CN111907139A - 一种基于碳纳米的防电磁辐射面料及其制备方法 - Google Patents
一种基于碳纳米的防电磁辐射面料及其制备方法 Download PDFInfo
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- CN111907139A CN111907139A CN202010733423.XA CN202010733423A CN111907139A CN 111907139 A CN111907139 A CN 111907139A CN 202010733423 A CN202010733423 A CN 202010733423A CN 111907139 A CN111907139 A CN 111907139A
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- Prior art keywords
- fabric
- fibers
- stirring
- fiber
- drying
- Prior art date
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- 239000004744 fabric Substances 0.000 title claims abstract description 115
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 230000005855 radiation Effects 0.000 title claims abstract description 23
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 229920000742 Cotton Polymers 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 19
- 238000009941 weaving Methods 0.000 claims abstract description 18
- 229920006231 aramid fiber Polymers 0.000 claims abstract description 12
- 239000000835 fiber Substances 0.000 claims description 122
- 238000003756 stirring Methods 0.000 claims description 72
- 238000001035 drying Methods 0.000 claims description 64
- 238000005406 washing Methods 0.000 claims description 54
- 238000010438 heat treatment Methods 0.000 claims description 44
- 239000003607 modifier Substances 0.000 claims description 43
- 238000009987 spinning Methods 0.000 claims description 41
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 36
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 34
- 239000000463 material Substances 0.000 claims description 34
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 claims description 33
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 30
- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical compound NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 claims description 26
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 25
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 25
- 239000002041 carbon nanotube Substances 0.000 claims description 24
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 24
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- 229920000049 Carbon (fiber) Polymers 0.000 claims description 23
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 23
- 239000008367 deionised water Substances 0.000 claims description 22
- 229910021641 deionized water Inorganic materials 0.000 claims description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 22
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 239000002245 particle Substances 0.000 claims description 21
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 20
- 229910017604 nitric acid Inorganic materials 0.000 claims description 20
- 229910052757 nitrogen Inorganic materials 0.000 claims description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- 238000001816 cooling Methods 0.000 claims description 16
- 238000010521 absorption reaction Methods 0.000 claims description 15
- 239000004793 Polystyrene Substances 0.000 claims description 14
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- 150000002815 nickel Chemical class 0.000 claims description 14
- 229920002223 polystyrene Polymers 0.000 claims description 14
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 13
- 229960003638 dopamine Drugs 0.000 claims description 13
- 239000012286 potassium permanganate Substances 0.000 claims description 12
- 238000004381 surface treatment Methods 0.000 claims description 12
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- 235000017166 Bambusa arundinacea Nutrition 0.000 claims description 10
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- 241001330002 Bambuseae Species 0.000 claims description 10
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- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims description 10
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- FYFFGSSZFBZTAH-UHFFFAOYSA-N methylaminomethanetriol Chemical compound CNC(O)(O)O FYFFGSSZFBZTAH-UHFFFAOYSA-N 0.000 claims description 10
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- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 claims description 10
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- 235000011150 stannous chloride Nutrition 0.000 claims description 10
- AXZWODMDQAVCJE-UHFFFAOYSA-L tin(II) chloride (anhydrous) Chemical compound [Cl-].[Cl-].[Sn+2] AXZWODMDQAVCJE-UHFFFAOYSA-L 0.000 claims description 10
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 10
- CDVAIHNNWWJFJW-UHFFFAOYSA-N 3,5-diethoxycarbonyl-1,4-dihydrocollidine Chemical compound CCOC(=O)C1=C(C)NC(C)=C(C(=O)OCC)C1C CDVAIHNNWWJFJW-UHFFFAOYSA-N 0.000 claims description 9
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- NCPXQVVMIXIKTN-UHFFFAOYSA-N trisodium;phosphite Chemical group [Na+].[Na+].[Na+].[O-]P([O-])[O-] NCPXQVVMIXIKTN-UHFFFAOYSA-N 0.000 claims description 5
- RRIWRJBSCGCBID-UHFFFAOYSA-L nickel sulfate hexahydrate Chemical compound O.O.O.O.O.O.[Ni+2].[O-]S([O-])(=O)=O RRIWRJBSCGCBID-UHFFFAOYSA-L 0.000 claims description 4
- 229940116202 nickel sulfate hexahydrate Drugs 0.000 claims description 4
- LAIZPRYFQUWUBN-UHFFFAOYSA-L nickel chloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Ni+2] LAIZPRYFQUWUBN-UHFFFAOYSA-L 0.000 claims description 3
- 230000001590 oxidative effect Effects 0.000 claims description 3
- LZKLAOYSENRNKR-LNTINUHCSA-N iron;(z)-4-oxoniumylidenepent-2-en-2-olate Chemical compound [Fe].C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O LZKLAOYSENRNKR-LNTINUHCSA-N 0.000 claims description 2
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- 230000000052 comparative effect Effects 0.000 description 9
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- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 6
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- GEYXPJBPASPPLI-UHFFFAOYSA-N manganese(III) oxide Inorganic materials O=[Mn]O[Mn]=O GEYXPJBPASPPLI-UHFFFAOYSA-N 0.000 description 2
- 229910000480 nickel oxide Inorganic materials 0.000 description 2
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 2
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- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 1
- 239000004005 microsphere Substances 0.000 description 1
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明公开了一种基于碳纳米的防电磁辐射面料及其制备方法，其中包括底布、屏蔽层和面布，面布由质量比为2：1的棉纤维、芳纶纤维编织而成，底布由质量比为2：1的棉质纤维、竹炭纤维编织而成，在底布和面布之间设置屏蔽层，在保证面料屏蔽性能的同时保证面料外观，制备得到的面料成品美观，触感柔软，透气轻薄。本发明公开了一种基于碳纳米的防电磁辐射面料及其制备方法，工艺设计合理，组分配比适宜，制备得到的面料外表美观，触感轻柔，且具有优异的电磁屏蔽性能，可应用于多种领域，实用性较高。
Description
技术领域
本发明涉及面料加工技术领域，具体是一种基于碳纳米的防电磁辐射面料及其制备方法。
背景技术
电磁辐射，一种电场和磁场的交互变化产生的电磁波向空中发射或泄露的现象，随着科技的进步和发展，各种电子不断进入我们的生活中，在带来便利的同时也造成了大量的电磁波辐射污染，长时间处于电磁污染环境下，会给人们的健康带来隐患。
现有技术中，针对抗电磁辐射污染，我们研发了大量的具有电磁屏蔽性能的面料，但该电磁屏蔽性能都无法满足我们的需求，给实际应用带来不便。
针对该问题，我们公开了一种基于碳纳米的防电磁辐射面料及其制备方法，以解决该问题。
发明内容
本发明的目的在于提供一种基于碳纳米的防电磁辐射面料及其制备方法，以解决现有技术中的问题。
为实现上述目的，本发明提供如下技术方案：
一种基于碳纳米的防电磁辐射面料，所述面料由底布、屏蔽层和面布热压复合，所述屏蔽层位于底布、面布之间；所述屏蔽层由改性混纱编织制得；所述改性混纱由混纱经过表面改性剂处理得到；
所述混纱包括碳化硅纤维、碳纳米管纤维和碳化硅纤维，所述碳化纤维、碳纳米管纤维和碳化硅纤维的质量比为(1-2)：1：1。
较优化的方案，所述表面改性剂包括表面改性剂A和表面改性剂B；所述表面改性剂A包括高锰酸钾、叔丁醇和正硅酸四乙酯；所述表面改性剂B包括二氯化锡、盐酸、二氯化钯、镍盐、还原剂和pH缓冲剂。
较优化的方案，所述底布由棉质纤维、竹炭纤维编织而成，所述棉质纤维、竹炭纤维质量比为2：1；所述面布由棉纤维、芳纶纤维编织而成，所述棉纤维、芳纶纤维的质量比为2：1。
较优化的方案，所述镍盐为六水合氯化镍、六水硫酸镍中的任意一种。
较优化的方案，所述还原剂为亚磷酸钠。
较优化的方案，一种基于碳纳米的防电磁辐射面料的制备方法，包括以下步骤：
1)准备物料；
2)碳化纤维的制备；
3)取碳化纤维、碳纳米管纤维和碳化硅纤维，制得混纱；
4)表面改性剂进行混纱表面处理，编织，得到屏蔽层；
5)取底布、屏蔽层和面布，热压复合得成品。
较优化的方案，包括以下步骤：
1)准备物料；
2)碳化纤维的制备：
a)取聚苯乙烯颗粒，三羟甲基氨基甲烷缓冲溶液溶解，超声分散，得物料A；
b)取聚丙烯腈、乙酰丙酮铁和二甲基甲酰胺，混合搅拌，再加入物料A，继续搅拌，接着加入多巴胺，静电纺丝，得到纺丝纤维；
c)取纺丝纤维，置于250-260℃下预氧化，接着置于氮气环境下，加热升温至300-400℃，保温，再升温至650-660℃，碳化，再升温至690-700℃，保温，降温后置于硝酸溶液中，60-65℃下加热处理，洗涤干燥，得到碳化纤维；
3)混纱的制备：取碳化纤维、碳纳米管纤维和碳化硅纤维，并线加捻，得到混纱，再将混纱置于浓硝酸中，120-130℃油浴下反应，去离子水洗涤，干燥备用；
4)表面改性剂进行表面处理：
a)表面改性剂A进行处理：取高锰酸钾，去离子水溶解搅拌，调节pH为8-9，加入步骤3)处理后的混纱、叔丁醇，加入正硅酸四乙酯，搅拌反应30-40min，接着置于氮气环境下进行γ辐照，辐照时搅拌并调节pH至10-11，离心分离，去离子水、乙醇交替洗涤，60-70℃下干燥24h，得到预处理纱线；
b)表面改性剂B进行处理：取预处理纱线，置于二氯化锡、盐酸混合溶液中，搅拌反应，洗涤干燥，再置于二氯化钯、盐酸溶液中，浸泡30-40min，洗涤至中性，干燥后置于氢氧化钠溶液中，调节pH至9，接着加入镍盐、还原剂、pH缓冲剂，搅拌，45-48℃下反应2-3h,洗涤干燥，再至于650-660℃下反应，冷却，得到改性混纱；
5)取改性混纱，洗涤干燥，编织，得到屏蔽层；取底布、屏蔽层和面布，分别干燥定型，再依次按照底布、屏蔽层和面布的顺序堆叠，热压复合，得到成品。
较优化的方案，包括以下步骤：
1)准备物料；
2)碳化纤维的制备：
a)取聚苯乙烯颗粒，三羟甲基氨基甲烷缓冲溶液溶解，超声分散10-15min，得物料A；
b)取聚丙烯腈、乙酰丙酮铁和二甲基甲酰胺，混合搅拌10-15h，再加入物料A，继续搅拌30-40min，接着加入多巴胺，搅拌24-28h，静电纺丝，得到纺丝纤维；
c)取纺丝纤维，置于250-260℃下预氧化5-6h，接着置于氮气环境下，加热升温至300-400℃，保温1-1.2h，再升温至650-660℃，碳化3-3.5h，再升温至690-700℃，保温20-30min，降温后置于硝酸溶液中，60-65℃下加热处理12-13h，洗涤干燥，得到碳化纤维；
3)混纱的制备：取碳化纤维、碳纳米管纤维和碳化硅纤维，并线加捻，得到混纱，再将混纱置于浓硝酸中，120-130℃油浴下反应4-6h，去离子水洗涤，干燥备用；
4)表面改性剂进行表面处理：
a)表面改性剂A进行处理：取高锰酸钾，去离子水溶解，搅拌5-15min，调节pH为8-9，加入步骤3)处理后的混纱、叔丁醇，搅拌10-15min，再加入正硅酸四乙酯，搅拌反应30-40min，接着置于氮气环境下进行γ辐照，辐照时搅拌并调节pH至10-11，离心分离，去离子水、乙醇交替洗涤，60-70℃下干燥24h，得到预处理纱线；
b)表面改性剂B进行处理：取预处理纱线，置于二氯化锡、盐酸混合溶液中，搅拌反应1-1.5h，洗涤干燥，再置于二氯化钯、盐酸溶液中，浸泡30-40min，洗涤至中性，干燥后置于氢氧化钠溶液中，调节pH至9，接着加入镍盐、还原剂、pH缓冲剂，搅拌20-30min，45-48℃下反应2-3h,洗涤干燥，再至于650-660℃下，反应1.5-2h，冷却，得到改性混纱；
5)取改性混纱，洗涤干燥，编织，得到屏蔽层；取底布、屏蔽层和面布，分别干燥定型，再依次按照底布、屏蔽层和面布的顺序堆叠，热压复合，得到成品。
较优化的方案，步骤2)的c)步骤中，加热升温速率均为5-6℃/min。
较优化的方案，步骤4)的a)步骤中，γ辐照时吸收剂量率为55-56Gy/min，吸收剂量为79-80KGy。
与现有技术相比，本发明的有益效果是：
本发明公开了一种基于碳纳米的防电磁辐射面料，其中包括底布、屏蔽层和面布，面布由质量比为2：1的棉纤维、芳纶纤维编织而成，底布由质量比为2：1的棉质纤维、竹炭纤维编织而成，在底布和面布之间设置屏蔽层，在保证面料的屏蔽性能的同时保留面料外观的可塑性，制备得到的面料成品美观，触感柔软，透气轻薄。
本申请中公开了一种碳化纤维，制备时先利用乙酰丙酮铁作为前驱体生成氧化铁，同时加入聚苯乙烯颗粒和多巴胺，聚苯乙烯颗粒可掺杂分散在各组分之中，而多巴胺可以自聚生成聚多巴胺，聚多巴胺具有较高的粘结性能，可在各组分表面沉积，静电纺丝后可得到纺丝纤维。再加热升温至300-400℃对纺丝纤维进行碳化，聚苯乙烯微球受热分解并产生大量气体，可产生爆破效应，使得聚多巴胺沉积层受力破裂，从而使纺丝纤维的形态发生改变；保温一段时间后继续升温至650-660℃，此时体系中的氧化铁在高温下可将纳米纤维中的有机物催化形成石墨化碳，再升温至690-700℃并保温，将纺丝纤维的杂原子官能团进行碳化，碳化后置于硝酸溶液中处理，除去残留氧化铁纳米粒子，得到碳化纤维，该碳化纤维为形态不规则的多孔纤维，表面粗糙，具有较高的比表面积，为后续的颗粒负载提供了丰富的反应位点。
本发明将碳化纤维、碳纳米管纤维和碳化硅纤维并线加捻后得到混纱，利用浓硝酸进行表面清洁，再利用表面改性剂对其进行表面处理；先利用表面改性剂A对其进行表面改性，将混纱置于高锰酸钾、叔丁醇等组分中，利用辐照还原法对其进行还原，反应时先调节pH为8-9，在该pH下进行γ射线辐照，此时高锰酸钾会被氧化并生成四氧化三锰粒子，同时辐照时调节pH至10-11，在该pH下体系中会生成二氧化锰粒子，由于碳化纤维、碳纳米管纤维均具有优异的比表面积，四氧化三锰粒子和二氧化锰粒子会负载在混纱表面；在制备过程中还添加了正硅酸四乙酯，正硅酸四乙酯水解并缩合生成二氧化硅，二氧化硅包裹在四氧化三锰粒子、二氧化锰粒子及混纱表面，制备得到预处理纱线。
接着本申请利用表面改性剂B对预处理纱线进行处理，先将其置于二氯化锡-盐酸混合溶液、二氯化钯-盐酸混合溶液中进行敏华、活化，再通过氧化还原法在预处理纱线表面沉积氧化镍，得到改性混纱，最后将改性混纱编织得到屏蔽层，该屏蔽层具有优异的吸波性能，使得成品面料具有优异的电磁屏蔽性能。
本发明中，碳纳米管纤维、碳化纤维、碳化硅纤维均具有优异的电磁屏蔽性能，但碳纳米管、碳化纤维单独使用时存在阻抗匹配特性较差、吸收带窄、性能弱等缺点，因此本申请利用辐照还原法在其表面负载锰氧化物，使得混纱具有强吸收、宽频带等特点，可作为吸波材料进行电磁吸收；同时在辐照还原过程中引入正硅酸四乙酯，从而引入二氧化硅，可有效提高混纱的电导率和介电常数，从而提高混纱的吸波性能；再利用表面改性B进行表面改性，在其表面沉积氧化镍，进一步提高改性纱线的吸波性能。
本发明制备时对各组分的形态进行调整，在制备碳化纤维时，利用多巴胺和聚苯乙烯等组分在高温下作用，使得碳化纤维呈现不规则、表面多孔结构，同时在后续表面处理时，在其负载四氧化三锰粒子和二氧化锰粒子，四氧化三锰为多面体结构，二氧化锰为棒状、球状混合结构，各组分粒子负载在碳化纤维表面，由于结构的不同和相互接触，会在碳化纤维表面生成特殊的交叉结构、多孔结构，电磁波渗透至面料中时会在不规则多孔通道中多次反射吸收，增加了电磁波的衰减而不被反射，进一步提高了面料的电磁屏蔽性能。
本发明公开了一种基于碳纳米的防电磁辐射面料及其制备方法，工艺设计合理，组分配比适宜，制备得到的面料外表美观，触感轻柔，且具有优异的电磁屏蔽性能，可应用于多种领域，实用性较高。
具体实施方式
下面将对本发明实例中的技术方案进行清楚、完整地描述，显然，所描述的实例仅仅是本发明一部分实例，而不是全部的实例。基于本发明中的实例，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例，都属于本发明保护的范围。
实例1：
S1：准备物料；
S2：碳化纤维的制备：
取聚苯乙烯颗粒，三羟甲基氨基甲烷缓冲溶液溶解，超声分散10min，得物料A；取聚丙烯腈、乙酰丙酮铁和二甲基甲酰胺，混合搅拌10h，再加入物料A，继续搅拌30min，接着加入多巴胺，搅拌24h，静电纺丝，得到纺丝纤维；
取纺丝纤维，置于250℃下预氧化5h，接着置于氮气环境下，加热升温至300℃，保温1h，再升温至650℃，碳化3h，再升温至690℃，保温20-30min，降温后置于硝酸溶液中，60℃下加热处理12h，洗涤干燥，得到碳化纤维；其中加热升温速率均为5℃/min；
S3：混纱的制备：
取碳化纤维、碳纳米管纤维和碳化硅纤维，并线加捻，得到混纱，再将混纱置于浓硝酸中，120℃油浴下反应4h，去离子水洗涤，干燥备用；
S4：表面改性剂进行表面处理：
表面改性剂A进行处理：取高锰酸钾，去离子水溶解，搅拌5min，调节pH为8，加入S3步骤处理后的混纱、叔丁醇，搅拌10min，再加入正硅酸四乙酯，搅拌反应30min，接着置于氮气环境下进行γ辐照，辐照时搅拌并调节pH至10，离心分离，去离子水、乙醇交替洗涤，60℃下干燥24h，得到预处理纱线；γ辐照时吸收剂量率为55Gy/min，吸收剂量为79KGy；
表面改性剂B进行处理：取预处理纱线，置于二氯化锡、盐酸混合溶液中，搅拌反应1h，洗涤干燥，再置于二氯化钯、盐酸溶液中，浸泡30min，洗涤至中性，干燥后置于氢氧化钠溶液中，调节pH至9，接着加入镍盐、还原剂、pH缓冲剂，搅拌20min，45℃下反应2h,洗涤干燥，再至于650℃下，反应1.5h，冷却，得到改性混纱；
S5：取改性混纱，洗涤干燥，编织，得到屏蔽层；取底布、屏蔽层和面布，分别干燥定型，再依次按照底布、屏蔽层和面布的顺序堆叠，热压复合，得到成品。
本实例中，所述碳化纤维、碳纳米管纤维和碳化硅纤维的质量比为1：1：1；所述底布由棉质纤维、竹炭纤维编织而成，所述棉质纤维、竹炭纤维质量比为2：1；所述面布由棉纤维、芳纶纤维编织而成，所述棉纤维、芳纶纤维的质量比为2：1；镍盐为六水合氯化镍；还原剂为亚磷酸钠。
实例2：
S1：准备物料；
S2：碳化纤维的制备：
取聚苯乙烯颗粒，三羟甲基氨基甲烷缓冲溶液溶解，超声分散12min，得物料A；取聚丙烯腈、乙酰丙酮铁和二甲基甲酰胺，混合搅拌12，再加入物料A，继续搅拌35min，接着加入多巴胺，搅拌26h，静电纺丝，得到纺丝纤维；
取纺丝纤维，置于255℃下预氧化5.5h，接着置于氮气环境下，加热升温至350℃，保温1.1h，再升温至655℃，碳化3.2h，再升温至695℃，保温25min，降温后置于硝酸溶液中，62℃下加热处理12.5h，洗涤干燥，得到碳化纤维；其中加热升温速率均为5℃/min；
S3：混纱的制备：
取碳化纤维、碳纳米管纤维和碳化硅纤维，并线加捻，得到混纱，再将混纱置于浓硝酸中，125℃油浴下反应5h，去离子水洗涤，干燥备用；
S4：表面改性剂进行表面处理：
表面改性剂A进行处理：取高锰酸钾，去离子水溶解，搅拌10min，调节pH为9，加入S3步骤处理后的混纱、叔丁醇，搅拌12min，再加入正硅酸四乙酯，搅拌反应35min，接着置于氮气环境下进行γ辐照，辐照时搅拌并调节pH至11，离心分离，去离子水、乙醇交替洗涤，65℃下干燥24h，得到预处理纱线；γ辐照时吸收剂量率为55Gy/min，吸收剂量为79KGy；
表面改性剂B进行处理：取预处理纱线，置于二氯化锡、盐酸混合溶液中，搅拌反应1.2h，洗涤干燥，再置于二氯化钯、盐酸溶液中，浸泡35min，洗涤至中性，干燥后置于氢氧化钠溶液中，调节pH至9，接着加入镍盐、还原剂、pH缓冲剂，搅拌25min，47℃下反应2.5h,洗涤干燥，再至于655℃下，反应1.8h，冷却，得到改性混纱；
S5：取改性混纱，洗涤干燥，编织，得到屏蔽层；取底布、屏蔽层和面布，分别干燥定型，再依次按照底布、屏蔽层和面布的顺序堆叠，热压复合，得到成品。
本实例中，所述碳化纤维、碳纳米管纤维和碳化硅纤维的质量比为1.5：1：1；所述底布由棉质纤维、竹炭纤维编织而成，所述棉质纤维、竹炭纤维质量比为2：1；所述面布由棉纤维、芳纶纤维编织而成，所述棉纤维、芳纶纤维的质量比为2：1；镍盐为六水硫酸镍；还原剂为亚磷酸钠。
实例3：
S1：准备物料；
S2：碳化纤维的制备：
取聚苯乙烯颗粒，三羟甲基氨基甲烷缓冲溶液溶解，超声分散15min，得物料A；取聚丙烯腈、乙酰丙酮铁和二甲基甲酰胺，混合搅拌15h，再加入物料A，继续搅拌40min，接着加入多巴胺，搅拌28h，静电纺丝，得到纺丝纤维；
取纺丝纤维，置于260℃下预氧化5-6h，接着置于氮气环境下，加热升温至400℃，保温1.2h，再升温至660℃，碳化3.5h，再升温至700℃，保温30min，降温后置于硝酸溶液中，65℃下加热处理13h，洗涤干燥，得到碳化纤维；其中加热升温速率均为6℃/min；
S3：混纱的制备：
取碳化纤维、碳纳米管纤维和碳化硅纤维，并线加捻，得到混纱，再将混纱置于浓硝酸中，130℃油浴下反应6h，去离子水洗涤，干燥备用；
S4：表面改性剂进行表面处理：
表面改性剂A进行处理：取高锰酸钾，去离子水溶解，搅拌15min，调节pH为9，加入S3步骤处理后的混纱、叔丁醇，搅拌15min，再加入正硅酸四乙酯，搅拌反应40min，接着置于氮气环境下进行γ辐照，辐照时搅拌并调节pH至11，离心分离，去离子水、乙醇交替洗涤，70℃下干燥24h，得到预处理纱线；γ辐照时吸收剂量率为56Gy/min，吸收剂量为80KGy；
表面改性剂B进行处理：取预处理纱线，置于二氯化锡、盐酸混合溶液中，搅拌反应1.5h，洗涤干燥，再置于二氯化钯、盐酸溶液中，浸泡40min，洗涤至中性，干燥后置于氢氧化钠溶液中，调节pH至9，接着加入镍盐、还原剂、pH缓冲剂，搅拌30min，48℃下反应3h,洗涤干燥，再至于660℃下，反应2h，冷却，得到改性混纱；
S5：取改性混纱，洗涤干燥，编织，得到屏蔽层；取底布、屏蔽层和面布，分别干燥定型，再依次按照底布、屏蔽层和面布的顺序堆叠，热压复合，得到成品。
本实例中，所述碳化纤维、碳纳米管纤维和碳化硅纤维的质量比为2：1：1；所述底布由棉质纤维、竹炭纤维编织而成，所述棉质纤维、竹炭纤维质量比为2：1；所述面布由棉纤维、芳纶纤维编织而成，所述棉纤维、芳纶纤维的质量比为2：1；镍盐为六水硫酸镍；还原剂为亚磷酸钠。
对比例1：
对比例1中未采用表面改性剂B对预处理纱线进行处理，其余影响因素与实例2一致。
具体步骤如下所示：
S1：准备物料；
S2：碳化纤维的制备：
取聚苯乙烯颗粒，三羟甲基氨基甲烷缓冲溶液溶解，超声分散12min，得物料A；取聚丙烯腈、乙酰丙酮铁和二甲基甲酰胺，混合搅拌12，再加入物料A，继续搅拌35min，接着加入多巴胺，搅拌26h，静电纺丝，得到纺丝纤维；
取纺丝纤维，置于255℃下预氧化5.5h，接着置于氮气环境下，加热升温至350℃，保温1.1h，再升温至655℃，碳化3.2h，再升温至695℃，保温25min，降温后置于硝酸溶液中，62℃下加热处理12.5h，洗涤干燥，得到碳化纤维；其中加热升温速率均为5℃/min；
S3：混纱的制备：
取碳化纤维、碳纳米管纤维和碳化硅纤维，并线加捻，得到混纱，再将混纱置于浓硝酸中，125℃油浴下反应5h，去离子水洗涤，干燥备用；
S4：表面改性剂进行表面处理：
表面改性剂A进行处理：取高锰酸钾，去离子水溶解，搅拌10min，调节pH为9，加入S3步骤处理后的混纱、叔丁醇，搅拌12min，再加入正硅酸四乙酯，搅拌反应35min，接着置于氮气环境下进行γ辐照，辐照时搅拌并调节pH至11，离心分离，去离子水、乙醇交替洗涤，65℃下干燥24h，得到预处理纱线；γ辐照时吸收剂量率为55Gy/min，吸收剂量为79KGy；
S5：取预处理纱线，洗涤干燥，编织，得到屏蔽层；取底布、屏蔽层和面布，分别干燥定型，再依次按照底布、屏蔽层和面布的顺序堆叠，热压复合，得到成品。
对比例2：
对比例2中未采用表面改性剂对混纱进行处理，其余影响因素与对比例1一致。
具体步骤如下所示：
S1：准备物料；
S2：碳化纤维的制备：
取聚苯乙烯颗粒，三羟甲基氨基甲烷缓冲溶液溶解，超声分散12min，得物料A；取聚丙烯腈、乙酰丙酮铁和二甲基甲酰胺，混合搅拌12，再加入物料A，继续搅拌35min，接着加入多巴胺，搅拌26h，静电纺丝，得到纺丝纤维；
取纺丝纤维，置于255℃下预氧化5.5h，接着置于氮气环境下，加热升温至350℃，保温1.1h，再升温至655℃，碳化3.2h，再升温至695℃，保温25min，降温后置于硝酸溶液中，62℃下加热处理12.5h，洗涤干燥，得到碳化纤维；其中加热升温速率均为5℃/min；
S3：混纱的制备：
取碳化纤维、碳纳米管纤维和碳化硅纤维，并线加捻，得到混纱，再将混纱置于浓硝酸中，125℃油浴下反应5h，去离子水洗涤，干燥备用；
S4：取S3处理后的混纱，洗涤干燥，编织，得到屏蔽层；取底布、屏蔽层和面布，分别干燥定型，再依次按照底布、屏蔽层和面布的顺序堆叠，热压复合，得到成品。
对比例3：
对比例3中未对纺丝纤维进行碳化及后续的表面改性剂处理，其余影响因素与对比例2一致。
具体步骤如下所示：
S1：准备物料；
S2：纺丝纤维的制备：
取聚苯乙烯颗粒，三羟甲基氨基甲烷缓冲溶液溶解，超声分散12min，得物料A；取聚丙烯腈、乙酰丙酮铁和二甲基甲酰胺，混合搅拌12，再加入物料A，继续搅拌35min，接着加入多巴胺，搅拌26h，静电纺丝，得到纺丝纤维；
S3：混纱的制备：
取纺丝纤维、碳纳米管纤维和碳化硅纤维，并线加捻，得到混纱，再将混纱置于浓硝酸中，125℃油浴下反应5h，去离子水洗涤，干燥备用；
S4：取S3处理后的混纱，洗涤干燥，编织，得到屏蔽层；取底布、屏蔽层和面布，分别干燥定型，再依次按照底布、屏蔽层和面布的顺序堆叠，热压复合，得到成品。
试验：
取实例1-3、对比例1-3制备的面料样品，分别依据GB/T22583-2009《防辐射针织品》进行电磁屏蔽测试，具体检测数据如下表所示：
结论：本发明工艺设计合理，组分配比适宜，制备得到的面料外表美观，触感轻柔，且具有优异的电磁屏蔽性能。
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。
Claims (10)
1.一种基于碳纳米的防电磁辐射面料，其特征在于：所述面料由底布、屏蔽层和面布热压复合，所述屏蔽层位于底布、面布之间；所述屏蔽层由改性混纱编织制得；所述改性混纱由混纱经过表面改性剂处理得到；
所述混纱包括碳化硅纤维、碳纳米管纤维和碳化硅纤维，所述碳化纤维、碳纳米管纤维和碳化硅纤维的质量比为(1-2)：1：1。
2.根据权利要求1所述的一种基于碳纳米的防电磁辐射面料，其特征在于：所述表面改性剂包括表面改性剂A和表面改性剂B；所述表面改性剂A包括高锰酸钾、叔丁醇和正硅酸四乙酯；所述表面改性剂B包括二氯化锡、盐酸、二氯化钯、镍盐、还原剂和pH缓冲剂。
3.根据权利要求1所述的一种基于碳纳米的防电磁辐射面料，其特征在于：所述底布由棉质纤维、竹炭纤维编织而成，所述棉质纤维、竹炭纤维质量比为2：1；所述面布由棉纤维、芳纶纤维编织而成，所述棉纤维、芳纶纤维的质量比为2：1。
4.根据权利要求2所述的一种基于碳纳米的防电磁辐射面料，其特征在于：所述镍盐为六水合氯化镍、六水硫酸镍中的任意一种。
5.根据权利要求2所述的一种基于碳纳米的防电磁辐射面料，其特征在于：所述还原剂为亚磷酸钠。
6.一种基于碳纳米的防电磁辐射面料的制备方法，其特征在于：包括以下步骤：
1)准备物料；
2)碳化纤维的制备；
3)取碳化纤维、碳纳米管纤维和碳化硅纤维，制得混纱；
4)表面改性剂进行混纱表面处理，编织，得到屏蔽层；
5)取底布、屏蔽层和面布，热压复合得成品。
7.根据权利要求6所述的一种基于碳纳米的防电磁辐射面料的制备方法，其特征在于：包括以下步骤：
1)准备物料；
2)碳化纤维的制备：
a)取聚苯乙烯颗粒，三羟甲基氨基甲烷缓冲溶液溶解，超声分散，得物料A；
b)取聚丙烯腈、乙酰丙酮铁和二甲基甲酰胺，混合搅拌，再加入物料A，继续搅拌，接着加入多巴胺，静电纺丝，得到纺丝纤维；
c)取纺丝纤维，置于250-260℃下预氧化，接着置于氮气环境下，加热升温至300-400℃，保温，再升温至650-660℃，碳化，再升温至690-700℃，保温，降温后置于硝酸溶液中，60-65℃下加热处理，洗涤干燥，得到碳化纤维；
3)混纱的制备：取碳化纤维、碳纳米管纤维和碳化硅纤维，并线加捻，得到混纱，再将混纱置于浓硝酸中，120-130℃油浴下反应，去离子水洗涤，干燥备用；
4)表面改性剂进行表面处理：
a)表面改性剂A进行处理：取高锰酸钾，去离子水溶解搅拌，调节pH为8-9，加入步骤3)处理后的混纱、叔丁醇，加入正硅酸四乙酯，搅拌反应30-40min，接着置于氮气环境下进行γ辐照，辐照时搅拌并调节pH至10-11，离心分离，去离子水、乙醇交替洗涤，60-70℃下干燥24h，得到预处理纱线；
b)表面改性剂B进行处理：取预处理纱线，置于二氯化锡、盐酸混合溶液中，搅拌反应，洗涤干燥，再置于二氯化钯、盐酸溶液中，浸泡30-40min，洗涤至中性，干燥后置于氢氧化钠溶液中，调节pH至9，接着加入镍盐、还原剂、pH缓冲剂，搅拌，45-48℃下反应2-3h,洗涤干燥，再至于650-660℃下反应，冷却，得到改性混纱；
5)取改性混纱，洗涤干燥，编织，得到屏蔽层；取底布、屏蔽层和面布，分别干燥定型，再依次按照底布、屏蔽层和面布的顺序堆叠，热压复合，得到成品。
8.根据权利要求7所述的一种基于碳纳米的防电磁辐射面料的制备方法，其特征在于：包括以下步骤：
1)准备物料；
2)碳化纤维的制备：
a)取聚苯乙烯颗粒，三羟甲基氨基甲烷缓冲溶液溶解，超声分散10-15min，得物料A；
b)取聚丙烯腈、乙酰丙酮铁和二甲基甲酰胺，混合搅拌10-15h，再加入物料A，继续搅拌30-40min，接着加入多巴胺，搅拌24-28h，静电纺丝，得到纺丝纤维；
c)取纺丝纤维，置于250-260℃下预氧化5-6h，接着置于氮气环境下，加热升温至300-400℃，保温1-1.2h，再升温至650-660℃，碳化3-3.5h，再升温至690-700℃，保温20-30min，降温后置于硝酸溶液中，60-65℃下加热处理12-13h，洗涤干燥，得到碳化纤维；
3)混纱的制备：取碳化纤维、碳纳米管纤维和碳化硅纤维，并线加捻，得到混纱，再将混纱置于浓硝酸中，120-130℃油浴下反应4-6h，去离子水洗涤，干燥备用；
4)表面改性剂进行表面处理：
a)表面改性剂A进行处理：取高锰酸钾，去离子水溶解，搅拌5-15min，调节pH为8-9，加入步骤3)处理后的混纱、叔丁醇，搅拌10-15min，再加入正硅酸四乙酯，搅拌反应30-40min，接着置于氮气环境下进行γ辐照，辐照时搅拌并调节pH至10-11，离心分离，去离子水、乙醇交替洗涤，60-70℃下干燥24h，得到预处理纱线；
b)表面改性剂B进行处理：取预处理纱线，置于二氯化锡、盐酸混合溶液中，搅拌反应1-1.5h，洗涤干燥，再置于二氯化钯、盐酸溶液中，浸泡30-40min，洗涤至中性，干燥后置于氢氧化钠溶液中，调节pH至9，接着加入镍盐、还原剂、pH缓冲剂，搅拌20-30min，45-48℃下反应2-3h,洗涤干燥，再至于650-660℃下，反应1.5-2h，冷却，得到改性混纱；
5)取改性混纱，洗涤干燥，编织，得到屏蔽层；取底布、屏蔽层和面布，分别干燥定型，再依次按照底布、屏蔽层和面布的顺序堆叠，热压复合，得到成品。
9.根据权利要求8所述的一种基于碳纳米的防电磁辐射面料的制备方法，其特征在于：步骤2)的c)步骤中，加热升温速率均为5-6℃/min。
10.根据权利要求8所述的一种基于碳纳米的防电磁辐射面料的制备方法，其特征在于：步骤4)的a)步骤中，γ辐照时吸收剂量率为55-56Gy/min，吸收剂量为79-80KGy。
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