210624918 A CN202210624918 A CN 202210624918A CN 114921950 A CN114921950 A CN 114921950A
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- 239000004744 fabric Substances 0.000 title claims abstract description 100
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 238000004519 manufacturing process Methods 0.000 title description 2
- 229920000742 Cotton Polymers 0.000 claims abstract description 131
- 239000002243 precursor Substances 0.000 claims abstract description 45
- 238000010438 heat treatment Methods 0.000 claims abstract description 44
- 239000000835 fiber Substances 0.000 claims abstract description 40
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims abstract description 37
- 239000004964 aerogel Substances 0.000 claims abstract description 30
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 11
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 11
- KYCGURZGBKFEQB-UHFFFAOYSA-N n',n'-dibutylpropane-1,3-diamine Chemical compound CCCCN(CCCC)CCCN KYCGURZGBKFEQB-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910052581 Si3N4 Inorganic materials 0.000 claims abstract description 5
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims abstract description 5
- 230000008021 deposition Effects 0.000 claims abstract description 4
- 238000009489 vacuum treatment Methods 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 56
- 239000000243 solution Substances 0.000 claims description 55
- 238000003756 stirring Methods 0.000 claims description 45
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 42
- 238000009987 spinning Methods 0.000 claims description 38
- 239000008367 deionised water Substances 0.000 claims description 36
- 229910021641 deionized water Inorganic materials 0.000 claims description 36
- 238000005406 washing Methods 0.000 claims description 33
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 32
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 30
- 239000002121 nanofiber Substances 0.000 claims description 30
- 238000002156 mixing Methods 0.000 claims description 29
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 25
- 238000001816 cooling Methods 0.000 claims description 24
- 239000002262 Schiff base Substances 0.000 claims description 22
- 238000001035 drying Methods 0.000 claims description 21
- 239000000758 substrate Substances 0.000 claims description 21
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 20
- 150000004753 Schiff bases Chemical class 0.000 claims description 20
- 239000012153 distilled water Substances 0.000 claims description 20
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 238000007710 freezing Methods 0.000 claims description 17
- 230000008014 freezing Effects 0.000 claims description 17
- 239000001257 hydrogen Substances 0.000 claims description 17
- 229910052739 hydrogen Inorganic materials 0.000 claims description 17
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 claims description 17
- 239000002211 L-ascorbic acid Substances 0.000 claims description 16
- 235000000069 L-ascorbic acid Nutrition 0.000 claims description 16
- 229960005070 ascorbic acid Drugs 0.000 claims description 16
- 239000010410 layer Substances 0.000 claims description 15
- 125000000717 hydrazino group Chemical group [H]N([*])N([H])[H] 0.000 claims description 14
- 229910052757 nitrogen Inorganic materials 0.000 claims description 14
- QYKABQMBXCBINA-UHFFFAOYSA-N 4-(oxan-2-yloxy)benzaldehyde Chemical compound C1=CC(C=O)=CC=C1OC1OCCCC1 QYKABQMBXCBINA-UHFFFAOYSA-N 0.000 claims description 12
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 12
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- 239000012792 core layer Substances 0.000 claims description 12
- 238000002791 soaking Methods 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 11
- DOZLVLCBCZGSSH-RQOWECAXSA-N (z)-2-bromobut-2-enal Chemical compound C\C=C(/Br)C=O DOZLVLCBCZGSSH-RQOWECAXSA-N 0.000 claims description 10
- ZKODPGZNBMIZFX-UHFFFAOYSA-N 2-(2-bromoethyl)oxirane Chemical compound BrCCC1CO1 ZKODPGZNBMIZFX-UHFFFAOYSA-N 0.000 claims description 10
- 229910052786 argon Inorganic materials 0.000 claims description 10
- YTLYLLTVENPWFT-UPHRSURJSA-N (Z)-3-aminoacrylic acid Chemical compound N\C=C/C(O)=O YTLYLLTVENPWFT-UPHRSURJSA-N 0.000 claims description 9
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 9
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 9
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims description 9
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims description 9
- 238000000151 deposition Methods 0.000 claims description 9
- 238000009941 weaving Methods 0.000 claims description 9
- 229920002678 cellulose Polymers 0.000 claims description 7
- 239000001913 cellulose Substances 0.000 claims description 7
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 7
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 7
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 7
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 6
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 6
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 6
- 239000005457 ice water Substances 0.000 claims description 6
- 239000003208 petroleum Substances 0.000 claims description 6
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 5
- 230000032683 aging Effects 0.000 claims description 5
- 239000002585 base Substances 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 4
- 238000009835 boiling Methods 0.000 claims description 2
- 238000007598 dipping method Methods 0.000 claims description 2
- 238000004108 freeze drying Methods 0.000 claims description 2
- 229940044631 ferric chloride hexahydrate Drugs 0.000 claims 3
- 230000000694 effects Effects 0.000 abstract description 12
- 230000005855 radiation Effects 0.000 abstract description 7
- 230000000844 anti-bacterial effect Effects 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 4
- QDHUQRBYCVAWEN-UHFFFAOYSA-N amino prop-2-enoate Chemical compound NOC(=O)C=C QDHUQRBYCVAWEN-UHFFFAOYSA-N 0.000 abstract description 3
- 239000002070 nanowire Substances 0.000 abstract description 3
- 229910021578 Iron(III) chloride Inorganic materials 0.000 abstract description 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 abstract description 2
- 230000002265 prevention Effects 0.000 abstract description 2
- 230000002238 attenuated effect Effects 0.000 abstract 1
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 abstract 1
- 229910052794 bromium Inorganic materials 0.000 abstract 1
- MLUCVPSAIODCQM-NSCUHMNNSA-N crotonaldehyde Chemical compound C\C=C\C=O MLUCVPSAIODCQM-NSCUHMNNSA-N 0.000 abstract 1
- MLUCVPSAIODCQM-UHFFFAOYSA-N crotonaldehyde Natural products CC=CC=O MLUCVPSAIODCQM-UHFFFAOYSA-N 0.000 abstract 1
- 238000012986 modification Methods 0.000 abstract 1
- 230000004048 modification Effects 0.000 abstract 1
- 230000000149 penetrating effect Effects 0.000 abstract 1
- 230000001737 promoting effect Effects 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 18
- 238000001132 ultrasonic dispersion Methods 0.000 description 11
- 230000005670 electromagnetic radiation Effects 0.000 description 6
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 3
- 229910052990 silicon hydride Inorganic materials 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 239000000084 colloidal system Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000002166 wet spinning Methods 0.000 description 2
- BSYNRYMUTXBXSQ-UHFFFAOYSA-N Aspirin Chemical compound CC(=O)OC1=CC=CC=C1C(O)=O BSYNRYMUTXBXSQ-UHFFFAOYSA-N 0.000 description 1
- -1 Schiff base compounds Chemical class 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 125000003172 aldehyde group Chemical group 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 230000003471 anti-radiation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229960004887 ferric hydroxide Drugs 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000006698 hydrazinolysis reaction Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- IEECXTSVVFWGSE-UHFFFAOYSA-M iron(3+);oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Fe+3] IEECXTSVVFWGSE-UHFFFAOYSA-M 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 125000001453 quaternary ammonium group Chemical class 0.000 description 1
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 1
- 230000035943 smell Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 125000001302 tertiary amino group Chemical group 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—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
- D06M11/36—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 with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/49—Oxides or hydroxides of elements of Groups 8, 9, 10 or 18 of the Periodic System; Ferrates; Cobaltates; Nickelates; Ruthenates; Osmates; Rhodates; Iridates; Palladates; Platinates
-
- 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
- D01D5/06—Wet spinning methods
-
- 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
- D01D5/24—Formation of filaments, threads, or the like with a hollow structure; Spinnerette packs therefor
-
- 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
- D01D5/253—Formation of filaments, threads, or the like with a non-circular cross section; Spinnerette packs therefor
-
- 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
- D01D5/28—Formation of filaments, threads, or the like while mixing different spinning solutions or melts during the spinning operation; Spinnerette packs therefor
- D01D5/30—Conjugate filaments; Spinnerette packs therefor
- D01D5/34—Core-skin structure; Spinnerette packs therefor
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- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/73—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 carbon or compounds thereof
- D06M11/74—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 carbon or compounds thereof with carbon or graphite; with carbides; with graphitic acids or their salts
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- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/77—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 silicon or compounds thereof
- D06M11/79—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 silicon or compounds thereof with silicon dioxide, silicic acids or their salts
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- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/12—Aldehydes; Ketones
- D06M13/127—Mono-aldehydes, e.g. formaldehyde; Monoketones
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- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
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- D06M14/00—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials
- D06M14/02—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials on to materials of natural origin
- D06M14/04—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials on to materials of natural origin of vegetal origin, e.g. cellulose or derivatives thereof
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- D06M16/00—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
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- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
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- D06M2101/04—Vegetal fibres
- D06M2101/06—Vegetal fibres cellulosic
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- 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
Abstract
本发明公开了一种轻质吸波面料及其制备方法,涉及面料技术领域。本发明以异形棉纤维为原料,利用丙烯酸氨基酯、2‑溴巴豆醛、3‑二丁胺基丙胺、4‑溴‑1,2‑环氧丁烷改性,提高抗菌活性,增益面料防霉性;接着,以氯化铁为原料,通过梯度升温热处理,形成中空结构的四氧化三铁纤维,与碳纳米管形成气凝胶前驱体;然后通过真空处理,促使气凝胶前驱体向改性棉纤维内部流动,并且在交变磁场的辅助下,四氧化三铁纤维穿插于改性棉纤维部分介孔,形成有效的电损耗网络;然后进行沉积处理,形成氮化硅纳米线薄膜,构成透波层,使电磁波不断衰减,在气凝胶内部耗散。本发明制备的面料具有防霉、防辐射的效果。
Description
技术领域
本发明涉及面料技术领域,具体为一种轻质吸波面料及其制备方法。
背景技术
电磁辐射是一种看不见、摸不着的污染,被人们称为“隐形杀手”。人们在日常生活中接触到的电视机、微波炉等大多数家用电器,以及雷达系统、广播信号收发系统、射频及微波医疗设备、通信发射台站等都可以产生各种形式、不同频率、不同强度的电磁辐射。为了控制电磁辐射带来的危害,越来越多防辐射面料问世。目前市场上销售的防辐射面料,其面料主要是将超细金属丝与纤维混合纺织而成的,或将金属离子涂层涂覆在纤维布料上,基本上都是屏蔽类的防辐射产品,易造成空间的电磁辐射重复污染这样一个缺陷。
此外,纺织品暴露在合适的温度和湿度情况下,霉菌就能很快的生长繁殖,使面料发臭,并且还会影响使用者的身体健康,引起不适,不能满足社会需求,故而提出了一种防霉效果好的轻质吸波面料解决上述问题。
发明内容
本发明的目的在于提供一种轻质吸波面料及其制备方法,以解决现有技术中存在的问题。
为了解决上述技术问题,本发明提供如下技术方案:一种轻质吸波面料,包括透波层、气凝胶面料,所述轻质吸波面料由以下方法制得,将改性棉纤维编织成面料基体,在磁场中,将面料基体浸渍于前驱体溶液,真空处理后,冷冻干燥,再次置于相同真空环境中,洗涤得气凝胶面料,向气凝胶面料气相沉积氮化硅至预定时间后,加压,继续沉积得轻质吸波面料。
进一步的,所述改性棉纤维由异形棉纤维、丙烯酸氨基酯、2-溴巴豆醛、3-二丁胺基丙胺、4-溴-1,2-环氧丁烷制得。
进一步的,所述异形棉纤维由以下方法制得,以棉纤维素和N,N-二甲基甲酰胺为皮层纺丝液,以聚乙烯吡咯烷酮和N,N-二甲基甲酰胺为芯层纺丝液,采用十字形同轴异形喷丝头,进行纺丝。
进一步的,所述前驱体溶液由将四氧化三铁纳米纤维、L-抗坏血酸、羧甲基纤维素、碳纳米管制得;所述四氧化三铁纳米纤维由以下方法制得,将六水合三氯化铁溶于蒸馏水中,加入沸腾蒸馏水,得胶体溶液,纺丝,得前驱体纤维;将前驱体纤维梯度升温后,冷却至室温,在氮氢混合气氛下,继续加热。
进一步的,一种轻质吸波面料的制备方法,包括以下制备步骤:
(1)将预处理棉纤维、水合肼、质量分数36%的盐酸按质量比1:1.6:1.8~1:2.4:2.6混合,加热至70~82℃,加入预处理棉纤维质量40~48倍的乙二醇,40~60rpm下搅拌30~46min后,升温至116~130℃,反应6~12h后,冰水浴冷却30~44min,捞出,用无水乙醇洗涤5~10次,40~60℃干燥6~10h,得肼基化棉纤维;将肼基化棉纤维、无水乙醇按质量比1:148~1:160混合,70~84℃、50~80rpm下搅拌40~66min,再加入肼基化棉纤维质量0.6~1.2倍的2-溴巴豆醛,相同温度、相同搅拌速度下反应2~6h后,冷却至室温,静置20~26h,捞出,得席夫碱棉纤维;
(2)将席夫碱棉纤维、3-二丁胺基丙胺、去离子水按质量比1:0.3:8~1:0.8:20混合,68~82℃、40~70rpm下搅拌2~6h后,捞出,用去离子水洗涤3~7min,再加入席夫碱棉纤维质量1.3~2.5倍的石油醚,加热至60~70℃,加入席夫碱棉纤维质量0.6~1.0倍的4-溴-1,2-环氧丁烷,保温反应10~16h后,真空度0.01~0.05MPa、64~80℃下蒸馏2~6h,捞出,用无水乙醇洗涤5~9次,得改性棉纤维;
(3)将改性棉纤维编织,得克重180~220g/m2的面料基体;在25~35Hz、0.4~0.6A的磁场中,将面料基体置于面料基体质量0.05~0.2倍的前驱体溶液,抽真空至1×10-5~5×10-5Pa,浸渍6~10h后,加热至80~94℃,处理30~44min后,取出,-38~-20℃冷冻1~3h,相同真空度、相同温度下还原2~5h后,用无水乙醇洗涤4~10次,50~68℃干燥8~12h得气凝胶面料;
(4)将气凝胶面料置于等离子体仪器中,抽真空至2×10-4~6×10-4Pa,按流量比2.6:13.3:1~9.3:33.3:1通入氩气、氮气和四氢化硅,至气压为2~7Pa,沉积28~41min后,按相同流量通入氩气、氮气和四氢化硅至气压为2~5MPa,反应2~6h得轻质吸波面料。
进一步的,步骤(1)所述预处理棉纤维由以下方法制得,将异形棉纤维、丙烯酸氨基酯、氢氧化钠和去离子水按质量比1:0.1:0.05:10~1:0.4:0.09:15,40~60rpm下搅拌30~46min后,加入异形棉纤维质量0.02~0.03倍的过硫酸钾、异形棉纤维质量8~10倍的去离子水,64~76℃下反应2~5h后,捞出,用蒸馏水冲洗4~10min,室温下干燥7~13h,得预处理棉纤维。
进一步的,所述异形棉纤维由以下方法制得,将棉纤维素、N,N-二甲基甲酰胺按质量比1:5~1:9混合,50~60℃、50~100rpm下搅拌2~5h后,55~68℃下脱泡40~56min,得皮层纺丝液;将聚乙烯吡咯烷酮、N,N-二甲基甲酰胺按质量比1:4~1:9混合,60~70℃、50~100rpm下搅拌4~7h后,55~68℃下脱泡40~56min,得芯层纺丝液;采用十字形同轴异形喷丝头,芯层纺丝液流速为0.2~1.0mL/h,皮层纺丝液流速为10mL/h,得初生纤维;将初生纤维置于初生纤维质量6~14倍的去离子水中,浸泡20~28h后,于-68~-60℃冷冻5~8h,再于-58~-50℃冷冻48~52h,得异形棉纤维。
进一步的,步骤(3)所述前驱体溶液由以下方法制得,将四氧化三铁纳米纤维分散四氧化三铁纳米纤维质量138~146倍的去离子水中,30~40kHz下超声分散16~28min后,按质量比1:0.01:0.8~1:0.03:1.4加入L-抗坏血酸、羧甲基纤维素、碳纳米管,L-抗坏血酸和四氧化三铁纳米纤维的质量比为3:1,相同频率下超声分散30~46min,得前驱体溶液。
进一步的,所述四氧化三铁纳米纤维由以下方法制得,将六水合三氯化铁溶于六水合三氯化铁质量4~8倍的蒸馏水中,40~80rpm搅拌下,以0.1~0.3mL/min加入六水合三氯化铁质量22~28倍的100℃蒸馏水,静置2~6min,冷却至室温,陈化10~14h后,以2~4mL/h纺丝,得前驱体纤维;将前驱体纤维以0.5~1.1℃/min升温至380~400℃,保温8~12h,再以8~12℃/min升温至700~720℃,保温1.5~3h后,冷却至室温;在氮氢混合气氛下,加热至390~420℃,还原1~3h,氮氢混合气氛中下氮气和氢气的体积比为1:0.014,得四氧化三铁纳米纤维。
进一步的,步骤(4)所述等离子体仪器的功率为300~500W;所述四氢化硅的流量为1.5sccm。
与现有技术相比,本发明所达到的有益效果是:
本发明以改性棉纤维为原料,编织成面料后,填充吸波气凝胶,并沉积透波层,以实现防辐射、防霉的效果。
首先,本发明利用湿法纺丝制备兼具中空和介孔结构的异形棉纤维,可使面料达到快干效果,减少面料受潮风险,提高面料的防霉性;然后利用丙烯酸氨基酯的双键接枝于棉纤维分子链中,令氨基肼基化后,与2-溴巴豆醛的醛基反应,形成席夫碱化合物,提高纤维抗菌活性,增益面料的防霉性;3-二丁胺基丙胺的氨基与丙烯酸氨基酯的羧基反应,4-溴-1,2-环氧丁烷又与3-二丁胺基丙胺的叔胺基,形成季铵盐,提高纤维抗菌活性和广谱性,能够有效抑制霉菌生物合成,导致细胞裂解,有效提高面料防霉效果。
其次,以氯化铁为原料,通过水解获得氢氧化铁胶体,纺丝得前驱体纤维,经过梯度升温热处理,纤维表面会先发生脱水和有机物氧化分解而形成一层坚硬的壳层作为支撑体,同时内部胶体由中心分离而向表面收缩,从而形成中空结构的四氧化三铁纤维,与碳纳米管混合构成气凝胶前驱体溶液;改性棉纤维编织成面料基体后,进行真空处理,使改性棉纤维的空腔、裂纹及介孔内的气体排出,促使气凝胶前驱体溶液向改性棉纤维内部流动,并且在交变磁场的辅助下,四氧化三铁纤维均匀分散,并且在磁场力及真空环境的推动下,穿过改性棉纤维部分介孔,经冷冻干燥,相互串联形成多维网络结构,形成有效的电损耗网络,使面料具有优异的吸波性能,从而具有防辐射效果;然后进行沉积处理,利用螺旋波等离子体,在气凝胶面料表面及孔隙内部成核生长,形成氮化硅纳米线,并且施加压力,使氮化硅纳米线沿面料表面生长,从而缠绕于气凝胶面料表面微孔,并且相互交联形成薄膜,构成透波层,能够使电磁波不断衰减,在气凝胶内部耗散,增益面料防辐射效果。
具体实施方式
下面将结合本发明实施例,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
为了更清楚的说明本发明提供的方法通过以下实施例进行详细说明,在以下实施例中制作的轻质吸波面料的各指标测试方法如下:
防辐射性:取相同大小的实施例与对比例进行防辐射效果测试,先用电磁检测仪对准电脑屏幕和手机,分别测其辐射值,然后将试样分别覆盖在电脑屏幕、手机上,进行测量,测量2次取平均值。
防霉性:取相同大小的实施例与对比例进行防霉效果测试,参照GB/t 24346评定防霉等级,具体的标准为:0级-在放大镜下无明显长霉;1级-霉菌生长稀少或局部生长,在样品表面的覆盖面积小于10%;2级-霉菌在样品表面覆盖面积为10~30%;3级-霉菌在样品表面覆盖面积为30~60%;4级-霉菌在样品表面覆盖面积大于60%。
实施例1
一种轻质吸波面料的制备方法,所述轻质吸波面料的制备方法包括以下制备步骤:
(1)将棉纤维素、N,N-二甲基甲酰胺按质量比1:5混合,50℃、50rpm下搅拌2h后,55℃下脱泡40min,得皮层纺丝液;将聚乙烯吡咯烷酮、N,N-二甲基甲酰胺按质量比1:4混合,60℃、50rpm下搅拌4h后,55℃下脱泡40min,得芯层纺丝液;采用十字形同轴异形喷丝头,芯层纺丝液流速为0.2mL/h,皮层纺丝液流速为10mL/h,得初生纤维;将初生纤维置于初生纤维质量6倍的去离子水中,浸泡20h后,于-68℃冷冻5h,再于-58℃冷冻48h,得异形棉纤维;将异形棉纤维、丙烯酸氨基酯、氢氧化钠和去离子水按质量比1:0.1:0.05:10,40rpm下搅拌30min后,加入异形棉纤维质量0.02倍的过硫酸钾、异形棉纤维质量8倍的去离子水,64℃下反应2h后,捞出,用蒸馏水冲洗4min,室温下干燥7h,得预处理棉纤维;
(2)将预处理棉纤维、水合肼、质量分数36%的盐酸按质量比1:1.6:1.8混合,加热至70℃,加入预处理棉纤维质量40倍的乙二醇,40rpm下搅拌30min后,升温至116℃,反应6h后,冰水浴冷却30min,捞出,用无水乙醇洗涤5次,40℃干燥6h,得肼基化棉纤维;将肼基化棉纤维、无水乙醇按质量比1:148混合,70℃、50rpm下搅拌40min,再加入肼基化棉纤维质量0.6倍的2-溴巴豆醛,相同温度、相同搅拌速度下反应2h后,冷却至室温,静置20h,捞出,得席夫碱棉纤维;
(3)将席夫碱棉纤维、3-二丁胺基丙胺、去离子水按质量比1:0.3:8混合,68℃、40rpm下搅拌2h后,捞出,用去离子水洗涤3min,再加入席夫碱棉纤维质量1.3倍的石油醚,加热至60℃,加入席夫碱棉纤维质量0.6倍的4-溴-1,2-环氧丁烷,保温反应10h后,真空度0.01MPa、64℃下蒸馏2h,捞出,用无水乙醇洗涤5次,得改性棉纤维;
(4)将六水合三氯化铁溶于六水合三氯化铁质量4倍的蒸馏水中,40rpm搅拌下,以0.1mL/min加入六水合三氯化铁质量22倍的100℃蒸馏水,静置2min,冷却至室温,陈化10h后,以2mL/h纺丝,得前驱体纤维;将前驱体纤维以0.5℃/min升温至380℃,保温8h,再以8℃/min升温至700℃,保温1.5h后,冷却至室温;在氮氢混合气氛下,加热至390℃,还原1h,氮氢混合气氛中下氮气和氢气的体积比为1:0.014,得四氧化三铁纳米纤维;
(5)将改性棉纤维编织,得克重180g/m2的面料基体;将四氧化三铁纳米纤维分散四氧化三铁纳米纤维质量138倍的去离子水中,30kHz下超声分散16min后,按质量比1:0.01:0.8加入L-抗坏血酸、羧甲基纤维素、碳纳米管,L-抗坏血酸和四氧化三铁纳米纤维的质量比为3:1,相同频率下超声分散30min,得前驱体溶液;在25Hz、0.4A的磁场中,将面料基体置于面料基体质量0.05倍的前驱体溶液,抽真空至1×10-5Pa,浸渍6h后,加热至80℃,处理30min后,取出,-38℃冷冻1h,相同真空度、相同温度下还原2h后,用无水乙醇洗涤4次,50℃干燥8h得气凝胶面料;
(6)将气凝胶面料置于功率为300W的等离子体仪器中,抽真空至2×10-4Pa,按流量比2.6:13.3:1通入氩气、氮气和四氢化硅,四氢化硅的流量为1.5sccm,至气压为2Pa,沉积28min后,按相同流量通入氩气、氮气和四氢化硅至气压为2MPa,反应2h得轻质吸波面料。
实施例2
一种轻质吸波面料的制备方法,所述轻质吸波面料的制备方法包括以下制备步骤:
(1)将棉纤维素、N,N-二甲基甲酰胺按质量比1:7混合,55℃、80rpm下搅拌3.5h后,62℃下脱泡48min,得皮层纺丝液;将聚乙烯吡咯烷酮、N,N-二甲基甲酰胺按质量比1:6.5混合,65℃、70rpm下搅拌5.5h后,61℃下脱泡48min,得芯层纺丝液;采用十字形同轴异形喷丝头,芯层纺丝液流速为0.6mL/h,皮层纺丝液流速为10mL/h,得初生纤维;将初生纤维置于初生纤维质量10倍的去离子水中,浸泡24h后,于-64℃冷冻6.5h,再于-54℃冷冻50h,得异形棉纤维;将异形棉纤维、丙烯酸氨基酯、氢氧化钠和去离子水按质量比1:0.25:0.07:12.5,50rpm下搅拌38min后,加入异形棉纤维质量0.025倍的过硫酸钾、异形棉纤维质量9倍的去离子水,70℃下反应3.5h后,捞出,用蒸馏水冲洗7min,室温下干燥10h,得预处理棉纤维;
(2)将预处理棉纤维、水合肼、质量分数36%的盐酸按质量比1:2:2.2混合,加热至76℃,加入预处理棉纤维质量44倍的乙二醇,50rpm下搅拌38min后,升温至123℃,反应9h后,冰水浴冷却37min,捞出,用无水乙醇洗涤7次,50℃干燥8h,得肼基化棉纤维;将肼基化棉纤维、无水乙醇按质量比1:154混合,77℃、65rpm下搅拌53min,再加入肼基化棉纤维质量0.9倍的2-溴巴豆醛,相同温度、相同搅拌速度下反应4h后,冷却至室温,静置23h,捞出,得席夫碱棉纤维;
(3)将席夫碱棉纤维、3-二丁胺基丙胺、去离子水按质量比1:0.55:14混合,75℃、55rpm下搅拌4h后,捞出,用去离子水洗涤5min,再加入席夫碱棉纤维质量1.9倍的石油醚,加热至65℃,加入席夫碱棉纤维质量0.8倍的4-溴-1,2-环氧丁烷,保温反应13h后,真空度0.03MPa、72℃下蒸馏4h,捞出,用无水乙醇洗涤7次,得改性棉纤维;
(4)将六水合三氯化铁溶于六水合三氯化铁质量6倍的蒸馏水中,60rpm搅拌下,以0.2mL/min加入六水合三氯化铁质量25倍的100℃蒸馏水,静置4min,冷却至室温,陈化12h后,以3mL/h纺丝,得前驱体纤维;将前驱体纤维以0.8℃/min升温至390℃,保温10h,再以10℃/min升温至710℃,保温2.25h后,冷却至室温;在氮氢混合气氛下,加热至405℃,还原2h,氮氢混合气氛中下氮气和氢气的体积比为1:0.014,得四氧化三铁纳米纤维;
(5)将改性棉纤维编织,得克重200g/m2的面料基体;将四氧化三铁纳米纤维分散四氧化三铁纳米纤维质量142倍的去离子水中,35kHz下超声分散22min后,按质量比1:0.02:1.1加入L-抗坏血酸、羧甲基纤维素、碳纳米管,L-抗坏血酸和四氧化三铁纳米纤维的质量比为3:1,相同频率下超声分散38min,得前驱体溶液;在30Hz、0.5A的磁场中,将面料基体置于面料基体质量0.13倍的前驱体溶液,抽真空至3×10-5Pa,浸渍8h后,加热至87℃,处理37min后,取出,-29℃冷冻2h,相同真空度、相同温度下还原3.5h后,用无水乙醇洗涤7次,59℃干燥10h得气凝胶面料;
(6)将气凝胶面料置于功率为400W的等离子体仪器中,抽真空至4×10-4Pa,按流量比5.9:23.3:1通入氩气、氮气和四氢化硅,四氢化硅的流量为1.5sccm,至气压为4Pa,沉积34min后,按相同流量通入氩气、氮气和四氢化硅至气压为3.5MPa,反应4h得轻质吸波面料。
实施例3
一种轻质吸波面料的制备方法,所述轻质吸波面料的制备方法包括以下制备步骤:
(1)将棉纤维素、N,N-二甲基甲酰胺按质量比1:9混合,60℃、100rpm下搅拌5h后,68℃下脱泡56min,得皮层纺丝液;将聚乙烯吡咯烷酮、N,N-二甲基甲酰胺按质量比1:9混合,70℃、100rpm下搅拌7h后,68℃下脱泡56min,得芯层纺丝液;采用十字形同轴异形喷丝头,芯层纺丝液流速为1.0mL/h,皮层纺丝液流速为10mL/h,得初生纤维;将初生纤维置于初生纤维质量14倍的去离子水中,浸泡28h后,于-60℃冷冻8h,再于-50℃冷冻52h,得异形棉纤维;将异形棉纤维、丙烯酸氨基酯、氢氧化钠和去离子水按质量比1:0.4:0.09:15,60rpm下搅拌46min后,加入异形棉纤维质量0.03倍的过硫酸钾、异形棉纤维质量10倍的去离子水,76℃下反应5h后,捞出,用蒸馏水冲洗10min,室温下干燥13h,得预处理棉纤维;
(2)将预处理棉纤维、水合肼、质量分数36%的盐酸按质量比1:2.4:2.6混合,加热至82℃,加入预处理棉纤维质量48倍的乙二醇,60rpm下搅拌46min后,升温至130℃,反应12h后,冰水浴冷却44min,捞出,用无水乙醇洗涤10次,60℃干燥10h,得肼基化棉纤维;将肼基化棉纤维、无水乙醇按质量比1:160混合,84℃、80rpm下搅拌66min,再加入肼基化棉纤维质量1.2倍的2-溴巴豆醛,相同温度、相同搅拌速度下反应6h后,冷却至室温,静置26h,捞出,得席夫碱棉纤维;
(3)将席夫碱棉纤维、3-二丁胺基丙胺、去离子水按质量比1:0.8:20混合,82℃、70rpm下搅拌6h后,捞出,用去离子水洗涤7min,再加入席夫碱棉纤维质量2.5倍的石油醚,加热至70℃,加入席夫碱棉纤维质量1.0倍的4-溴-1,2-环氧丁烷,保温反应16h后,真空度0.05MPa、80℃下蒸馏6h,捞出,用无水乙醇洗涤9次,得改性棉纤维;
(4)将六水合三氯化铁溶于六水合三氯化铁质量8倍的蒸馏水中,80rpm搅拌下,以0.3mL/min加入六水合三氯化铁质量28倍的100℃蒸馏水,静置6min,冷却至室温,陈化14h后,以4mL/h纺丝,得前驱体纤维;将前驱体纤维以1.1℃/min升温至400℃,保温12h,再以12℃/min升温至720℃,保温3h后,冷却至室温;在氮氢混合气氛下,加热至420℃,还原3h,氮氢混合气氛中下氮气和氢气的体积比为1:0.014,得四氧化三铁纳米纤维;
(5)将改性棉纤维编织,得克重220g/m2的面料基体;将四氧化三铁纳米纤维分散四氧化三铁纳米纤维质量146倍的去离子水中,40kHz下超声分散28min后,按质量比1:0.03:1.4加入L-抗坏血酸、羧甲基纤维素、碳纳米管,L-抗坏血酸和四氧化三铁纳米纤维的质量比为3:1,相同频率下超声分散46min,得前驱体溶液;在35Hz、0.6A的磁场中,将面料基体置于面料基体质量0.2倍的前驱体溶液,抽真空至5×10-5Pa,浸渍10h后,加热至94℃,处理44min后,取出,-20℃冷冻3h,相同真空度、相同温度下还原5h后,用无水乙醇洗涤10次,68℃干燥12h得气凝胶面料;
(6)将气凝胶面料置于功率为500W的等离子体仪器中,抽真空至6×10-4Pa,按流量比9.3:33.3:1通入氩气、氮气和四氢化硅,四氢化硅的流量为1.5sccm,至气压为7Pa,沉积41min后,按相同流量通入氩气、氮气和四氢化硅至气压为5MPa,反应6h得轻质吸波面料。
对比例1
对比例1与实施例2的区别仅在于步骤(1)的不同,将步骤(1)改为:将棉纤维、丙烯酸氨基酯、氢氧化钠和去离子水按质量比1:0.25:0.07:12.5,50rpm下搅拌38min后,加入异形棉纤维质量0.025倍的过硫酸钾、异形棉纤维质量9倍的去离子水,70℃下反应3.5h后,捞出,用蒸馏水冲洗7min,室温下干燥10h,得预处理棉纤维。其余制备步骤同实施例2。
对比例2
对比例2与实施例2的区别在于无步骤(2),将步骤(3)改为:将预处理棉纤维、3-二丁胺基丙胺、去离子水按质量比1:0.55:14混合,75℃、55rpm下搅拌4h后,捞出,用去离子水洗涤5min,再加入预处理棉纤维质量1.9倍的石油醚,加热至65℃,加入预处理棉纤维质量0.8倍的4-溴-1,2-环氧丁烷,保温反应13h后,真空度0.03MPa、72℃下蒸馏4h,捞出,用无水乙醇洗涤7次,得改性棉纤维。其余制备步骤同实施例2。
对比例3
对比例3与实施例2的区别在于无步骤(3),将步骤(2)改为:将预处理棉纤维、水合肼、质量分数36%的盐酸按质量比1:2:2.2混合,加热至76℃,加入预处理棉纤维质量44倍的乙二醇,50rpm下搅拌38min后,升温至123℃,反应9h后,冰水浴冷却37min,捞出,用无水乙醇洗涤7次,50℃干燥8h,得肼基化棉纤维;将肼基化棉纤维、无水乙醇按质量比1:154混合,77℃、65rpm下搅拌53min,再加入肼基化棉纤维质量0.9倍的2-溴巴豆醛,相同温度、相同搅拌速度下反应4h后,冷却至室温,静置23h,捞出,得改性棉纤维。其余制备步骤同实施例2。
对比例4
对比例4与实施例2的区别在于无步骤(4),将步骤(5)改为:将改性棉纤维编织,得克重200g/m2的面料基体;将四氧化三铁分散四氧化三铁质量142倍的去离子水中,35kHz下超声分散22min后,按质量比1:0.02:1.1加入L-抗坏血酸、羧甲基纤维素、碳纳米管,L-抗坏血酸和四氧化三铁的质量比为3:1,相同频率下超声分散38min,得前驱体溶液;在30Hz、0.5A的磁场中,将面料基体置于面料基体质量0.13倍的前驱体溶液,抽真空至3×10-5Pa,浸渍8h后,加热至87℃,处理37min后,取出,-29℃冷冻2h,相同真空度、相同温度下还原3.5h后,用无水乙醇洗涤7次,59℃干燥10h得气凝胶面料。其余制备步骤同实施例2。
对比例5
对比例5与实施例2的区别在于步骤(5)的不同,将步骤(5)改为:将改性棉纤维编织,得克重200g/m2的面料基体;将四氧化三铁纳米纤维分散四氧化三铁纳米纤维质量142倍的去离子水中,35kHz下超声分散22min后,按质量比1:0.02:1.1加入L-抗坏血酸、羧甲基纤维素、碳纳米管,L-抗坏血酸和四氧化三铁纳米纤维的质量比为3:1,相同频率下超声分散38min,得前驱体溶液;将面料基体置于面料基体质量0.13倍的前驱体溶液,抽真空至3×10-5Pa,浸渍8h后,加热至87℃,处理37min后,取出,-29℃冷冻2h,相同真空度、相同温度下还原3.5h后,用无水乙醇洗涤7次,59℃干燥10h得气凝胶面料。其余制备步骤同实施例2。
对比例6
对比例6与实施例2的区别在于无步骤(6),其余制备步骤同实施例2。
效果例
下表1给出了采用本发明实施例1至3与对比例1至6的轻质吸波面料的性能分析结果。
表1
从实施例与对比例的电脑屏幕、手机覆盖前后的电磁辐射值的实验数据对比可发现,本发明通过制备异形棉纤维,兼具中空和介孔结构,真空环境下,浸泡于前驱体溶液,能使改性棉纤维的空腔、介孔内的气体排出,促使前驱体溶液向改性棉纤维内部流动,同时采用四氧化三铁中空纳米纤维与碳纳米管为前驱体溶液,利用其细长结构,在磁场力推动下,穿插于改性棉纤维的介孔内,并且相互搭接,形成多维网络结构,形成有效的电损耗网络,使面料具有优异的吸波性能,然后沉积透波层,使电磁辐射波呈“之”字形损耗,在气凝胶内部耗散,提高面料的防辐射能力;从实施例与对比例的防霉等级实验数据对比可发现,本发明利用湿法纺丝制备兼具中空和介孔结构的异形棉纤维,可使面料达到快干效果,减少面料受潮风险,提高面料的防霉性;然后利用丙烯酸氨基酯、2-溴巴豆醛、3-二丁胺基丙胺、4-溴-1,2-环氧丁烷进行改性,在纤维表面形成季铵盐-席夫碱化合物薄膜,叠加抗菌活性,能够有效抑制霉菌生物合成,有效提高面料防霉效果。
对于本领域技术人员而言,显然本发明不限于上述示范性实施例的细节,而且在不背离本发明的精神或基本特征的情况下,能够以其他的具体形式实现本发明。因此,无论从哪一点来看,均应将实施例看作是示范性的,而且是非限制性的,本发明的范围由所附权利要求而不是上述说明限定,因此旨在将落在权利要求的等同要件的含义和范围内的所有变化囊括在本发明内。不应将权利要求中的任何标记视为限制所涉及的权利要求。
Claims (10)
1.一种轻质吸波面料,包括透波层、气凝胶面料,其特征在于,所述轻质吸波面料由以下方法制得,将改性棉纤维编织成面料基体,在磁场中,将面料基体浸渍于前驱体溶液,真空处理后,冷冻干燥,再次置于相同真空环境中,洗涤得气凝胶面料,向气凝胶面料气相沉积氮化硅至预定时间后,加压,继续沉积得轻质吸波面料。
2.根据权利要求1所述的一种轻质吸波面料,其特征在于,所述改性棉纤维由异形棉纤维、丙烯酸氨基酯、2-溴巴豆醛、3-二丁胺基丙胺、4-溴-1,2-环氧丁烷制得。
3.根据权利要求2所述的一种轻质吸波面料,其特征在于,所述异形棉纤维由以下方法制得,以棉纤维素和N,N-二甲基甲酰胺为皮层纺丝液,以聚乙烯吡咯烷酮和N,N-二甲基甲酰胺为芯层纺丝液,采用十字形同轴异形喷丝头,进行纺丝。
4.根据权利要求1所述的一种轻质吸波面料,其特征在于,所述前驱体溶液由将四氧化三铁纳米纤维、L-抗坏血酸、羧甲基纤维素、碳纳米管制得;所述四氧化三铁纳米纤维由以下方法制得,将六水合三氯化铁溶于蒸馏水中,加入沸腾蒸馏水,得胶体溶液,纺丝,得前驱体纤维;将前驱体纤维梯度升温后,冷却至室温,在氮氢混合气氛下,继续加热。
5.一种轻质吸波面料的制备方法,其特征在于,包括以下制备步骤:
(1)将预处理棉纤维、水合肼、质量分数36%的盐酸按质量比1:1.6:1.8~1:2.4:2.6混合,加热至70~82℃,加入预处理棉纤维质量40~48倍的乙二醇,40~60rpm下搅拌30~46min后,升温至116~130℃,反应6~12h后,冰水浴冷却30~44min,捞出,用无水乙醇洗涤5~10次,40~60℃干燥6~10h,得肼基化棉纤维;将肼基化棉纤维、无水乙醇按质量比1:148~1:160混合,70~84℃、50~80rpm下搅拌40~66min,再加入肼基化棉纤维质量0.6~1.2倍的2-溴巴豆醛,相同温度、相同搅拌速度下反应2~6h后,冷却至室温,静置20~26h,捞出,得席夫碱棉纤维;
(2)将席夫碱棉纤维、3-二丁胺基丙胺、去离子水按质量比1:0.3:8~1:0.8:20混合,68~82℃、40~70rpm下搅拌2~6h后,捞出,用去离子水洗涤3~7min,再加入席夫碱棉纤维质量1.3~2.5倍的石油醚,加热至60~70℃,加入席夫碱棉纤维质量0.6~1.0倍的4-溴-1,2-环氧丁烷,保温反应10~16h后,真空度0.01~0.05MPa、64~80℃下蒸馏2~6h,捞出,用无水乙醇洗涤5~9次,得改性棉纤维;
(3)将改性棉纤维编织,得克重180~220g/m2的面料基体;在25~35Hz、0.4~0.6A的磁场中,将面料基体置于面料基体质量0.05~0.2倍的前驱体溶液,抽真空至1×10-5~5×10-5Pa,浸渍6~10h后,加热至80~94℃,处理30~44min后,取出,-38~-20℃冷冻1~3h,相同真空度、相同温度下还原2~5h后,用无水乙醇洗涤4~10次,50~68℃干燥8~12h得气凝胶面料;
(4)将气凝胶面料置于等离子体仪器中,抽真空至2×10-4~6×10-4Pa,按流量比2.6:13.3:1~9.3:33.3:1通入氩气、氮气和四氢化硅,至气压为2~7Pa,沉积28~41min后,按相同流量通入氩气、氮气和四氢化硅至气压为2~5MPa,反应2~6h得轻质吸波面料。
6.根据权利要求5所述的一种轻质吸波面料的制备方法,其特征在于,步骤(1)所述预处理棉纤维由以下方法制得,将异形棉纤维、丙烯酸氨基酯、氢氧化钠和去离子水按质量比1:0.1:0.05:10~1:0.4:0.09:15,40~60rpm下搅拌30~46min后,加入异形棉纤维质量0.02~0.03倍的过硫酸钾、异形棉纤维质量8~10倍的去离子水,64~76℃下反应2~5h后,捞出,用蒸馏水冲洗4~10min,室温下干燥7~13h,得预处理棉纤维。
7.根据权利要求6所述的一种轻质吸波面料的制备方法,其特征在于,所述异形棉纤维由以下方法制得,将棉纤维素、N,N-二甲基甲酰胺按质量比1:5~1:9混合,50~60℃、50~100rpm下搅拌2~5h后,55~68℃下脱泡40~56min,得皮层纺丝液;将聚乙烯吡咯烷酮、N,N-二甲基甲酰胺按质量比1:4~1:9混合,60~70℃、50~100rpm下搅拌4~7h后,55~68℃下脱泡40~56min,得芯层纺丝液;采用十字形同轴异形喷丝头,芯层纺丝液流速为0.2~1.0mL/h,皮层纺丝液流速为10mL/h,得初生纤维;将初生纤维置于初生纤维质量6~14倍的去离子水中,浸泡20~28h后,于-68~-60℃冷冻5~8h,再于-58~-50℃冷冻48~52h,得异形棉纤维。
8.根据权利要求5所述的一种轻质吸波面料的制备方法,其特征在于,步骤(3)所述前驱体溶液由以下方法制得,将四氧化三铁纳米纤维分散四氧化三铁纳米纤维质量138~146倍的去离子水中,30~40kHz下超声分散16~28min后,按质量比1:0.01:0.8~1:0.03:1.4加入L-抗坏血酸、羧甲基纤维素、碳纳米管,L-抗坏血酸和四氧化三铁纳米纤维的质量比为3:1,相同频率下超声分散30~46min,得前驱体溶液。
9.根据权利要求8所述的一种轻质吸波面料的制备方法,其特征在于,所述四氧化三铁纳米纤维由以下方法制得,将六水合三氯化铁溶于六水合三氯化铁质量4~8倍的蒸馏水中,40~80rpm搅拌下,以0.1~0.3mL/min加入六水合三氯化铁质量22~28倍的100℃蒸馏水,静置2~6min,冷却至室温,陈化10~14h后,以2~4mL/h纺丝,得前驱体纤维;将前驱体纤维以0.5~1.1℃/min升温至380~400℃,保温8~12h,再以8~12℃/min升温至700~720℃,保温1.5~3h后,冷却至室温;在氮氢混合气氛下,加热至390~420℃,还原1~3h,氮氢混合气氛中下氮气和氢气的体积比为1:0.014,得四氧化三铁纳米纤维。
10.根据权利要求5所述的一种轻质吸波面料的制备方法,其特征在于,步骤(4)所述等离子体仪器的功率为300~500W;所述四氢化硅的流量为1.5sccm。
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