CN114657775B - 一种阻燃耐寒防割屏蔽多频谱面料及其制备方法 - Google Patents
一种阻燃耐寒防割屏蔽多频谱面料及其制备方法 Download PDFInfo
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- CN114657775B CN114657775B CN202210378840.6A CN202210378840A CN114657775B CN 114657775 B CN114657775 B CN 114657775B CN 202210378840 A CN202210378840 A CN 202210378840A CN 114657775 B CN114657775 B CN 114657775B
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- 239000003063 flame retardant Substances 0.000 title claims abstract description 99
- 239000004744 fabric Substances 0.000 title claims abstract description 91
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 238000002360 preparation method Methods 0.000 title claims abstract description 33
- 238000004519 manufacturing process Methods 0.000 title description 2
- 239000000835 fiber Substances 0.000 claims abstract description 284
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 97
- -1 polytetrafluoroethylene Polymers 0.000 claims abstract description 90
- 229920005749 polyurethane resin Polymers 0.000 claims abstract description 76
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 71
- 229920002302 Nylon 6,6 Polymers 0.000 claims abstract description 65
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 49
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 49
- 239000000805 composite resin Substances 0.000 claims abstract description 47
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- 229910021641 deionized water Inorganic materials 0.000 claims description 52
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- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 48
- 238000002156 mixing Methods 0.000 claims description 45
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- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 42
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- 239000004332 silver Substances 0.000 claims description 36
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 28
- 229910052708 sodium Inorganic materials 0.000 claims description 28
- 239000011734 sodium Substances 0.000 claims description 28
- XFTALRAZSCGSKN-UHFFFAOYSA-M sodium;4-ethenylbenzenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C1=CC=C(C=C)C=C1 XFTALRAZSCGSKN-UHFFFAOYSA-M 0.000 claims description 27
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 24
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 24
- 239000000203 mixture Substances 0.000 claims description 24
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 24
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims description 22
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 21
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- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 claims description 18
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- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 16
- 239000011888 foil Substances 0.000 claims description 16
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- 238000001556 precipitation Methods 0.000 claims description 13
- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical compound C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 claims description 12
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 claims description 12
- ROFVEXUMMXZLPA-UHFFFAOYSA-N Bipyridyl Chemical compound N1=CC=CC=C1C1=CC=CC=N1 ROFVEXUMMXZLPA-UHFFFAOYSA-N 0.000 claims description 12
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 12
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 12
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 12
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 12
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 12
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims description 12
- 229940077388 benzenesulfonate Drugs 0.000 claims description 12
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- 238000004140 cleaning Methods 0.000 claims description 12
- 229910000365 copper sulfate Inorganic materials 0.000 claims description 12
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 12
- 239000008098 formaldehyde solution Substances 0.000 claims description 12
- 239000008103 glucose Substances 0.000 claims description 12
- 239000011259 mixed solution Substances 0.000 claims description 12
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 12
- 229910017604 nitric acid Inorganic materials 0.000 claims description 12
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 claims description 12
- 230000000149 penetrating effect Effects 0.000 claims description 12
- 229920002635 polyurethane Polymers 0.000 claims description 12
- 239000004814 polyurethane Substances 0.000 claims description 12
- NNFCIKHAZHQZJG-UHFFFAOYSA-N potassium cyanide Chemical compound [K+].N#[C-] NNFCIKHAZHQZJG-UHFFFAOYSA-N 0.000 claims description 12
- LJCNRYVRMXRIQR-OLXYHTOASA-L potassium sodium L-tartrate Chemical compound [Na+].[K+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O LJCNRYVRMXRIQR-OLXYHTOASA-L 0.000 claims description 12
- 229940074439 potassium sodium tartrate Drugs 0.000 claims description 12
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- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims description 12
- 235000011006 sodium potassium tartrate Nutrition 0.000 claims description 12
- 239000003381 stabilizer Substances 0.000 claims description 12
- 239000001119 stannous chloride Substances 0.000 claims description 12
- 235000011150 stannous chloride Nutrition 0.000 claims description 12
- 235000002906 tartaric acid Nutrition 0.000 claims description 12
- 239000011975 tartaric acid Substances 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 11
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 9
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 9
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 claims description 9
- 239000013638 trimer Substances 0.000 claims description 9
- PQUCIEFHOVEZAU-UHFFFAOYSA-N Diammonium sulfite Chemical compound [NH4+].[NH4+].[O-]S([O-])=O PQUCIEFHOVEZAU-UHFFFAOYSA-N 0.000 claims description 8
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 8
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- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 2
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 239000010949 copper Substances 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 3
- MNCGMVDMOKPCSQ-UHFFFAOYSA-M sodium;2-phenylethenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C=CC1=CC=CC=C1 MNCGMVDMOKPCSQ-UHFFFAOYSA-M 0.000 abstract description 2
- 239000001509 sodium citrate Substances 0.000 description 12
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 12
- 229920001467 poly(styrenesulfonates) Polymers 0.000 description 8
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
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- MAGFQRLKWCCTQJ-UHFFFAOYSA-N 4-ethenylbenzenesulfonic acid Chemical compound OS(=O)(=O)C1=CC=C(C=C)C=C1 MAGFQRLKWCCTQJ-UHFFFAOYSA-N 0.000 description 1
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- D06M11/83—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 metals; with metal-generating compounds, e.g. metal carbonyls; Reduction of metal compounds on textiles
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- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
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- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
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- 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 Table; Ferrates; Cobaltates; Nickelates; Ruthenates; Osmates; Rhodates; Iridates; Palladates; Platinates
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- 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
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- D06M2101/16—Synthetic fibres, other than mineral fibres
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Abstract
本发明公开了一种阻燃耐寒防割屏蔽多频谱面料及其制备方法。取1414对位芳纶纤维、阻燃涤纶纤维、316L不锈钢纤维、镀银阻燃改性PPS纤维、镀铜尼龙66纤维、石墨烯改性聚四氟乙烯短纤,纺丝,编制,得到面料,在面料上依次涂覆Ti3C2Tx分散液、GO‑Fe3O4聚氨酯树脂复合溶液,制得一种阻燃耐寒防割屏蔽多频谱面料。Ti3C2Tx分散液具有优异的屏蔽多频谱的效果,对苯乙烯磺酸钠电化学剥离的石墨烯纳米片结构更稳定,具有更多的活性位点,可以复合更多的Fe3O4纳米粒子,提高材料的屏蔽多频谱性能。
Description
技术领域
本发明涉及面料技术领域,具体为一种阻燃耐寒防割屏蔽多频谱面料及其制备方法。
背景技术
随着工业技术的高速发展和人们生活水平的不断提高,电磁技术得到了广泛应用,在丰富人们日常生活的同时,也带来了严重的电磁辐射问题,如果对有害的电磁波接触时间过长,人的身体健康会受到伤害,影响人们正常生活,同时传递信息的电磁波在传输过程中有泄露的风险,带来的信息泄露问题会对个人信息安全,电磁辐射渗透到人类生活的方方面面,为了尽可能减少其对人体的伤害,对屏蔽多频谱面有更高的要求。
电磁波在传播过程中会产生无形的磁场和电场。当电磁波遇到特殊介质时,会产生吸收、反射反应,如果介质具有良好的磁性和导电性,会利于介质对电磁波的吸收和反射,因此,电磁屏蔽材料需要有良好的导电性,以此实现对电磁波的介电损耗,使得让辐射过来的电磁波在传播过程中衰弱,同时屏蔽多频谱面料中性能优异的磁性物质能增强对电磁波的磁损耗以便于吸收电磁波。
与此同时,在要求面料具有屏蔽多频谱的功能的同时,还需要面料有其他的性能,如:阻燃、耐寒、防割,以此来满足其在苛刻环境的应用。
为了解决上述问题,本发明提供了一种阻燃耐寒防割屏蔽多频谱面料及其制备方法,在具有优异的屏蔽多频谱功能的同时,还具有优良的阻燃、耐寒、防割性能,使得以此方法生产的面料能满足严苛环境中的应用。
发明内容
本发明的目的在于提供一种阻燃耐寒防割屏蔽多频谱面料及其制备方法,以解决上述背景技术中提出的问题。
为了解决上述技术问题,本发明提供如下技术方案:
一种阻燃耐寒防割屏蔽多频谱面料的制备方法,其特征在于:
步骤一:取KOH、硝酸银溶液,滴加氨水,至沉淀消失,加入乙醇稳定剂,搅拌均匀,制得镀银液;取葡萄糖、酒石酸、去离子水,搅拌均匀,制得还原剂溶液;
将预处理后的PPS纤维置于镀银液中反应10-20min,加入还原液,在30-50℃下搅拌,取出PPS纤维,清洗,烘干,制得镀银阻燃改性PPS纤维;
步骤二:取去离子水、硫酸铜、甲醛搅拌均匀,搅拌均匀,得到组份A;取酒石酸钾钠、乙二胺四乙酸、氢氧化钠、氯化镍、氰化钾、渗透剂JFC,搅拌均匀,加入组份A,加入预处理后的尼龙66纤维,在50-70℃下搅拌,加入α,α’-联吡啶,搅拌,制得镀铜尼龙66纤维;
步骤三:取聚四氟乙烯树脂,混合均匀,加入石墨烯,混合30-40min,静置58-60h,塑化9-10h,得到塑化后的混合料,压制成坯料,挤出,牵伸,静电处理,烘干,制得石墨烯改性聚四氟乙烯短纤;
步骤四:取1414对位芳纶纤维、阻燃涤纶纤维、316L不锈钢纤维、镀银阻燃改性PPS纤维、镀铜尼龙66纤维、石墨烯改性聚四氟乙烯短纤,纺丝,编制,得到面料,在面料表面涂布Ti3C2Tx分散液,晾干1-2h,涂布GO-Fe3O4聚氨酯树脂复合溶液,引入水平的磁场,磁场强度为220-240mT,在55-65℃下烘干10-12h,得到阻燃耐寒防割屏蔽多频谱面料。
较为优化地,面料包括以下成分:按照百分比计,18-20%的1414对位芳纶纤维、18-20%的阻燃涤纶纤维、30-32%的316L不锈钢纤维、8%-10%的镀银阻燃改性PPS纤维、14-16%的镀铜尼龙66纤维、6-8%的石墨烯改性聚四氟乙烯短纤。
较为优化地,其特征在于:预处理后的PPS纤维的制备方法为:将PPS纤维置于丙酮中浸泡22-24h,洗涤,烘干,在45g/L的KOH中浸泡1-2h,取出,置于0.1mol/L硝酸溶液中浸泡10-20min,取出,置于15g/L的氯化亚锡和质量分数为2%的盐酸配制的混合液中浸泡5-7min,烘干,置于30g/L的的次亚磷酸钠溶液中浸泡2-3min,烘干,得到预处理过的PPS纤维;
预处理后的尼龙66纤维的制备方法为:取尼龙66纤维置于氢氧化钠溶液中22-24h,取出,置于氯化钯、聚氨酯、烷基苯磺酸钠混合物中浸渍2-3h,取出,置于甲醛溶液中浸泡20-30min,烘干,得到预处理后的尼龙66纤维。
较为优化地,步骤四中,步骤四中,在面料表面涂布Ti3C2Tx分散液,晾干1-2h,涂布GO-Fe3O4聚氨酯树脂复合溶液,引入水平的磁场,磁场强度为220-240mT,在55-65℃下烘干10-12h;
Ti3C2Tx分散液的制备方法为:取氟化锂、盐酸搅拌均匀,加入Ti3AlC2粉末,在40-42℃下搅拌反应44-50h,洗涤,在-2-2℃下超声30-40min,离心,加入1000ml去离子水,搅拌均匀,得到Ti3C2Tx分散液。
较为优化地,步骤四中,GO-Fe3O4聚氨酯树脂复合溶液的制备方法为:取聚氨酯树脂、2-丁酮,混合均匀,得到聚氨酯树脂乳液;取GO-Fe3O4复合材料、N-甲基吡咯烷酮,超声分散1-2h,加入聚氨酯树脂乳液、甲苯二异氰酸酯三聚体,超声分散1-2h,得到GO-Fe3O4聚氨酯树脂复合溶液。
较为优化地,步骤四中,Ti3C2Tx分散液与GO-Fe3O4聚氨酯树脂复合溶液的质量比为1.0:(1.2-1.4)。
较为优化地,GO-Fe3O4复合材料的制备方法为:取聚苯乙烯磺酸钠修饰的石墨烯纳米片、乙二醇,加入四氧化三铁纳米粒子、尿素,滴加聚乙二醇400,搅拌30-40min,在180-200℃下反应7-9h,冷却,洗涤,烘干,得到GO-Fe3O4复合材料。
较为优化地,聚苯乙烯磺酸钠修饰的石墨烯纳米片的制备方法为:取对苯乙烯磺酸钠、去离子水,搅拌均匀,得到对苯乙烯磺酸钠溶液;取石墨箔作为阳极,铂电极作为阴极,阳极与阴极之间的间隔为1-2cm,电压为14-16V,平行放置于对苯乙烯磺酸钠溶液中6-8h;加入过硫酸铵、亚硫酸铵,超声分散2-3h,过滤,收集悬浮物,洗涤,干燥,得到聚苯乙烯磺酸钠修饰的石墨烯纳米片。
与现有技术相比,本发明所达到的有益效果是:
(1)芳纶布纤维断裂伸长大、高韧性、耐剪切性能好,具有优良的尺寸稳定性能、热收缩率低、耐酸碱性能好、阻燃性能好,不会因使用时间和洗涤次数的增加而降低或丧失阻燃性能,将芳纶布作为面料基底,可以使得面料具有耐割、阻燃的性能。
使用氟化锂和盐酸合成HF刻蚀Ti3AlC2,得到Ti3C2Tx,Li+在刻蚀中起插层作用,增大了Ti3C2Tx的层间距,便于后续的超声剥离。
先在芳纶布上涂布Ti3C2Tx纳米片,大片层的Ti3C2Tx能包裹在芳纶纤维表面,使得每根芳纶纤维都成为导电体,相互连接以此形成良好的导电通路,Ti3C2Tx屏蔽多频谱芳纶布具有高电磁波吸收性能,以此来达到电磁干扰屏蔽效果,提高了面料的屏蔽多频谱性能。
(2)使用电化学方法对石墨烯进行剥离,将其置于对苯乙烯磺酸钠溶液中,对苯乙烯磺酸阴离子插入到石墨层之间的空间中,扩大了相邻石墨烯的片层间间距,石墨烯片层间的范德华力不足以维持其以平行的方式相连,最终相互分离,得到了被剥离的石墨烯纳米片。对苯乙烯磺酸上的双键与氧自由基反应从而减少了石墨烯被氧化的程度,因此对苯乙烯磺酸钠电化学剥离的石墨烯纳米片氧化程度低,石墨烯片层上的缺陷较少,分散良好,因此得到的石墨烯片层结构更稳定,而且不容易被破坏,而且具有更多的活性位点,可以复合更多的Fe3O4纳米粒子。
在燃烧过程中,对苯乙烯磺酸钠电化学剥离的石墨烯纳米片片层会阻碍氧气和热解产物在聚合物内部的传输,阻挡挥发热解产物,聚集沉淀形成炭层,由此隔离氧气和低分子量的可燃热解产物,从而提升了面料的阻燃性。
使用Fe3O4纳米粒子对由对苯乙烯磺酸钠电化学剥离的石墨烯纳米片进行复合,Fe3O4纳米粒子有着屏蔽多频谱的功能,与Ti3C2Tx相互配合,增强了面料的屏蔽多频谱功能。涂布GO-Fe3O4聚氨酯树脂复合溶液,并引入水平的磁场,使得氧化石墨烯在芳纶布表面排布地更均匀,使得面料的屏蔽性能更稳定。
并将GO-Fe3O4复合材料加入耐寒聚氨酯树脂中,形成复合溶液,涂布在芳纶布上提高面料的阻燃、耐寒性能。在涂布有Ti3C2Tx分散液的芳纶布上涂覆GO-Fe3O4聚氨酯树脂复合溶液,两者相互交联,提升了涂层之间的结合力,使其能更好地粘附在芳纶布上。
具体实施方式
下面将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。
实施例1
步骤一:将PPS纤维置于丙酮中浸泡23h,洗涤,烘干,在45g/L的KOH中浸泡1.5h,取出,置于0.1mol/L硝酸溶液中浸泡15min,取出,置于15g/L的氯化亚锡和质量分数为2%的盐酸配制的混合液中浸泡6min,烘干,置于30g/L的的次亚磷酸钠溶液中浸泡2.5min,烘干,得到预处理后的PPS纤维;
取2.6gKOH、400ml硝酸银溶液,滴加氨水,至沉淀消失,加入3g乙醇稳定剂,制得镀银液;取3.3g葡萄糖、1g酒石酸、400ml去离子水,搅拌均匀,制得还原剂溶液;
将预处理后的PPS纤维置于镀银液中反应15min,加入还原液,在40℃下搅拌,取出PPS纤维,清洗,烘干,制得镀银阻燃改性PPS纤维;
步骤二:取尼龙66纤维置于氢氧化钠溶液中23h,取出,置于氯化钯、聚氨酯、烷基苯磺酸钠混合物中浸渍2.5h,取出,置于甲醛溶液中浸泡25min,取出;
取800ml去离子水、16g硫酸铜、15g甲醛搅拌均匀,搅拌均匀,得到组份A;取15g酒石酸钾钠、22g乙二胺四乙酸、7g氢氧化钠、1g氯化镍、10mg氰化钾、3g渗透剂JFC,搅拌均匀,加入组份A,加入尼龙66纤维,在60℃下搅拌,加入20mgα,α’-联吡啶,搅拌,制得镀铜尼龙66纤维;
步骤三:取聚四氟乙烯树脂,混合均匀,加入石墨烯,混合35min,静置59h,塑化9.5h,得到塑化后的混合料,压制成坯料,挤出,牵伸,静电处理,烘干,制得石墨烯改性聚四氟乙烯短纤;
步骤四:取1414对位芳纶纤维、阻燃涤纶纤维、316L不锈钢纤维、镀银阻燃改性PPS纤维、镀铜尼龙66纤维、石墨烯改性聚四氟乙烯短纤,纺丝,编制,得到面料。
面料包括以下成分:按照百分比计,19%的1414对位芳纶纤维、19%的阻燃涤纶纤维、31%的316L不锈钢纤维、9%的镀银阻燃改性PPS纤维、15%的镀铜尼龙66纤维、7%的石墨烯改性聚四氟乙烯短纤。
1414对位芳纶纤维购自烟台泰和,阻燃涤纶纤维购自四川东材,316L不锈钢纤维购自湖南惠同。
实施例2
步骤一:将PPS纤维置于丙酮中浸泡22h,洗涤,烘干,在45g/L的KOH中浸泡1h,取出,置于0.1mol/L硝酸溶液中浸泡10min,取出,置于15g/L的氯化亚锡和质量分数为2%的盐酸配制的混合液中浸泡5min,烘干,置于30g/L的的次亚磷酸钠溶液中浸泡2min,烘干,得到预处理后的PPS纤维;
取2.6gKOH、400ml硝酸银溶液,滴加氨水,至沉淀消失,加入3g乙醇稳定剂,制得镀银液;取3.3g葡萄糖、1g酒石酸、400ml去离子水,制得还原剂溶液;
将预处理后的PPS纤维置于镀银液中反应10min,加入还原液,在30℃下搅拌,取出PPS纤维,清洗,烘干,制得镀银阻燃改性PPS纤维;
步骤二:取尼龙66纤维置于氢氧化钠溶液中22h,取出,置于氯化钯、聚氨酯、烷基苯磺酸钠混合物中浸渍2h,取出,置于甲醛溶液中浸泡20min,取出;
取800ml去离子水、16g硫酸铜、15g甲醛搅拌均匀,搅拌均匀,得到组份A;取15g酒石酸钾钠、22g乙二胺四乙酸、7g氢氧化钠、1g氯化镍、10mg氰化钾、3g渗透剂JFC,搅拌均匀,加入组份A,加入尼龙66纤维,在50℃下搅拌,加入20mgα,α’-联吡啶,制得镀铜尼龙66纤维;
步骤三:取聚四氟乙烯树脂,混合均匀,加入石墨烯,混合30min,静置58h,塑化9h,得到塑化后的混合料,压制成坯料,挤出,牵伸,静电处理,烘干,制得石墨烯改性聚四氟乙烯短纤;
步骤四:取1414对位芳纶纤维、阻燃涤纶纤维、316L不锈钢纤维、镀银阻燃改性PPS纤维、镀铜尼龙66纤维、石墨烯改性聚四氟乙烯短纤,纺丝,编制,得到面料,在面料表面涂布Ti3C2Tx分散液,晾干1h,涂布GO-Fe3O4聚氨酯树脂复合溶液,引入水平的磁场,磁场强度为220mT,在55℃下烘干10h,得到阻燃耐寒防割屏蔽多频谱面料;
面料包括以下成分:按照百分比计,20%的1414对位芳纶纤维、20%的阻燃涤纶纤维、30%的316L不锈钢纤维、10%的镀银阻燃改性PPS纤维、14%的镀铜尼龙66纤维、6%的石墨烯改性聚四氟乙烯短纤。
1414对位芳纶纤维购自烟台泰和,阻燃涤纶纤维购自四川东材,316L不锈钢纤维购自湖南惠同。
实施例3
步骤一:将PPS纤维置于丙酮中浸泡24h,洗涤,烘干,在45g/L的KOH中浸泡2h,取出,置于0.1mol/L硝酸溶液中浸泡20min,取出,置于15g/L的氯化亚锡和质量分数为2%的盐酸配制的混合液中浸泡7min,烘干,置于30g/L的的次亚磷酸钠溶液中浸泡3min,烘干,得到预处理后的PPS纤维;
取2.6gKOH、400ml硝酸银溶液,滴加氨水,至沉淀消失,加入3g乙醇稳定剂,制得镀银液;取3.3g葡萄糖、1g酒石酸、400ml去离子水,制得还原剂溶液;
将预处理后的PPS纤维置于镀银液中反应20min,加入还原液,在50℃下搅拌,取出PPS纤维,清洗,烘干,制得镀银阻燃改性PPS纤维;
步骤二:取尼龙66纤维置于氢氧化钠溶液中24h,取出,置于氯化钯、聚氨酯、烷基苯磺酸钠混合物中浸渍3h,取出,置于甲醛溶液中浸泡30min,取出;
取800ml去离子水、16g硫酸铜、15g甲醛搅拌均匀,搅拌均匀,得到组份A;取15g酒石酸钾钠、22g乙二胺四乙酸、7g氢氧化钠、1g氯化镍、10mg氰化钾、3g渗透剂JFC,搅拌均匀,加入组份A,加入尼龙66纤维,在70℃下搅拌,加入20mgα,α’-联吡啶,制得镀铜尼龙66纤维;
步骤三:取聚四氟乙烯树脂,混合均匀,加入石墨烯,混合40min,静置60h,塑化10h,得到塑化后的混合料,压制成坯料,挤出,牵伸,静电处理,烘干,制得石墨烯改性聚四氟乙烯短纤;
步骤四:取1414对位芳纶纤维、阻燃涤纶纤维、316L不锈钢纤维、镀银阻燃改性PPS纤维、镀铜尼龙66纤维、石墨烯改性聚四氟乙烯短纤,纺丝,编制,得到面料,在面料表面涂布Ti3C2Tx分散液,晾干2h,涂布GO-Fe3O4聚氨酯树脂复合溶液,引入水平的磁场,磁场强度为240mT,在65℃下烘干12h,得到阻燃耐寒防割屏蔽多频谱面料;
面料包括以下成分:按照百分比计,20%的1414对位芳纶纤维、19%的阻燃涤纶纤维、30%的316L不锈钢纤维、8%的镀银阻燃改性PPS纤维、15%的镀铜尼龙66纤维、8%的石墨烯改性聚四氟乙烯短纤。
1414对位芳纶纤维购自烟台泰和,阻燃涤纶纤维购自四川东材,316L不锈钢纤维购自湖南惠同。
实施例4
步骤一:制备Ti3C2Tx分散液
取3g氟化锂、45ml盐酸搅拌均匀,加入Ti3AlC2粉末,在41℃下搅拌反应47h,洗涤,在0℃下超声35min,离心,加入1000ml去离子水,搅拌均匀,得到Ti3C2Tx分散液。
步骤二:制备聚苯乙烯磺酸钠修饰的石墨烯纳米片
取5g对苯乙烯磺酸钠、500ml去离子水,搅拌均匀,得到对苯乙烯磺酸钠溶液;取石墨箔作为阳极,铂电极作为阴极,平行放置于对苯乙烯磺酸钠溶液中7h,阳极与阴极之间的间隔为1.5cm,电压为15V;加入10g过硫酸铵、7g亚硫酸铵,超声分散2.5h,过滤,收集悬浮物,洗涤,干燥,得到聚苯乙烯磺酸钠修饰的石墨烯纳米片。
步骤三:取FeCl3·6H2O、FeCl2·4H2O、去离子水混合均匀,加入氨水,在68℃下搅拌35min,加入枸橼酸钠,在40℃下搅拌2.5h,用磁铁吸引分离,洗涤,烘干,得到四氧化三铁纳米粒子;
四氧化三铁纳米粒子包括以下成分:按照重量计,13份FeCl3·6H2O、15份FeCl2·4H2O、22份去离子水、15份氨水、11份枸橼酸钠。
取3g聚苯乙烯磺酸钠修饰的石墨烯纳米片、20ml乙二醇,加入12g四氧化三铁纳米粒子、20g尿素,滴加30ml聚乙二醇400,搅拌35min,在190℃下反应8h,冷却,洗涤,烘干,得到GO-Fe3O4复合材料;
取21g聚氨酯树脂、15ml2-丁酮,混合均匀,得到聚氨酯树脂乳液,取5gGO-Fe3O4复合材料、20mlN-甲基吡咯烷酮,超声分散1.5h,加入聚氨酯树脂乳液、8.2g甲苯二异氰酸酯三聚体,超声分散1.5h,得到GO-Fe3O4聚氨酯树脂复合溶液。
步骤四:将PPS纤维置于丙酮中浸泡23h,洗涤,烘干,在45g/L的KOH中浸泡1.5h,取出,置于0.1mol/L硝酸溶液中浸泡15min,取出,置于15g/L的氯化亚锡和质量分数为2%的盐酸配制的混合液中浸泡6min,烘干,置于30g/L的的次亚磷酸钠溶液中浸泡2.5min,烘干,得到预处理后的PPS纤维;
取2.6gKOH、400ml硝酸银溶液,滴加氨水,至沉淀消失,加入3g乙醇稳定剂,制得镀银液;取3.3g葡萄糖、1g酒石酸、400ml去离子水,制得还原剂溶液;
将预处理后的PPS纤维置于镀银液中反应15min,加入还原液,在40℃下搅拌,取出PPS纤维,清洗,烘干,制得镀银阻燃改性PPS纤维;
步骤五:取尼龙66纤维置于氢氧化钠溶液中23h,取出,置于氯化钯、聚氨酯、烷基苯磺酸钠混合物中浸渍2.5h,取出,置于甲醛溶液中浸泡25min,取出;
取800ml去离子水、16g硫酸铜、15g甲醛搅拌均匀,搅拌均匀,得到组份A;取15g酒石酸钾钠、22g乙二胺四乙酸、7g氢氧化钠、1g氯化镍、10mg氰化钾、3g渗透剂JFC,搅拌均匀,加入组份A,加入尼龙66纤维,在60℃下搅拌,加入20mgα,α’-联吡啶,搅拌,制得镀铜尼龙66纤维;
步骤六:取聚四氟乙烯树脂,混合均匀,加入石墨烯,混合35min,静置59h,塑化9.5h,得到塑化后的混合料,压制成坯料,挤出,牵伸,静电处理,烘干,制得石墨烯改性聚四氟乙烯短纤;
步骤七:取1414对位芳纶纤维、阻燃涤纶纤维、316L不锈钢纤维、镀银阻燃改性PPS纤维、镀铜尼龙66纤维、石墨烯改性聚四氟乙烯短纤,纺丝,编制,得到面料,在面料表面涂布Ti3C2Tx分散液,晾干1.5h,涂布GO-Fe3O4聚氨酯树脂复合溶液,引入水平的磁场,磁场强度为230mT,在60℃下烘干11h,得到阻燃耐寒防割屏蔽多频谱面料;
面料包括以下成分:按照百分比计,19%的1414对位芳纶纤维、19%的阻燃涤纶纤维、31%的316L不锈钢纤维、9%的镀银阻燃改性PPS纤维、15%的镀铜尼龙66纤维、7%的石墨烯改性聚四氟乙烯短纤。
Ti3C2Tx分散液的涂布量为20g/m2;GO-Fe3O4聚氨酯树脂复合溶液的涂布量为26g/m2。
实施例5
步骤一:制备Ti3C2Tx分散液
取3g氟化锂、45ml盐酸搅拌均匀,加入Ti3AlC2粉末,在40℃下搅拌反应44h,洗涤,在-2℃下超声30min,离心,加入1000ml去离子水,搅拌均匀,得到Ti3C2Tx分散液。
步骤二:制备聚苯乙烯磺酸钠修饰的石墨烯纳米片
取5g对苯乙烯磺酸钠、500ml去离子水,搅拌均匀,得到对苯乙烯磺酸钠溶液;取石墨箔作为阳极,铂电极作为阴极,平行放置于对苯乙烯磺酸钠溶液中6h,阳极与阴极之间的间隔为1cm,电压为14V;加入10g过硫酸铵、7g亚硫酸铵,超声分散2h,过滤,收集悬浮物,洗涤,干燥,得到聚苯乙烯磺酸钠修饰的石墨烯纳米片。
步骤三:取FeCl3·6H2O、FeCl2·4H2O、去离子水混合均匀,加入氨水,在66℃下搅拌30min,加入枸橼酸钠,在38℃下搅拌2h,用磁铁吸引分离,洗涤,烘干,得到四氧化三铁纳米粒子;
四氧化三铁纳米粒子包括以下成分:按照重量计,10份FeCl3·6H2O、10份FeCl2·4H2O、15份去离子水、10份氨水、8份枸橼酸钠。
取3g聚苯乙烯磺酸钠修饰的石墨烯纳米片、20ml乙二醇,加入12g四氧化三铁纳米粒子、20g尿素,滴加30ml聚乙二醇400,搅拌30min,在180℃下反应7h,冷却,洗涤,烘干,得到GO-Fe3O4复合材料;
取21g聚氨酯树脂、15ml2-丁酮,混合均匀,得到聚氨酯树脂乳液,取5gGO-Fe3O4复合材料、20mlN-甲基吡咯烷酮,超声分散1h,加入聚氨酯树脂乳液、8.2g甲苯二异氰酸酯三聚体,超声分散1h,得到GO-Fe3O4聚氨酯树脂复合溶液。
步骤四:将PPS纤维置于丙酮中浸泡23h,洗涤,烘干,在45g/L的KOH中浸泡1h,取出,置于0.1mol/L硝酸溶液中浸泡10min,取出,置于15g/L的氯化亚锡和质量分数为2%的盐酸配制的混合液中浸泡5min,烘干,置于30g/L的的次亚磷酸钠溶液中浸泡2min,烘干,得到预处理后的PPS纤维;
取2.6gKOH、400ml硝酸银溶液,滴加氨水,至沉淀消失,加入3g乙醇稳定剂,制得镀银液;取3.3g葡萄糖、1g酒石酸、400ml去离子水,制得还原剂溶液;
将预处理后的PPS纤维置于镀银液中反应10min,加入还原液,在30℃下搅拌,取出PPS纤维,清洗,烘干,制得镀银阻燃改性PPS纤维;
步骤五:取尼龙66纤维置于氢氧化钠溶液中22h,取出,置于氯化钯、聚氨酯、烷基苯磺酸钠混合物中浸渍2h,取出,置于甲醛溶液中浸泡20min,取出;
取800ml去离子水、16g硫酸铜、15g甲醛搅拌均匀,搅拌均匀,得到组份A;取15g酒石酸钾钠、22g乙二胺四乙酸、7g氢氧化钠、1g氯化镍、10mg氰化钾、3g渗透剂JFC,搅拌均匀,加入组份A,加入尼龙66纤维,在50℃下搅拌,加入20mgα,α’-联吡啶,制得镀铜尼龙66纤维;
步骤六:取聚四氟乙烯树脂,混合均匀,加入石墨烯,混合30min,静置58h,塑化9h,得到塑化后的混合料,压制成坯料,挤出,牵伸,静电处理,烘干,制得石墨烯改性聚四氟乙烯短纤;
步骤七:取1414对位芳纶纤维、阻燃涤纶纤维、316L不锈钢纤维、镀银阻燃改性PPS纤维、镀铜尼龙66纤维、石墨烯改性聚四氟乙烯短纤,纺丝,编制,得到面料,在面料表面涂布Ti3C2Tx分散液,晾干1h,涂布GO-Fe3O4聚氨酯树脂复合溶液,引入水平的磁场,磁场强度为220mT,在55℃下烘干10h,得到阻燃耐寒防割屏蔽多频谱面料;
面料包括以下成分:按照百分比计,20%的1414对位芳纶纤维、20%的阻燃涤纶纤维、30%的316L不锈钢纤维、10%的镀银阻燃改性PPS纤维、14%的镀铜尼龙66纤维、6%的石墨烯改性聚四氟乙烯短纤。
Ti3C2Tx分散液的涂布量为20g/m2;GO-Fe3O4聚氨酯树脂复合溶液的涂布量为22g/m2。
实施例6
步骤一:制备Ti3C2Tx分散液
取3g氟化锂、45ml盐酸搅拌均匀,加入Ti3AlC2粉末,在42℃下搅拌反应50h,洗涤,在2℃下超声40min,离心,加入1000ml去离子水,搅拌均匀,得到Ti3C2Tx分散液。
步骤二:制备聚苯乙烯磺酸钠修饰的石墨烯纳米片
取5g对苯乙烯磺酸钠、500ml去离子水,搅拌均匀,得到对苯乙烯磺酸钠溶液;取石墨箔作为阳极,铂电极作为阴极,平行放置于对苯乙烯磺酸钠溶液中8h,阳极与阴极之间的间隔为2cm,电压为16V;加入10g过硫酸铵、7g亚硫酸铵,超声分散3h,过滤,收集悬浮物,洗涤,干燥,得到聚苯乙烯磺酸钠修饰的石墨烯纳米片。
步骤三:取FeCl3·6H2O、FeCl2·4H2O、去离子水混合均匀,加入氨水,在70℃下搅拌40min,加入枸橼酸钠,在42℃下搅拌3h,用磁铁吸引分离,洗涤,烘干,得到四氧化三铁纳米粒子;
四氧化三铁纳米粒子包括以下成分:按照重量计,15份FeCl3·6H2O、20份FeCl2·4H2O、30份去离子水、20份氨水、14份枸橼酸钠。
取3g聚苯乙烯磺酸钠修饰的石墨烯纳米片、20ml乙二醇,加入12g四氧化三铁纳米粒子、20g尿素,滴加30ml聚乙二醇400,搅拌40min,在200℃下反应9h,冷却,洗涤,烘干,得到GO-Fe3O4复合材料;
取21g聚氨酯树脂、15ml2-丁酮,混合均匀,得到聚氨酯树脂乳液,取5gGO-Fe3O4复合材料、20mlN-甲基吡咯烷酮,超声分散2h,加入聚氨酯树脂乳液、8.2g甲苯二异氰酸酯三聚体,超声分散2h,得到GO-Fe3O4聚氨酯树脂复合溶液。
步骤四:将PPS纤维置于丙酮中浸泡24h,洗涤,烘干,在45g/L的KOH中浸泡2h,取出,置于0.1mol/L硝酸溶液中浸泡20min,取出,置于15g/L的氯化亚锡和质量分数为2%的盐酸配制的混合液中浸泡7min,烘干,置于30g/L的的次亚磷酸钠溶液中浸泡3min,烘干,得到预处理后的PPS纤维;
取2.6gKOH、400ml硝酸银溶液,滴加氨水,至沉淀消失,加入3g乙醇稳定剂,制得镀银液;取3.3g葡萄糖、1g酒石酸、400ml去离子水,制得还原剂溶液;
将预处理后的PPS纤维置于镀银液中反应20min,加入还原液,在50℃下搅拌,取出PPS纤维,清洗,烘干,制得镀银阻燃改性PPS纤维;
步骤五:取尼龙66纤维置于氢氧化钠溶液中24h,取出,置于氯化钯、聚氨酯、烷基苯磺酸钠混合物中浸渍3h,取出,置于甲醛溶液中浸泡30min,取出;
取800ml去离子水、16g硫酸铜、15g甲醛搅拌均匀,搅拌均匀,得到组份A;取15g酒石酸钾钠、22g乙二胺四乙酸、7g氢氧化钠、1g氯化镍、10mg氰化钾、3g渗透剂JFC,搅拌均匀,加入组份A,加入尼龙66纤维,在70℃下搅拌,加入20mgα,α’-联吡啶,制得镀铜尼龙66纤维;
步骤六:取聚四氟乙烯树脂,混合均匀,加入石墨烯,混合40min,静置60h,塑化10h,得到塑化后的混合料,压制成坯料,挤出,牵伸,静电处理,烘干,制得石墨烯改性聚四氟乙烯短纤;
步骤七:取1414对位芳纶纤维、阻燃涤纶纤维、316L不锈钢纤维、镀银阻燃改性PPS纤维、镀铜尼龙66纤维、石墨烯改性聚四氟乙烯短纤,纺丝,编制,得到面料,在面料表面涂布Ti3C2Tx分散液,晾干2h,涂布GO-Fe3O4聚氨酯树脂复合溶液,引入水平的磁场,磁场强度为240mT,在65℃下烘干12h,得到阻燃耐寒防割屏蔽多频谱面料;
面料包括以下成分:按照百分比计,20%的1414对位芳纶纤维、19%的阻燃涤纶纤维、30%的316L不锈钢纤维、8%的镀银阻燃改性PPS纤维、15%的镀铜尼龙66纤维、8%的石墨烯改性聚四氟乙烯短纤。
Ti3C2Tx分散液的涂布量为20g/m2;GO-Fe3O4聚氨酯树脂复合溶液的涂布量为28g/m2。
实施例7:不涂布Ti3C2Tx纳米片,其余与实施例1相同。
步骤一:制备聚苯乙烯磺酸钠修饰的石墨烯纳米片
取5g对苯乙烯磺酸钠、500ml去离子水,搅拌均匀,得到对苯乙烯磺酸钠溶液;取石墨箔作为阳极,铂电极作为阴极,平行放置于对苯乙烯磺酸钠溶液中7h,阳极与阴极之间的间隔为1.5cm,电压为15V;加入10g过硫酸铵、7g亚硫酸铵,超声分散2.5h,过滤,收集悬浮物,洗涤,干燥,得到聚苯乙烯磺酸钠修饰的石墨烯纳米片。
步骤二:取FeCl3·6H2O、FeCl2·4H2O、去离子水混合均匀,加入氨水,在68℃下搅拌35min,加入枸橼酸钠,在40℃下搅拌2.5h,用磁铁吸引分离,洗涤,烘干,得到四氧化三铁纳米粒子;
四氧化三铁纳米粒子包括以下成分:按照重量计,13份FeCl3·6H2O、15份FeCl2·4H2O、22份去离子水、15份氨水、11份枸橼酸钠。
取3g聚苯乙烯磺酸钠修饰的石墨烯纳米片、20ml乙二醇,加入12g四氧化三铁纳米粒子、20g尿素,滴加30ml聚乙二醇400,搅拌35min,在190℃下反应8h,冷却,洗涤,烘干,得到GO-Fe3O4复合材料;
取21g聚氨酯树脂、15ml2-丁酮,混合均匀,得到聚氨酯树脂乳液,取5gGO-Fe3O4复合材料、20mlN-甲基吡咯烷酮,超声分散1.5h,加入聚氨酯树脂乳液、8.2g甲苯二异氰酸酯三聚体,超声分散1.5h,得到GO-Fe3O4聚氨酯树脂复合溶液。
步骤三:将PPS纤维置于丙酮中浸泡23h,洗涤,烘干,在45g/L的KOH中浸泡1.5h,取出,置于0.1mol/L硝酸溶液中浸泡15min,取出,置于15g/L的氯化亚锡和质量分数为2%的盐酸配制的混合液中浸泡6min,烘干,置于30g/L的的次亚磷酸钠溶液中浸泡2.5min,烘干,得到预处理后的PPS纤维;
取2.6gKOH、400ml硝酸银溶液,滴加氨水,至沉淀消失,加入3g乙醇稳定剂,制得镀银液;取3.3g葡萄糖、1g酒石酸、400ml去离子水,制得还原剂溶液;
将预处理后的PPS纤维置于镀银液中反应15min,加入还原液,在40℃下搅拌,取出PPS纤维,清洗,烘干,制得镀银阻燃改性PPS纤维;
步骤四:取尼龙66纤维置于氢氧化钠溶液中23h,取出,置于氯化钯、聚氨酯、烷基苯磺酸钠混合物中浸渍2.5h,取出,置于甲醛溶液中浸泡25min,取出;
取800ml去离子水、16g硫酸铜、15g甲醛搅拌均匀,搅拌均匀,得到组份A;取15g酒石酸钾钠、22g乙二胺四乙酸、7g氢氧化钠、1g氯化镍、10mg氰化钾、3g渗透剂JFC,搅拌均匀,加入组份A,加入尼龙66纤维,在60℃下搅拌,加入20mgα,α’-联吡啶,搅拌,制得镀铜尼龙66纤维;
步骤五:取聚四氟乙烯树脂,混合均匀,加入石墨烯,混合35min,静置59h,塑化9.5h,得到塑化后的混合料,压制成坯料,挤出,牵伸,静电处理,烘干,制得石墨烯改性聚四氟乙烯短纤;
步骤六:取1414对位芳纶纤维、阻燃涤纶纤维、316L不锈钢纤维、镀银阻燃改性PPS纤维、镀铜尼龙66纤维、石墨烯改性聚四氟乙烯短纤,纺丝,编制,得到面料,在面料表面涂布GO-Fe3O4聚氨酯树脂复合溶液,引入水平的磁场,磁场强度为230mT,在60℃下烘干11h,得到阻燃耐寒防割屏蔽多频谱面料;
面料包括以下成分:按照百分比计,19%的1414对位芳纶纤维、19%的阻燃涤纶纤维、31%的316L不锈钢纤维、9%的镀银阻燃改性PPS纤维、15%的镀铜尼龙66纤维、7%的石墨烯改性聚四氟乙烯短纤。
GO-Fe3O4聚氨酯树脂复合溶液的涂布量为26g/m2。
实施例8:不对石墨烯纳米片进行修饰,其余与实施例1相同。
步骤一:制备Ti3C2Tx分散液
取3g氟化锂、45ml盐酸搅拌均匀,加入Ti3AlC2粉末,在41℃下搅拌反应47h,洗涤,在0℃下超声35min,离心,加入1000ml去离子水,搅拌均匀,得到Ti3C2Tx分散液。
步骤二:取FeCl3·6H2O、FeCl2·4H2O、去离子水混合均匀,加入氨水,在68℃下搅拌35min,加入枸橼酸钠,在40℃下搅拌2.5h,用磁铁吸引分离,洗涤,烘干,得到四氧化三铁纳米粒子;
四氧化三铁纳米粒子包括以下成分:按照重量计,13份FeCl3·6H2O、15份FeCl2·4H2O、22份去离子水、15份氨水、11份枸橼酸钠。
取3g石墨烯纳米片、20ml乙二醇,加入12g四氧化三铁纳米粒子、20g尿素,滴加30ml聚乙二醇400,搅拌35min,在190℃下反应8h,冷却,洗涤,烘干,得到GO-Fe3O4复合材料;
取21g聚氨酯树脂、15ml2-丁酮,混合均匀,得到聚氨酯树脂乳液,取5gGO-Fe3O4复合材料、20mlN-甲基吡咯烷酮,超声分散1.5h,加入聚氨酯树脂乳液、8.2g甲苯二异氰酸酯三聚体,超声分散1.5h,得到GO-Fe3O4聚氨酯树脂复合溶液。
步骤四:在芳纶布表面涂布Ti3C2Tx分散液,晾干1.5h,涂布GO-Fe3O4聚氨酯树脂复合溶液,引入水平的磁场,磁场强度为235mT,在60℃下烘干11h,冷却,得到阻燃耐寒防割屏蔽多频谱面料。
步骤五:将PPS纤维置于丙酮中浸泡23h,洗涤,烘干,在45g/L的KOH中浸泡1.5h,取出,置于0.1mol/L硝酸溶液中浸泡15min,取出,置于15g/L的氯化亚锡和质量分数为2%的盐酸配制的混合液中浸泡6min,烘干,置于30g/L的的次亚磷酸钠溶液中浸泡2.5min,烘干,得到预处理后的PPS纤维;
取2.6gKOH、400ml硝酸银溶液,滴加氨水,至沉淀消失,加入3g乙醇稳定剂,制得镀银液;取3.3g葡萄糖、1g酒石酸、400ml去离子水,制得还原剂溶液;
将预处理后的PPS纤维置于镀银液中反应15min,加入还原液,在40℃下搅拌,取出PPS纤维,清洗,烘干,制得镀银阻燃改性PPS纤维;
步骤六:取尼龙66纤维置于氢氧化钠溶液中23h,取出,置于氯化钯、聚氨酯、烷基苯磺酸钠混合物中浸渍2.5h,取出,置于甲醛溶液中浸泡25min,取出;
取800ml去离子水、16g硫酸铜、15g甲醛搅拌均匀,搅拌均匀,得到组份A;取15g酒石酸钾钠、22g乙二胺四乙酸、7g氢氧化钠、1g氯化镍、10mg氰化钾、3g渗透剂JFC,搅拌均匀,加入组份A,加入尼龙66纤维,在60℃下搅拌,加入20mgα,α’-联吡啶,搅拌,制得镀铜尼龙66纤维;
步骤七:取聚四氟乙烯树脂,混合均匀,加入石墨烯,混合35min,静置59h,塑化9.5h,得到塑化后的混合料,压制成坯料,挤出,牵伸,静电处理,烘干,制得石墨烯改性聚四氟乙烯短纤;
步骤八:取1414对位芳纶纤维、阻燃涤纶纤维、316L不锈钢纤维、镀银阻燃改性PPS纤维、镀铜尼龙66纤维、石墨烯改性聚四氟乙烯短纤,纺丝,编制,得到面料,在面料表面涂布Ti3C2Tx分散液,晾干1.5h,涂布GO-Fe3O4聚氨酯树脂复合溶液,引入水平的磁场,磁场强度为230mT,在60℃下烘干11h,得到阻燃耐寒防割屏蔽多频谱面料;
面料包括以下成分:按照百分比计,19%的1414对位芳纶纤维、19%的阻燃涤纶纤维、31%的316L不锈钢纤维、9%的镀银阻燃改性PPS纤维、15%的镀铜尼龙66纤维、7%的石墨烯改性聚四氟乙烯短纤。
Ti3C2Tx分散液的涂布量为20g/m2;GO-Fe3O4聚氨酯树脂复合溶液的涂布量为26g/m2。
实施例9:不在石墨烯纳米片上复合四氧化三铁纳米粒子,其余与实施例1相同。
步骤一:制备Ti3C2Tx分散液
取3g氟化锂、45ml盐酸搅拌均匀,加入Ti3AlC2粉末,在41℃下搅拌反应47h,洗涤,在0℃下超声35min,离心,加入1000ml去离子水,搅拌均匀,得到Ti3C2Tx分散液。
步骤二:制备聚苯乙烯磺酸钠修饰的石墨烯纳米片
取5g对苯乙烯磺酸钠、500ml去离子水,搅拌均匀,得到对苯乙烯磺酸钠溶液;取石墨箔作为阳极,铂电极作为阴极,平行放置于对苯乙烯磺酸钠溶液中7h,阳极与阴极之间的间隔为1.5cm,电压为15V;加入10g过硫酸铵、7g亚硫酸铵,超声分散2.5h,过滤,收集悬浮物,洗涤,干燥,得到聚苯乙烯磺酸钠修饰的石墨烯纳米片。
步骤三:取21g聚氨酯树脂、15ml2-丁酮,混合均匀,得到聚氨酯树脂乳液,取5g聚苯乙烯磺酸钠修饰的石墨烯纳米片、20mlN-甲基吡咯烷酮,超声分散1.5h,加入聚氨酯树脂乳液、8.2g甲苯二异氰酸酯三聚体,超声分散1.5h,得到石墨烯聚氨酯树脂复合溶液。
步骤四:将PPS纤维置于丙酮中浸泡23h,洗涤,烘干,在45g/L的KOH中浸泡1.5h,取出,置于0.1mol/L硝酸溶液中浸泡15min,取出,置于15g/L的氯化亚锡和质量分数为2%的盐酸配制的混合液中浸泡6min,烘干,置于30g/L的的次亚磷酸钠溶液中浸泡2.5min,烘干,得到预处理后的PPS纤维;
取2.6gKOH、400ml硝酸银溶液,滴加氨水,至沉淀消失,加入3g乙醇稳定剂,制得镀银液;取3.3g葡萄糖、1g酒石酸、400ml去离子水,制得还原剂溶液;
将预处理后的PPS纤维置于镀银液中反应15min,加入还原液,在40℃下搅拌,取出PPS纤维,清洗,烘干,制得镀银阻燃改性PPS纤维;
步骤五:取尼龙66纤维置于氢氧化钠溶液中23h,取出,置于氯化钯、聚氨酯、烷基苯磺酸钠混合物中浸渍2.5h,取出,置于甲醛溶液中浸泡25min,取出;
取800ml去离子水、16g硫酸铜、15g甲醛搅拌均匀,搅拌均匀,得到组份A;取15g酒石酸钾钠、22g乙二胺四乙酸、7g氢氧化钠、1g氯化镍、10mg氰化钾、3g渗透剂JFC,搅拌均匀,加入组份A,加入尼龙66纤维,在60℃下搅拌,加入20mgα,α’-联吡啶,搅拌,制得镀铜尼龙66纤维;
步骤六:取聚四氟乙烯树脂,混合均匀,加入石墨烯,混合35min,静置59h,塑化9.5h,得到塑化后的混合料,压制成坯料,挤出,牵伸,静电处理,烘干,制得石墨烯改性聚四氟乙烯短纤;
步骤七:取1414对位芳纶纤维、阻燃涤纶纤维、316L不锈钢纤维、镀银阻燃改性PPS纤维、镀铜尼龙66纤维、石墨烯改性聚四氟乙烯短纤,纺丝,编制,得到面料,在面料表面涂布Ti3C2Tx分散液,晾干1.5h,涂布GO-Fe3O4聚氨酯树脂复合溶液,引入水平的磁场,磁场强度为230mT,在60℃下烘干11h,得到阻燃耐寒防割屏蔽多频谱面料;
面料包括以下成分:按照百分比计,19%的1414对位芳纶纤维、19%的阻燃涤纶纤维、31%的316L不锈钢纤维、9%的镀银阻燃改性PPS纤维、15%的镀铜尼龙66纤维、7%的石墨烯改性聚四氟乙烯短纤。
Ti3C2Tx分散液的涂布量为20g/m2;GO-Fe3O4聚氨酯树脂复合溶液的涂布量为26g/m2。
实施例10:Ti3C2Tx分散液与GO-Fe3O4聚氨酯树脂复合溶液的质量比为0.8:1.3,其余与实施例1相同。
步骤一:制备Ti3C2Tx分散液
取3g氟化锂、45ml盐酸搅拌均匀,加入Ti3AlC2粉末,在41℃下搅拌反应47h,洗涤,在0℃下超声35min,离心,加入1000ml去离子水,搅拌均匀,得到Ti3C2Tx分散液。
步骤二:制备聚苯乙烯磺酸钠修饰的石墨烯纳米片
取5g对苯乙烯磺酸钠、500ml去离子水,搅拌均匀,得到对苯乙烯磺酸钠溶液;取石墨箔作为阳极,铂电极作为阴极,平行放置于对苯乙烯磺酸钠溶液中7h,阳极与阴极之间的间隔为1.5cm,电压为15V;加入10g过硫酸铵、7g亚硫酸铵,超声分散2.5h,过滤,收集悬浮物,洗涤,干燥,得到聚苯乙烯磺酸钠修饰的石墨烯纳米片。
步骤三:取FeCl3·6H2O、FeCl2·4H2O、去离子水混合均匀,加入氨水,在68℃下搅拌35min,加入枸橼酸钠,在40℃下搅拌2.5h,用磁铁吸引分离,洗涤,烘干,得到四氧化三铁纳米粒子;
四氧化三铁纳米粒子包括以下成分:按照重量计,13份FeCl3·6H2O、15份FeCl2·4H2O、22份去离子水、15份氨水、11份枸橼酸钠。
取3g聚苯乙烯磺酸钠修饰的石墨烯纳米片、20ml乙二醇,加入12g四氧化三铁纳米粒子、20g尿素,滴加30ml聚乙二醇400,搅拌35min,在190℃下反应8h,冷却,洗涤,烘干,得到GO-Fe3O4复合材料;
取21g聚氨酯树脂、15ml2-丁酮,混合均匀,得到聚氨酯树脂乳液,取5gGO-Fe3O4复合材料、20mlN-甲基吡咯烷酮,超声分散1.5h,加入聚氨酯树脂乳液、8.2g甲苯二异氰酸酯三聚体,超声分散1.5h,得到GO-Fe3O4聚氨酯树脂复合溶液。
步骤四:将PPS纤维置于丙酮中浸泡23h,洗涤,烘干,在45g/L的KOH中浸泡1.5h,取出,置于0.1mol/L硝酸溶液中浸泡15min,取出,置于15g/L的氯化亚锡和质量分数为2%的盐酸配制的混合液中浸泡6min,烘干,置于30g/L的的次亚磷酸钠溶液中浸泡2.5min,烘干,得到预处理后的PPS纤维;
取2.6gKOH、400ml硝酸银溶液,滴加氨水,至沉淀消失,加入3g乙醇稳定剂,制得镀银液;取3.3g葡萄糖、1g酒石酸、400ml去离子水,制得还原剂溶液;
将预处理后的PPS纤维置于镀银液中反应15min,加入还原液,在40℃下搅拌,取出PPS纤维,清洗,烘干,制得镀银阻燃改性PPS纤维;
步骤五:取尼龙66纤维置于氢氧化钠溶液中23h,取出,置于氯化钯、聚氨酯、烷基苯磺酸钠混合物中浸渍2.5h,取出,置于甲醛溶液中浸泡25min,取出;
取800ml去离子水、16g硫酸铜、15g甲醛搅拌均匀,搅拌均匀,得到组份A;取15g酒石酸钾钠、22g乙二胺四乙酸、7g氢氧化钠、1g氯化镍、10mg氰化钾、3g渗透剂JFC,搅拌均匀,加入组份A,加入尼龙66纤维,在60℃下搅拌,加入20mgα,α’-联吡啶,搅拌,制得镀铜尼龙66纤维;
步骤六:取聚四氟乙烯树脂,混合均匀,加入石墨烯,混合35min,静置59h,塑化9.5h,得到塑化后的混合料,压制成坯料,挤出,牵伸,静电处理,烘干,制得石墨烯改性聚四氟乙烯短纤;
步骤七:取1414对位芳纶纤维、阻燃涤纶纤维、316L不锈钢纤维、镀银阻燃改性PPS纤维、镀铜尼龙66纤维、石墨烯改性聚四氟乙烯短纤,纺丝,编制,得到面料,在面料表面涂布Ti3C2Tx分散液,晾干1.5h,涂布GO-Fe3O4聚氨酯树脂复合溶液,引入水平的磁场,磁场强度为230mT,在60℃下烘干11h,得到阻燃耐寒防割屏蔽多频谱面料;
面料包括以下成分:按照百分比计,19%的1414对位芳纶纤维、19%的阻燃涤纶纤维、31%的316L不锈钢纤维、9%的镀银阻燃改性PPS纤维、15%的镀铜尼龙66纤维、7%的石墨烯改性聚四氟乙烯短纤。
Ti3C2Tx分散液的涂布量为20g/m2;GO-Fe3O4聚氨酯树脂复合溶液的涂布量为26g/m2。
实验
取实施例1~实施例7制备得到的阻燃耐寒防割屏蔽多频谱面料进行性能测试,使用HC-2氧指数仪,对面料进行阻燃性能测试,测量标准为ASTMD2863,所用织物样品为150×58mm2;使用矢量网络分析仪AV3672型号仪器,对面料进行屏蔽多频谱测试,测试面料在8.2-12.4GHz区域的参数,面料尺寸为22.8×10mm。得到的数据如下所示:
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结论:有表上数据可知,实施例5不涂布Ti3C2Tx纳米片,面料的屏蔽多频谱功能差;实施例6不对石墨烯纳米片进行修饰,石墨烯片层结构不稳定,不容易被破坏,活性位点少,接枝的Fe3O4纳米粒子少,屏蔽性能、阻燃性能变差;实施例7不在石墨烯纳米片上复合四氧化三铁纳米粒子,屏蔽多频谱效果变差;实施例8Ti3C2Tx分散液与GO-Fe3O4聚氨酯树脂复合溶液的质量比为0.8:1.3,和实施例2-4相比,性能变差。
最后应说明的是:以上所述仅为本发明的优选实施例而已,并不用于限制本发明,尽管参照前述实施例对本发明进行了详细的说明,对于本领域的技术人员来说,其依然可以对前述各实施例所记载的技术方案进行修改,或者对其中部分技术特征进行等同替换。凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (8)
1.一种阻燃耐寒防割屏蔽多频谱面料的制备方法,其特征在于:
步骤一:取KOH、硝酸银溶液,滴加氨水,至沉淀消失,加入乙醇稳定剂,搅拌均匀,制得镀银液;取葡萄糖、酒石酸、去离子水,搅拌均匀,制得还原剂溶液;
将预处理后的PPS纤维置于镀银液中反应10-20min,加入还原液,在30-50℃下搅拌,取出PPS纤维,清洗,烘干,制得镀银阻燃改性PPS纤维;
步骤二:取去离子水、硫酸铜、甲醛搅拌均匀,搅拌均匀,得到组份A;取酒石酸钾钠、乙二胺四乙酸、氢氧化钠、氯化镍、氰化钾、渗透剂JFC,搅拌均匀,加入组份A,加入预处理后的尼龙66纤维,在50-70℃下搅拌,加入α,α’-联吡啶,搅拌,制得镀铜尼龙66纤维;
步骤三:取聚四氟乙烯树脂,混合均匀,加入石墨烯,混合30-40min,静置58-60h,塑化9-10h,得到塑化后的混合料,压制成坯料,挤出,牵伸,静电处理,烘干,制得石墨烯改性聚四氟乙烯短纤;
步骤四:取1414对位芳纶纤维、阻燃涤纶纤维、316L不锈钢纤维、镀银阻燃改性PPS纤维、镀铜尼龙66纤维、石墨烯改性聚四氟乙烯短纤,纺丝,编制,得到面料;
步骤四中,在面料表面涂布Ti3C2Tx分散液,晾干1-2h,涂布GO-Fe3O4聚氨酯树脂复合溶液,引入水平的磁场,磁场强度为220-240mT,在55-65℃下烘干10-12h;
Ti3C2Tx分散液的制备方法为:取氟化锂、盐酸搅拌均匀,加入Ti3AlC2粉末,在40-42℃下搅拌反应44-50h,洗涤,在-2-2℃下超声30-40min,离心,加入1000ml去离子水,搅拌均匀,得到Ti3C2Tx分散液。
2.根据权利要求1所述的一种阻燃耐寒防割屏蔽多频谱面料的制备方法,其特征在于:面料包括以下成分:按照百分比计,18-20%的1414对位芳纶纤维、18-20%的阻燃涤纶纤维、30-32%的316L不锈钢纤维、8%-10%的镀银阻燃改性PPS纤维、14-16%的镀铜尼龙66纤维、6-8%的石墨烯改性聚四氟乙烯短纤。
3.根据权利要求1所述的一种阻燃耐寒防割屏蔽多频谱面料的制备方法,其特征在于:预处理后的PPS纤维的制备方法为:将PPS纤维置于丙酮中浸泡22-24h,洗涤,烘干,在45g/L的KOH中浸泡1-2h,取出,置于0.1mol/L硝酸溶液中浸泡10-20min,取出,置于15g/L的氯化亚锡和质量分数为2%的盐酸配制的混合液中浸泡5-7min,烘干,置于30g/L的的次亚磷酸钠溶液中浸泡2-3min,烘干,得到预处理过的PPS纤维;
预处理后的尼龙66纤维的制备方法为:取尼龙66纤维置于氢氧化钠溶液中22-24h,取出,置于氯化钯、聚氨酯、烷基苯磺酸钠混合物中浸渍2-3h,取出,置于甲醛溶液中浸泡20-30min,烘干,得到预处理后的尼龙66纤维。
4.根据权利要求1所述的一种阻燃耐寒防割屏蔽多频谱面料的制备方法,其特征在于:步骤四中,GO-Fe3O4聚氨酯树脂复合溶液的制备方法为:取聚氨酯树脂、2-丁酮,混合均匀,得到聚氨酯树脂乳液;取GO-Fe3O4复合材料、N-甲基吡咯烷酮,超声分散1-2h,加入聚氨酯树脂乳液、甲苯二异氰酸酯三聚体,超声分散1-2h,得到GO-Fe3O4聚氨酯树脂复合溶液。
5.根据权利要求1所述的一种阻燃耐寒防割屏蔽多频谱面料的制备方法,其特征在于:步骤四中,Ti3C2Tx分散液与GO-Fe3O4聚氨酯树脂复合溶液的质量比为1.0:(1.2-1.4)。
6.根据权利要求1所述的一种阻燃耐寒防割屏蔽多频谱面料的制备方法,其特征在于:GO-Fe3O4复合材料的制备方法为:取聚苯乙烯磺酸钠修饰的石墨烯纳米片、乙二醇,加入四氧化三铁纳米粒子、尿素,滴加聚乙二醇400,搅拌30-40min,在180-200℃下反应7-9h,冷却,洗涤,烘干,得到GO-Fe3O4复合材料。
7.根据权利要求6所述的一种阻燃耐寒防割屏蔽多频谱面料的制备方法,其特征在于:聚苯乙烯磺酸钠修饰的石墨烯纳米片的制备方法为:取对苯乙烯磺酸钠、去离子水,搅拌均匀,得到对苯乙烯磺酸钠溶液;取石墨箔作为阳极,铂电极作为阴极,阳极与阴极之间的间隔为1-2cm,电压为14-16V,平行放置于对苯乙烯磺酸钠溶液中6-8h;加入过硫酸铵、亚硫酸铵,超声分散2-3h,过滤,收集悬浮物,洗涤,干燥,得到聚苯乙烯磺酸钠修饰的石墨烯纳米片。
8.根据权利要求1-7任意一项所述的一种阻燃耐寒防割屏蔽多频谱面料的制备方法制备得到的一种阻燃耐寒防割屏蔽多频谱面料。
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