CN110667199A - 一种高阻燃、透气、防静电面料 - Google Patents
一种高阻燃、透气、防静电面料 Download PDFInfo
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- CN110667199A CN110667199A CN201910794881.1A CN201910794881A CN110667199A CN 110667199 A CN110667199 A CN 110667199A CN 201910794881 A CN201910794881 A CN 201910794881A CN 110667199 A CN110667199 A CN 110667199A
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- flame
- retardant
- breathable
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- 239000004744 fabric Substances 0.000 title claims abstract description 90
- 239000003063 flame retardant Substances 0.000 claims abstract description 180
- 229920000742 Cotton Polymers 0.000 claims abstract description 178
- 230000000844 anti-bacterial effect Effects 0.000 claims abstract description 106
- 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 claims abstract description 105
- -1 flame-retardant compound Chemical class 0.000 claims abstract description 82
- 239000003242 anti bacterial agent Substances 0.000 claims abstract description 37
- 238000002360 preparation method Methods 0.000 claims abstract description 29
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 63
- 229910021389 graphene Inorganic materials 0.000 claims description 59
- CIMANFYHPPXAJW-UHFFFAOYSA-N 2-(8-chlorooctyl)oxirane Chemical compound ClCCCCCCCCC1CO1 CIMANFYHPPXAJW-UHFFFAOYSA-N 0.000 claims description 20
- VOUIEAZSNLLDLK-UHFFFAOYSA-N 2-(4-chlorobutyl)oxirane Chemical compound ClCCCCC1CO1 VOUIEAZSNLLDLK-UHFFFAOYSA-N 0.000 claims description 19
- 239000004593 Epoxy Substances 0.000 claims description 18
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 18
- 150000001350 alkyl halides Chemical class 0.000 claims description 18
- MWSLLEWOGABAFW-UHFFFAOYSA-N 1-bromo-1,3,5-triazinane-2,4,6-trione Chemical compound BrN1C(=O)NC(=O)NC1=O MWSLLEWOGABAFW-UHFFFAOYSA-N 0.000 claims description 16
- BRLQWZUYTZBJKN-UHFFFAOYSA-N Epichlorohydrin Chemical compound ClCC1CO1 BRLQWZUYTZBJKN-UHFFFAOYSA-N 0.000 claims description 16
- 239000002994 raw material Substances 0.000 claims description 16
- OSDWBNJEKMUWAV-UHFFFAOYSA-N Allyl chloride Chemical compound ClCC=C OSDWBNJEKMUWAV-UHFFFAOYSA-N 0.000 claims description 14
- 150000004820 halides Chemical class 0.000 claims description 14
- WQMAANNAZKNUDL-UHFFFAOYSA-N 2-dimethylaminoethyl chloride Chemical compound CN(C)CCCl WQMAANNAZKNUDL-UHFFFAOYSA-N 0.000 claims description 13
- 150000007973 cyanuric acids Chemical class 0.000 claims description 10
- ROSDSFDQCJNGOL-UHFFFAOYSA-N Dimethylamine Chemical compound CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 claims description 7
- 239000000853 adhesive Substances 0.000 claims description 6
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- ISAOUZVKYLHALD-UHFFFAOYSA-N 1-chloro-1,3,5-triazinane-2,4,6-trione Chemical compound ClN1C(=O)NC(=O)NC1=O ISAOUZVKYLHALD-UHFFFAOYSA-N 0.000 claims description 3
- WRYDGMWSKBGVHS-UHFFFAOYSA-N 2-bromo-n,n-diethylethanamine Chemical compound CCN(CC)CCBr WRYDGMWSKBGVHS-UHFFFAOYSA-N 0.000 claims description 3
- BIWJXEPRNRDVPB-UHFFFAOYSA-N 3-bromo-n,n-dimethylpropan-1-amine Chemical compound CN(C)CCCBr BIWJXEPRNRDVPB-UHFFFAOYSA-N 0.000 claims description 3
- WVUULNDRFBHTFG-UHFFFAOYSA-N 3-chloro-n,n-diethylpropan-1-amine Chemical compound CCN(CC)CCCCl WVUULNDRFBHTFG-UHFFFAOYSA-N 0.000 claims description 3
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- BHELZAPQIKSEDF-UHFFFAOYSA-N allyl bromide Chemical group BrCC=C BHELZAPQIKSEDF-UHFFFAOYSA-N 0.000 claims description 3
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 24
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- 238000002791 soaking Methods 0.000 description 16
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 description 13
- 229910052757 nitrogen Inorganic materials 0.000 description 13
- 238000003756 stirring Methods 0.000 description 13
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 12
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- LRWZZZWJMFNZIK-UHFFFAOYSA-N 2-chloro-3-methyloxirane Chemical compound CC1OC1Cl LRWZZZWJMFNZIK-UHFFFAOYSA-N 0.000 description 4
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- 125000002147 dimethylamino group Chemical group [H]C([H])([H])N(*)C([H])([H])[H] 0.000 description 4
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- ZRRZAIJKJYIGIV-UHFFFAOYSA-N 2-(3-bromopropyl)oxirane Chemical compound BrCCCC1CO1 ZRRZAIJKJYIGIV-UHFFFAOYSA-N 0.000 description 2
- HVDVDGGJUWKUJB-UHFFFAOYSA-N 6-chloro-n,n-dimethylhexan-1-amine Chemical group CN(C)CCCCCCCl HVDVDGGJUWKUJB-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
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- 238000010521 absorption reaction Methods 0.000 description 2
- 239000004599 antimicrobial Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000000903 blocking effect Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
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- HOMWBVGCEKMCBR-UHFFFAOYSA-N oct-7-en-1-amine Chemical group NCCCCCCC=C HOMWBVGCEKMCBR-UHFFFAOYSA-N 0.000 description 2
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- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 description 2
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- LSOXTBBDZHIHDE-UHFFFAOYSA-N 2-(3-chloropropyl)oxirane Chemical compound ClCCCC1CO1 LSOXTBBDZHIHDE-UHFFFAOYSA-N 0.000 description 1
- DDDKRQUCUNMSDF-UHFFFAOYSA-N 2-(4-bromobutyl)oxirane Chemical compound BrCCCCC1CO1 DDDKRQUCUNMSDF-UHFFFAOYSA-N 0.000 description 1
- ASVKKRLMJCWVQF-UHFFFAOYSA-N 3-buten-1-amine Chemical compound NCCC=C ASVKKRLMJCWVQF-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
- B32B5/02—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
- B32B5/024—Woven fabric
-
- 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
- A41D31/08—Heat resistant; Fire retardant
- A41D31/085—Heat resistant; Fire retardant using layered materials
-
- 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
- A41D31/14—Air permeable, i.e. capable of being penetrated by gases
- A41D31/145—Air permeable, i.e. capable of being penetrated by gases using layered materials
-
- 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
- A41D31/26—Electrically protective, e.g. preventing static electricity or electric shock
- A41D31/265—Electrically protective, e.g. preventing static electricity or electric shock using layered materials
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
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- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/12—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by using adhesives
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
- B32B5/02—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
- B32B5/08—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 the fibres or filaments of a layer being of different substances, e.g. conjugate fibres, mixture of different fibres
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
- B32B5/22—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed
- B32B5/24—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer
- B32B5/26—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer another layer next to it also being fibrous or filamentary
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
- B32B7/04—Interconnection of layers
- B32B7/12—Interconnection of layers using interposed adhesives or interposed materials with bonding properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
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Abstract
本发明涉及纺织面料技术领域,更具体地,本发明涉及一种高阻燃、透气、防静电面料及其制备方法。所述面料由抗菌内层与阻燃外层组成,其中,按重量份计,抗菌内层包括棉纤维80~120份、抗菌剂800~1200份,阻燃外层包括棉纤维100~150份、阻燃复合物15~25份。利用本发明制备的高阻燃、透气、防静电面料具有多种优异性能,具体表现为两种抗菌剂相互协同,在高效抗菌的同时因其独特的内部结构及自身性质,实现多次洗涤后仍具有优异的抗菌性能,体现高耐洗涤效果;多种阻燃剂依据不同的阻燃机理,达到综合阻止、抑制燃烧的目的,与此同时,阻燃剂与棉纤维相互作用,提高高阻燃、透气、防静电面料的拉伸强度。
Description
技术领域
本发明涉及纺织面料技术领域,更具体地,本发明涉及一种高阻燃、透气、防静电面料及其制备方法。
背景技术
随着科学技术的不断发展和现代化建设的加快,对纺织品面料种类及其功能提出了更高的要求,同时也对纺织品面料功能的多样化有了更多的要求。纺织品面料不再满足于一种功能,而是要求集多种功能于一体,从而更好地适应多种环境,更好地防御来自各种因素所造成的伤害。
消防员服装是消防员进行灭火救援时穿着的用来对躯干、头颈、手臂和腿部进行防御的专用服装的总称,是保护活跃在消防第一线的消防队员人身安全的最重要装备品。消防服的性能如何,直接影响着消防员的生命安全和救灾效率。随着科技的发展和环境需求的不同,防护服种类也变得多样化。
面对复杂多样的环境,消防员服装面料多采用两层或多层主要结构来达到不同功能的合理组合。从内到外分为贴身内层与阻燃外层。对现有的消防员服装面料进行调研后,发现存在着许多问题:(1)消防员服装面料的抗菌性能较差,在面临环境较为恶劣的情况下,外部的细菌容易通过消防服危害人体,且消防员服装面料的抗菌性能随着洗涤次数的增多,抗菌性能逐渐变差;(2)消防员服装面料阻燃外层达不到高阻燃效果,同时由于消防员在面对多种环境时活动幅度较大,例如跑、跳、攀爬等动作会对消防员服装面料有一定的拉伸,所以消防员服装面料需要具有一定的拉伸性能,但是现有的消防员服装面料存在拉伸强度差等问题。
基于消防员服装面料以上存在的问题,本发明涉及一种高阻燃、透气、防静电面料及其制备方法。
发明内容
为了解决上述问题,本发明第一方面提供了一种高阻燃、透气、防静电面料,其特征在于,所述面料由抗菌内层与阻燃外层组成,其中,按重量份计,抗菌内层包括棉纤维80~120份、抗菌剂800~1200份,阻燃外层包括棉纤维100~150份、阻燃复合物15~25份。
作为本发明的一种优选技术方案,其中,所述抗菌剂的制备原料包括单卤代氰尿酸、二氨基卤代烷、烯类卤化物、环氧卤代烷,所述阻燃复合物的制备原料包括氧化石墨烯、氨基烯类化合物、硅烷偶联剂。
作为本发明的一种优选技术方案,其中,所述单卤代氰尿酸、二氨基卤代烷、烯类卤化物、环氧卤代烷的摩尔比为1:(0.8~1.2):(0.8~1.2):(1~1.5)。
作为本发明的一种优选技术方案,其中,所述单卤代氰尿酸包括1-溴-1,3,5-三嗪-2,4,6-三酮和/或1-氯-1,3,5-三嗪-2,4,6-三酮。
作为本发明的一种优选技术方案,其中,所述二氨基卤代烷包括2-氯-N,N-二甲基乙胺、(2-溴甲基)二甲胺、N,N-二甲基-3-氯丙胺、(3-溴丙基)二甲基胺、2-溴-N,N-二乙基乙胺、3-氯-1-二乙氨基丙烷中至少一种。
作为本发明的一种优选技术方案,其中,所述烯类卤化物包括3-氯丙烯、3-溴丙烯、4-氯-1-丁烯、4-溴-1-丁烯中至少一种。
作为本发明的一种优选技术方案,其中,所述环氧卤代烷包括环氧氯丙烷、(4-氯丁基)环氧乙烷、(8-氯辛基)环氧乙烷。
作为本发明的一种优选技术方案,其中,所述环氧氯丙烷、(4-氯丁基)环氧乙烷、(8-氯辛基)环氧乙烷的摩尔比为1:(1~2):(2~3)。
作为本发明的一种优选技术方案,其中,所述氧化石墨烯、氨基烯类化合物、硅烷偶联剂的质量份比为1:(1~2):(0.3~0.5)。
本发明第二方面提供了高阻燃、透气、防静电面料的制备方法,包括以下步骤:所述面料的抗菌内层与阻燃外层通过胶黏剂粘合而成。
有益效果
利用本发明制备的高阻燃、透气、防静电面料具有多种优异性能,具体表现为两种抗菌剂相互协同,在高效抗菌的同时因其独特的内部结构及自身性质,实现多次洗涤后仍具有优异的抗菌性能,体现高耐洗涤效果;多种阻燃剂依据不同的阻燃机理,达到综合阻止、抑制燃烧的目的,与此同时,阻燃剂与棉纤维相互作用,提高高阻燃、透气、防静电面料的拉伸强度。
具体实施方式
下面结合具体实施方式对本发明提供技术方案中的技术特征作进一步清楚、完整的描述,并非对其保护范围的限制。
本发明中的词语“优选的”、“更优选的”等是指,在某些情况下可提供某些有益效果的本发明实施方案。然而,在相同的情况下或其他情况下,其他实施方案也可能是优选的。此外,对一个或多个优选实施方案的表述并不暗示其他实施方案不可用,也并非旨在将其他实施方案排除在本发明的范围之外。
本发明第一方面提供了一种高阻燃、透气、防静电面料,所述面料由抗菌内层与阻燃外层组成,其中,按重量份计,抗菌内层包括棉纤维80~120份、抗菌剂800~1200份,阻燃外层包括棉纤维100~150份、阻燃复合物15~25份。
棉纤维
棉纤维的主要成份是纤维素,纤维素是天然高分子化合物,纤维素的化学结构式由α-葡萄糖为基本结构单元重复构成,其元素组成为碳44.44%、氢6.17%、氧49.39%。此外,棉纤维还附有5%左右的其他物质,称为伴生物,伴生物对纺纱工艺与漂练、印染加工均有影响。棉纤维的表面含有脂蜡质,俗称棉蜡,棉蜡对棉纤维具有保护作用,是棉纤维具有良好纺纱性能的原因之一,但在高温时,棉蜡容易熔融,所以棉布容易绕胶辊。经脱脂处理,原棉吸湿性增加,吸水能力可达本身重量的23~24倍。棉纤维预处理方法主要有:化学处理法、生物酶处理法。
作为一种优选的实施方式,所述棉纤维包括但不限于购自佛山市南海区诗豪纱线有限公司。
在一种优选的实施方式中,所述抗菌内层棉纤维与阻燃外层棉纤维预处理步骤如下:
棉纤维与5g/L的NaOH溶液浴比为1∶(25~35),将棉纤维浸入NaOH溶液中,60~80℃恒温处理20~40min,洗涤、烘干,得到预处理后的棉纤维。
抗菌内层
抗菌剂是指能够在一定时间内,可以让细菌、真菌、酵母菌和病毒等微生物的生长和繁殖保持在必要的水平以下的化学物质。抗菌剂种类主要分为两大类:无机抗菌剂和有机抗菌剂。
在一种优选的实施方式中,所述抗菌剂的制备原料包括单卤代氰尿酸、二氨基卤代烷、烯类卤化物、环氧卤代烷。
在一种优选的实施方式中,所述单卤代氰尿酸、二氨基卤代烷、烯类卤化物、环氧卤代烷的摩尔比为1:(0.8~1.2):(0.8~1.2):(1~1.5)。
更优选地,所述单卤代氰尿酸、二氨基卤代烷、烯类卤化物、环氧卤代烷的摩尔比为1:1:1:1.2。
在一种优选的实施方式中,所述单卤代氰尿酸包括1-溴-1,3,5-三嗪-2,4,6-三酮和/或1-氯-1,3,5-三嗪-2,4,6-三酮。
更优选地,所述单卤代氰尿酸为1-溴-1,3,5-三嗪-2,4,6-三酮。
所述1-溴-1,3,5-三嗪-2,4,6-三酮的CAS号为15114-35-9。
在一种优选的实施方式中,所述二氨基卤代烷的碳原子数为2~6。
在一种优选的实施方式中,所述二氨基卤代烷包括2-氯-N,N-二甲基乙胺、(2-溴甲基)二甲胺、N,N-二甲基-3-氯丙胺、(3-溴丙基)二甲基胺、2-溴-N,N-二乙基乙胺、3-氯-1-二乙氨基丙烷中至少一种。
更优选地,所述二氨基卤代烷为2-氯-N,N-二甲基乙胺。
所述2-氯-N,N-二甲基乙胺的CAS号为107-99-3。
在一种优选的实施方式中,所述烯类卤化物的碳原子数为3~4。
在一种优选的实施方式中,所述烯类卤化物包括3-氯丙烯、3-溴丙烯、4-氯-1-丁烯、4-溴-1-丁烯中至少一种。
更优选地,所述烯类卤化物为3-氯丙烯。
所述3-氯丙烯的CAS号为107-05-1。
在一种优选的实施方式中,所述环氧卤代烷包括环氧氯丙烷、(4-氯丁基)环氧乙烷、(8-氯辛基)环氧乙烷、(3-氯丙基)环氧乙烷、(3-溴丙基)环氧乙烷、(2-溴乙基)环氧乙烷、2-(3-溴丙基)环氧乙烷、6-溴-1,2-环氧己烷中至少一种。
更优选地,所述环氧卤代烷包括环氧氯丙烷、(4-氯丁基)环氧乙烷、(8-氯辛基)环氧乙烷。
所述环氧氯丙烷的CAS号为106-89-8。
所述(4-氯丁基)环氧乙烷的CAS号为81724-56-3。
所述(8-氯辛基)环氧乙烷的CAS号为185559-27-7。
在一种优选的实施方式中,所述环氧氯丙烷、(4-氯丁基)环氧乙烷、(8-氯辛基)环氧乙烷的摩尔比为1:(1~2):(2~3)。
更优选地,所述环氧氯丙烷、(4-氯丁基)环氧乙烷、(8-氯辛基)环氧乙烷的摩尔比为1:1.5:2.5。
在一种优选的实施方式中,所述抗菌内层的制备过程如下:
(1)中间体1的制备过程
1-溴-1,3,5-三嗪-2,4,6-三酮溶于KOH溶液中,反应0.5~1.5h后,向反应体系中加入甲醇再加入烯类卤化物,50~70℃下反应1~3h,在相同的反应温度下,向体系中加入二氨基卤代烷,反应1~3h,重结晶制备中间体1;
(2)棉纤维接枝溶液1的制备过程
将1/3质量份中间体1与环氧氯丙烷加入0.5mol/L盐酸溶液中,20~30℃条件下反应5~8h,得到棉纤维接枝溶液1;
(3)棉纤维接枝溶液2的制备过程
将1/3质量份中间体1与(4-氯丁基)环氧乙烷加入0.5mol/L盐酸溶液中,20~30℃条件下反应5~8h,得到棉纤维接枝溶液2;
(4)将1/3质量份中间体1与(8-氯辛基)环氧乙烷加入0.5mol/L盐酸溶液中,20~30℃条件下反应5~8h,得到棉纤维接枝溶液3;
(5)将预处理后的棉纤维浸渍于棉纤维接枝溶液1中,50~70℃条件下水浴10~30min,去除多余棉纤维接枝溶液1,将浸渍后的棉纤维于60~90℃条件下预烘3~10min;后将棉纤维浸渍于棉纤维接枝溶液2中,50~70℃条件下水浴10~30min,去除多余棉纤维接枝溶液2,于60~90℃条件下预烘3~10min;后浸渍于棉纤维接枝溶液3中,50~70℃条件下水浴10~20min,后在氮气保护条件下,加入偶氮二异丁腈,水浴10~20min,去除多余棉纤维接枝溶液3,于60~90℃条件下预烘20~50min,置于120~140℃烘箱中10~30min,取出后用清水洗净、干燥,并由此纺纱、编织得到抗菌内层。
本申请人发现卤胺杀菌剂具有强大的抗菌功效以及再生性,但导致棉纤维的亲水性有一定的降低;季铵盐杀菌剂具有较强的亲水性以及静电吸附作用,但长期被单独使用容易使其失去杀菌性。将卤胺杀菌剂与季铵盐杀菌剂有效的结合在一起,可以充分发挥两者的优点。两种杀菌剂共用可提高杀菌剂有效负载浓度,从而杀菌性能得到提升。在保留强大的抗菌功效的同时,能凭借季铵盐杀菌剂较强亲水性提高棉纤维的亲水性,同时卤胺杀菌剂可通过简单的次卤素盐卤化,N-H可转化为N-X(X=Cl,Br等),得到氧化态卤化物,再次获得杀菌性能,实现卤胺杀菌剂再生。
本申请人意外的发现,当1-溴-1,3,5-三嗪-2,4,6-三酮、N,N-二甲氨基卤代烷、3-氯丙烯与环氧卤代烷的摩尔比为1:(0.8~1.2):(0.8~1.2):(1~1.5)时,负载双杀菌剂的棉纤维具有更好的耐洗涤性。推测可能的原因为:1-溴-1,3,5-三嗪-2,4,6-三酮在烯基溴化物、N,N-二甲氨基卤代烷改性的过程中,会得到多种形式的中间体:含有单个双键与单个二甲胺功能基的中间体、含有两个双键功能基的中间体、含有两个二甲胺功能基的中间体,上述含二甲胺功能基(含有单个双键与单个二甲胺功能基、含有两个二甲胺功能基)的中间体通过不同链长度的环氧卤代烃与纤维基体接枝在棉纤维表面,形成稳定的季铵盐抗菌表层,并且通过控制不同链长度可有效控制链的柔韧性,同时由于季铵盐的静电斥力,使得中间体能够垂直于棉纤维的表面,减少链缠绕,扩大杀菌剂有效作用面积。同时二氨基卤代烷的碳原子数为2~6,同样可以减少链缠绕,与此同时,烯类卤化物的碳原子数为3~4有利于聚合反应的发生,形成稳定的链段。
同时上述含有单个双键与单个二甲胺功能基的中间体由于季铵盐的静电斥力,能够使得卤胺杀菌剂在季铵盐杀菌剂的上层,自由基聚合形成卤胺杀菌剂链,在清洗的过程当中,因其位阻效应形成季铵盐杀菌剂的第一道保护屏障,同时含有两个双键功能基的中间体因其参与自由基聚合,自由分布在卤胺杀菌剂链的内外两侧,内外两侧自由分布的卤胺杀菌剂相较单个双键与单个二甲胺功能基形成的卤胺杀菌剂自由度较大,当有细菌侵入时,外侧自由分布的卤胺杀菌剂首先进行细菌捕捉,当细菌突破外侧自由分布的卤胺杀菌剂与卤胺杀菌剂链,内侧自由分布的卤胺杀菌剂又可对细菌进行有效捕捉,同时内侧自由分布的卤胺杀菌剂可以增大与季铵盐杀菌剂的啮合度,在清洗的过程中形成季铵盐杀菌剂的第二道保护屏障。与此同时,不同链长度的季铵盐抗菌表层自身因为位阻效应又可以形成自身的保护屏障。若N,N-二甲氨基卤代烷或烯类卤化物的加入量过多,只能形成单形式中间体,无法形成多形式保护屏障;N,N-二甲氨基卤代烷或烯类卤化物的加入量过少,杀菌效率较低。综上所述,多种保护屏障与位阻效应可有效提高棉纤维的耐水洗性。
阻燃外层
阻燃剂是一种能够提高可燃物阻燃和自熄性能的功能化助剂。目前主要应用在天然或合成的高分子材料中,其作用是抑制火焰蔓延,直至自熄,对于防止火灾的发生和保障人们的生命财产安全具有至关重要的意义。阻燃剂按照不同的化学结构主要有无机阻燃剂、卤系阻燃剂、硅系阻燃剂、氮系阻燃剂、膨胀型阻燃剂等。
在一种优选的实施方式中,所述阻燃复合物的制备原料包括氧化石墨烯、氨基烯类化合物、硅烷偶联剂。
在一种优选的实施方式中,所述氧化石墨烯、氨基烯类化合物、硅烷偶联剂的质量份比为1:(1~2):(0.3~0.5)。
更优选地,所述氧化石墨烯、氨基烯类化合物、硅烷偶联剂的质量份比为1:1.5:0.4。
氧化石墨烯
氧化石墨烯(Graphene Oxide,GO)是石墨烯的一种衍生物,是由氧化石墨发生剥离而形成的单层或多层氧化石墨,尽管氧化过程破坏了石墨烯高度共轭结构,但是仍保持着特殊的表面性能与层状结构,为典型的准二维空间结构,其片层上含有很多含氧基团,具有较高的比表面能、良好的亲水性和机械性能,在水和大多数极性有机溶剂中具有很好的分散稳定性。氧化石墨烯片层骨架的基面和边缘上有多种含氧官能团共存的结构,使得氧化石墨烯可以通过调控所含含氧官能团的种类及数量,来调制其导电性和带隙.与石墨烯相比,具有更加优异的性能,具有良好的润湿性能和表面活性,在改善材料的阻燃等综合性能方面发挥着非常重要的作用。
在阻燃方面,氧化石墨烯在材料中阻燃作用如下:
(1)物理隔绝层
氧化石墨烯凭借其特殊的二维片层结构,在材料中层层叠加,形成致密的物理隔绝层,使阻燃性能得到了提升;
(2)隔绝空气层
氧化石墨烯与材料进行交联复合作用,在材料中形成了一层致密的保护膜,能有效的阻隔与空气的接触,在高温或燃烧的过程中降低氧气含量,显著提升了阻燃作用;
(3)在高温或燃烧的情况下,氧化石墨烯会产生CO2和H2O,CO2作为非助燃气体,降低氧气含量,H2O在此过程中接触到炽热的材料,就会变成水蒸气,这时从炽热的材料上夺取大量的热,起到降低温度的效果,同时氧化石墨烯生成更加致密且连续的炭化层结构,进一步起到阻燃作用。
在一种优选的实施方式中,所述氧化石墨烯包括但不限于购自青岛岩海碳材料有限公司。
在一种优选的实施方式中,所述氨基烯类化合物的碳原子数为3~5。
在一种优选的实施方式中,所述氨基烯类化合物包括2-丙烯-1-胺、3-丁烯-1-胺、戊-4-烯-1-胺中至少一种。
更优选地,所述氨基烯类化合物为2-丙烯-1-胺。
所述2-丙烯-1-胺的CAS号为30551-89-4。
硅烷偶联剂
硅烷偶联剂的分子结构式一般为:Y-R-Si(OR)3(式中Y-有机官能基,SiOR-硅烷氧基)。硅烷氧基对无机物具有反应性,有机官能基对有机物具有反应性或相容性。因此,当硅烷偶联剂介于无机和有机界面之间,可形成有机基体-硅烷偶联剂-无机基体的结合层。
在一种优选的实施方式中,所述硅烷偶联剂包括A151(乙烯基三乙氧基硅烷)、A171(乙烯基三甲氧基硅烷)、A172(乙烯基三(β-甲氧乙氧基)硅烷)中至少一种。
更优选地,所述硅烷偶联剂为A151(乙烯基三乙氧基硅烷)。
所述A151(乙烯基三乙氧基硅烷)的CAS号为78-08-0。
在一种优选的实施方式中,所述阻燃复合物的制备方法如下:
(1)将氧化石墨烯加入到A151(乙烯基三乙氧基硅烷)溶液中,20~40℃条件下反应3~7h,洗涤后得到A151(乙烯基三乙氧基硅烷)预插层氧化石墨烯;
(2)在冰浴条件下,将预插层氧化石墨烯加入到2-丙烯-1-胺中,超声处理0.5~1.5h后,搅拌3~7h,将过硫酸铵的盐酸溶液加入上述混合溶液中,反应5~10h后将产物洗涤干燥,得到阻燃复合物。
在一种优选的实施方式中,所述阻燃外层的制备方法如下:
(1)将阻燃复合物在去离子中超声10~30min,得到阻燃复合物分散液;
(2)将预处理棉纤维浸渍于阻燃复合物分散液中,浸渍温度为50~100℃,浸渍时间为1~2h,于60~90℃条件下预烘3~10min,置于120~140℃烘箱中10~30min,取出后用清水洗净、干燥,并由此纺纱、编织得到阻燃外层。
本申请人发现氧化石墨烯与棉纤维通过作用力,独特的片层结构在棉纤维中层层叠加,形成物理阻燃层,使得阻燃性能提升,另一方面,在高温的情况下,氧化石墨烯会产生CO2和H2O,同时生成致密且连续的炭化层结构,进一步起到阻燃作用。氨基烯类化合物作为氮系阻燃剂,氮系阻燃剂在燃烧过程中释放出水、氮气、二氧化碳、氨气等不燃性气体,从而降低氧气含量,起到气相阻燃效果。硅烷偶联剂作为硅系阻燃剂,硅系阻燃剂的机理主要是迁移阻隔机理,即在燃烧的过程中,硅系阻燃剂迁移至表面,同时形成均质的绝热炭化(Si-C)层,起到阻隔内部与外界氧气接触的作用。氧化石墨烯与氮系阻燃剂、硅系阻燃剂相互配合,形成多层类三明治结构,能够形成更加高效的复合阻燃剂。
本申请人意外发现,当氧化石墨烯与氨基烯类化合物、乙烯基三甲氧基硅烷加入量的质量份比为1:(1~2):(0.3~0.5)时,棉纤维的力学性能和阻燃提升;通过乙烯基三甲氧基硅烷预插层,使得层间作用力受到破坏,氨基烯类化合物更易进入氧化石墨烯层,而且当氨基烯类化合物的碳原子数为3~5时,氨基烯类更加容易进入氧化石墨烯层,减少链段缠绕的同时,能够引入更多的氮系阻燃剂,此外,在聚合的过程中引发受限膨胀效应,且聚合放热能够提供内在驱动力,进一步扩大石墨烯层之间的距离,实现动态扩层的效果,最终形成一种特殊的三维杂化结构。插层处理后的氧化石墨烯在与棉纤维相互作用的过程中因为层间距的增大,氧化石墨烯层与层之间的作用力变小,且氨基烯类化合物插层后聚合形成柔性链,同时由于机械剪切作用,使得氧化石墨烯片层之间相互错位偏移,使得棉纤维在拉伸的过程中,一方面拉伸应力部分转移至插层氧化石墨烯上,出现应力分散,另一方面,不仅需要克服棉纤维本身的拉伸应力,同时氧化石墨烯的插层结构也抵消了部分应力,故而增强棉纤维的拉伸强度。与此同时,错位偏移后暴露出的氨基烯类化合物含有大量的氨基,易与棉纤维表面相互作用,在改变棉纤维表面极性、降低表面斥力的同时,提高拉伸强度。
当氧化石墨烯与氨基烯类化合物、乙烯基三甲氧基硅烷加入量的质量份比为1:(1~2):(0.3~0.5)时,阻燃效果提升,在此范围中,高温的情况下,氧化石墨烯可形成有效的物理阻燃层,并且生成致密且连续的炭化层结构,同时氧化石墨烯与氮系阻燃剂、硅系阻燃剂形成的多层类三明治结构使得棉纤维得到层层保护。当氨基烯类化合物的加入量过多时,导致氧化石墨烯层间距过大,最终形成相距较远的单片层氧化石墨烯负载氨基烯类化合物与乙烯基三甲氧基硅烷,失去了氧化石墨烯片层结构层层叠加形成物理阻燃层的效果,只有合适的片层间距,才能够使得氧化石墨烯与氮系阻燃剂、硅系阻燃剂相互配合效果更好,形成更加高效的复合阻燃剂。
本发明第二方面提供了高阻燃、透气、防静电面料的制备方法,包括以下步骤:所述面料的抗菌内层与阻燃外层通过胶黏剂粘合而成。
另外,如果没有其它说明,所用原料都是市售得到的。
实施例1
本发明的实施例1提供了一种高阻燃、透气、防静电面料,所述面料由抗菌内层与阻燃外层组成,其中,按重量份计,抗菌内层包括棉纤维100份、抗菌剂1000份,阻燃外层包括棉纤维125份、阻燃复合物20份。
所述抗菌剂的制备原料包括1-溴-1,3,5-三嗪-2,4,6-三酮、2-氯-N,N-二甲基乙胺、3-氯丙烯、环氧卤代烷;
所述环氧卤代烷包括环氧氯丙烷、(4-氯丁基)环氧乙烷、(8-氯辛基)环氧乙烷;
所述抗菌剂的制备方法为:
(1)中间体1的制备过程
1-溴-1,3,5-三嗪-2,4,6-三酮(1mmol)溶于含有2m mol KOH的500mL水溶液中,反应1h后,向反应体系中加入100mL甲醇,混合均匀后,再加入3-氯丙烯(1mmol),60℃下反应2h,在相同的反应温度下,向体系中加入2-氯-N,N-二甲基乙胺(1mmol),反应2h,重结晶制备中间体1;
(2)棉纤维接枝溶液1的制备过程
在室温条件下,将1/3质量份中间体1加入300mL 5mmol/L盐酸溶液中搅拌20min,加入环氯丙烷(0.24mmol),25℃条件下反应6h,得到棉纤维接枝溶液1;
(3)棉纤维接枝溶液2的制备过程
在室温条件下,将1/3质量份中间体1加入300mL 5mmol/L盐酸溶液中搅拌20min,加入(4-氯丁基)环氧乙烷(0.36mmol),25℃条件下反应6h,得到棉纤维接枝溶液2;
(4)在室温条件下,将1/3质量份中间体1加入300mL 5mmol/L盐酸溶液中搅拌20min,加入(8-氯辛基)环氧乙烷(0.6mmol),25℃条件下反应6h,得到棉纤维接枝溶液3。
所述抗菌剂包括棉纤维接枝溶液1、棉纤维接枝溶液2、棉纤维接枝溶液3,且棉纤维接枝溶液1、棉纤维接枝溶液2、棉纤维接枝溶液3的体积为1:1:1;
所述阻燃复合物的制备原料包括氧化石墨烯、氨基烯类化合物、硅烷偶联剂;
所述阻燃复合物的制备如下:
(1)将0.04g A151(乙烯基三乙氧基硅烷)加入到200mL乙醇与水混合溶液(体积比为1:1)中,将0.1g氧化石墨烯加入到上述体系中,30℃条件下反应5h,洗涤后得到A151(乙烯基三乙氧基硅烷)预插层氧化石墨烯;
(2)在冰浴条件下,将预插层氧化石墨烯、2-丙烯-1-胺(0.15g)加入到300mL5mmol/L的盐酸溶液中,超声处理1h后,搅拌5h,将过硫酸铵(0.03g)加入上述混合溶液中,反应7h后将产物洗涤干燥,得到阻燃复合物。
所述高阻燃、透气、防静电面料的制备方法如下:
A.棉纤维预处理
棉纤维与5g/L的NaOH溶液浴比为1∶(25~35),将棉纤维浸入5g/L的NaOH溶液中,70℃恒温处理30min,水洗至中性,50℃烘干,得到预处理后的棉纤维。
B.抗菌内层的制备
将预处理后的棉纤维浸渍于棉纤维接枝溶液1中,60℃条件下水浴20min,去除多余棉纤维接枝溶液1,将浸渍后的棉纤维于70℃条件下预烘5min;后将棉纤维浸渍于棉纤维接枝溶液2中,60℃条件下水浴20min,去除多余棉纤维接枝溶液2,于70℃条件下预烘5min;后浸渍于棉纤维接枝溶液3中,60℃条件下水浴15min,后在氮气保护条件下,加入偶氮二异丁腈(0.1g),水浴150min,去除多余棉纤维接枝溶液3,于70℃条件下预烘35min,置于130℃烘箱中20min,取出后用清水洗净、干燥,并由此纺纱、编织得到抗菌内层。
C.阻燃外层的制备
(1)将阻燃复合物在500mL去离子水中超声20min,得到阻燃复合物分散液;
(2)将预处理棉纤维浸渍于阻燃复合物分散液中,浸渍温度为70℃,浸渍时间为1.5h,于70℃条件下预烘5min,置于130℃烘箱中20min,取出后用清水洗净、干燥,并由此纺纱、编织得到阻燃外层。
D.高阻燃、透气、防静电面料的制备
将抗菌内层与阻燃外层通过胶黏剂粘合制备高阻燃、透气、防静电面料。
实施例2
本发明的实施例2提供了一种高阻燃、透气、防静电面料,所述面料由抗菌内层与阻燃外层组成,其中,按重量份计,抗菌内层包括棉纤维80份、抗菌剂800份,阻燃外层包括棉纤维100份、阻燃复合物15份。
所述抗菌剂的制备原料包括1-溴-1,3,5-三嗪-2,4,6-三酮、2-氯-N,N-二甲基乙胺、3-氯丙烯、环氧卤代烷;
所述环氧卤代烷包括环氧氯丙烷、(4-氯丁基)环氧乙烷、(8-氯辛基)环氧乙烷;
所述抗菌剂的制备方法为:
(1)中间体1的制备过程
1-溴-1,3,5-三嗪-2,4,6-三酮(1mmol)溶于含有2m mol KOH的500mL水溶液中,反应1h后,向反应体系中加入100mL甲醇,混合均匀后,再加入3-氯丙烯(1mmol),60℃下反应2h,在相同的反应温度下,向体系中加入2-氯-N,N-二甲基乙胺(1mmol),反应2h,重结晶制备中间体1;
(2)棉纤维接枝溶液1的制备过程
在室温条件下,将1/3质量份中间体1加入300mL 5mmol/L盐酸溶液中搅拌20min,加入环氯丙烷(0.24mmol),25℃条件下反应6h,得到棉纤维接枝溶液1;
(3)棉纤维接枝溶液2的制备过程
在室温条件下,将1/3质量份中间体1加入300mL 5mmol/L盐酸溶液中搅拌20min,加入(4-氯丁基)环氧乙烷(0.36mmol),25℃条件下反应6h,得到棉纤维接枝溶液2;
(4)在室温条件下,将1/3质量份中间体1加入300mL 5mmol/L盐酸溶液中搅拌20min,加入(8-氯辛基)环氧乙烷(0.6mmol),25℃条件下反应6h,得到棉纤维接枝溶液3;
所述抗菌剂包括棉纤维接枝溶液1、棉纤维接枝溶液2、棉纤维接枝溶液3,且棉纤维接枝溶液1、棉纤维接枝溶液2、棉纤维接枝溶液3的体积为1:1:1;
阻燃复合物的制备原料包括氧化石墨烯、氨基烯类化合物、硅烷偶联剂;
所述阻燃复合物的制备如下:
(1)将0.04g A151(乙烯基三乙氧基硅烷)加入到200mL乙醇/水混合溶液(体积比为1:1)中,将0.1g氧化石墨烯加入到上述体系中,30℃条件下反应5h,洗涤后得到A151(乙烯基三乙氧基硅烷)预插层氧化石墨烯;
(2)在冰浴条件下,将预插层氧化石墨烯、2-丙烯-1-胺(0.15g)加入到300mL5mmol/L的盐酸溶液中,超声处理1h后,搅拌5h,将过硫酸铵(0.03g)加入上述混合溶液中,反应7h后将产物洗涤干燥,得到阻燃复合物。
所述高阻燃、透气、防静电面料的制备方法如下:
A.棉纤维预处理
棉纤维与5g/L的NaOH溶液浴比为1∶(25~35),将棉纤维浸入5g/L的NaOH溶液中,70℃恒温处理30min,水洗至中性,50℃烘干,得到预处理后的棉纤维。
B.抗菌内层的制备
将预处理后的棉纤维浸渍于棉纤维接枝溶液1中,60℃条件下水浴20min,去除多余棉纤维接枝溶液1,将浸渍后的棉纤维于70℃条件下预烘5min;后将棉纤维浸渍于棉纤维接枝溶液2中,60℃条件下水浴20min,去除多余棉纤维接枝溶液2,于70℃条件下预烘5min;后浸渍于棉纤维接枝溶液3中,60℃条件下水浴15min,后在氮气保护条件下,加入偶氮二异丁腈(0.1g),水浴150min,去除多余棉纤维接枝溶液3,于70℃条件下预烘35min,置于130℃烘箱中20min,取出后用清水洗净、干燥,并由此纺纱、编织得到抗菌内层。
C.阻燃外层的制备
(1)将阻燃复合物在500mL去离子水中超声20min,得到阻燃复合物分散液;
(2)将预处理棉纤维浸渍于阻燃复合物分散液中,浸渍温度为70℃,浸渍时间为1.5h,于70℃条件下预烘5min,置于130℃烘箱中20min,取出后用清水洗净、干燥,并由此纺纱、编织得到阻燃外层。
D.高阻燃、透气、防静电面料的制备
将抗菌内层与阻燃外层通过胶黏剂粘合制备高阻燃、透气、防静电面料。
实施例3
本发明的实施例3提供了一种高阻燃、透气、防静电面料,所述面料由抗菌内层与阻燃外层组成,其中,按重量份计,抗菌内层包括棉纤维120份、抗菌剂1200份,阻燃外层包括棉纤维150份、阻燃复合物25份。
所述抗菌剂的制备原料包括1-溴-1,3,5-三嗪-2,4,6-三酮、2-氯-N,N-二甲基乙胺、3-氯丙烯、环氧卤代烷;
所述环氧卤代烷包括环氧氯丙烷、(4-氯丁基)环氧乙烷、(8-氯辛基)环氧乙烷;
所述抗菌剂的制备方法为:
(1)中间体1的制备过程
1-溴-1,3,5-三嗪-2,4,6-三酮(1mmol)溶于含有2m mol KOH的500mL水溶液中,反应1h后,向反应体系中加入100mL甲醇,混合均匀后,再加入3-氯丙烯(1mmol),60℃下反应2h,在相同的反应温度下,向体系中加入2-氯-N,N-二甲基乙胺(1mmol),反应2h,重结晶制备中间体1;
(2)棉纤维接枝溶液1的制备过程
在室温条件下,将1/3质量份中间体1加入300mL 5mmol/L盐酸溶液中搅拌20min,加入环氯丙烷(0.24mmol),25℃条件下反应6h,得到棉纤维接枝溶液1;
(3)棉纤维接枝溶液2的制备过程
在室温条件下,将1/3质量份中间体1加入300mL 5mmol/L盐酸溶液中搅拌20min,加入(4-氯丁基)环氧乙烷(0.36mmol),25℃条件下反应6h,得到棉纤维接枝溶液2;
(4)在室温条件下,将1/3质量份中间体1加入300mL 5mmol/L盐酸溶液中搅拌20min,加入(8-氯辛基)环氧乙烷(0.6mmol),25℃条件下反应6h,得到棉纤维接枝溶液3;
所述抗菌剂包括棉纤维接枝溶液1、棉纤维接枝溶液2、棉纤维接枝溶液3,且棉纤维接枝溶液1、棉纤维接枝溶液2、棉纤维接枝溶液3的体积为1:1:1。
阻燃复合物的制备原料包括氧化石墨烯、氨基烯类化合物、硅烷偶联剂;
所述阻燃复合物的制备如下:
(1)将0.04g A151(乙烯基三乙氧基硅烷)加入到200mL乙醇与水混合溶液(体积比为1:1)中,将0.1g氧化石墨烯加入到上述体系中,30℃条件下反应5h,洗涤后得到A151(乙烯基三乙氧基硅烷)预插层氧化石墨烯;
(2)在冰浴条件下,将预插层氧化石墨烯、2-丙烯-1-胺(0.15g)加入到300mL5mmol/L的盐酸溶液中,超声处理1h后,搅拌5h,将过硫酸铵(0.03g)加入上述混合溶液中,反应7h后将产物洗涤干燥,得到阻燃复合物;
所述氧化石墨烯、2-丙烯-1-胺、A151(乙烯基三乙氧基硅烷)的质量份比为1:1.5:0.4。
所述高阻燃、透气、防静电面料的制备方法如下:
A.棉纤维预处理
棉纤维与5g/L的NaOH溶液浴比为1∶(25~35),将棉纤维浸入5g/L的NaOH溶液中,70℃恒温处理30min,水洗至中性,50℃烘干,得到预处理后的棉纤维。
B.抗菌内层的制备
将预处理后的棉纤维浸渍于棉纤维接枝溶液1中,60℃条件下水浴20min,去除多余棉纤维接枝溶液1,将浸渍后的棉纤维于70℃条件下预烘5min;后将棉纤维浸渍于棉纤维接枝溶液2中,60℃条件下水浴20min,去除多余棉纤维接枝溶液2,于70℃条件下预烘5min;后浸渍于棉纤维接枝溶液3中,60℃条件下水浴15min,后在氮气保护条件下,加入偶氮二异丁腈(0.1g),水浴150min,去除多余棉纤维接枝溶液3,于70℃条件下预烘35min,置于130℃烘箱中20min,取出后用清水洗净、干燥,并由此纺纱、编织得到抗菌内层。
C.阻燃外层的制备
(1)将阻燃复合物在500mL去离子中超声20min,得到阻燃复合物分散液;
(2)将预处理棉纤维浸渍于阻燃复合物分散液中,浸渍温度为70℃,浸渍时间为1.5h,于70℃条件下预烘5min,置于130℃烘箱中20min,取出后用清水洗净、干燥,并由此纺纱、编织得到阻燃外层。
D.高阻燃、透气、防静电面料的制备
将抗菌内层与阻燃外层通过胶黏剂粘合制备高阻燃、透气、防静电面料。
实施例4
本发明的实施例4提供了一种高阻燃、透气、防静电面料,所述面料由抗菌内层与阻燃外层组成,其中,按重量份计,抗菌内层包括棉纤维100份、抗菌剂1000份,阻燃外层包括棉纤维125份、阻燃复合物20份。
其具体实施方式同实施例1,不同之处在于,所述环氧卤代烷仅为环氧氯丙烷。
实施例5
本发明的实施例5提供了一种高阻燃、透气、防静电面料,所述面料由抗菌内层与阻燃外层组成,其中,按重量份计,抗菌内层包括棉纤维100份、抗菌剂1000份,阻燃外层包括棉纤维125份、阻燃复合物20份。
其具体实施方式同实施例1,不同之处在于,所述环氧卤代烷仅为(4-氯丁基)环氧乙烷。
实施例6
本发明的实施例6提供了一种高阻燃、透气、防静电面料,所述面料由抗菌内层与阻燃外层组成,其中,按重量份计,抗菌内层包括棉纤维100份、抗菌剂1000份,阻燃外层包括棉纤维125份、阻燃复合物20份。
其具体实施方式同实施例1,不同之处在于,所述环氧卤代烷仅为(8-氯辛基)环氧乙烷。
实施例7
本发明的实施例7提供了一种高阻燃、透气、防静电面料,所述面料由抗菌内层与阻燃外层组成,其中,按重量份计,抗菌内层包括棉纤维100份、抗菌剂1000份,阻燃外层包括棉纤维125份、阻燃复合物20份。
其具体实施方式同实施例1,不同之处在于,所述环氧卤代烷仅为环氧氯丙烷与(8-氯辛基)环氧乙烷。
实施例8
本发明的实施例8提供了一种高阻燃、透气、防静电面料,所述面料由抗菌内层与阻燃外层组成,其中,按重量份计,抗菌内层包括棉纤维100份、抗菌剂1000份,阻燃外层包括棉纤维125份、阻燃复合物20份。
其具体实施方式同实施例1,不同之处在于,所述2-氯-N,N-二甲基乙胺替换为6-氯-N,N-二甲基-1-己胺(CAS号:82874-32-6)。
实施例9
本发明的实施例9提供了一种高阻燃、透气、防静电面料,所述面料由抗菌内层与阻燃外层组成,其中,按重量份计,抗菌内层包括棉纤维100份、抗菌剂1000份,阻燃外层包括棉纤维125份、阻燃复合物20份。
其具体实施方式同实施例1,不同之处在于,所述3-氯丙烯替换为8-氯-1-辛烯。
实施例10
本发明的实施例10提供了一种高阻燃、透气、防静电面料,所述面料由抗菌内层与阻燃外层组成,其中,按重量份计,抗菌内层包括棉纤维100份、抗菌剂1000份,阻燃外层包括棉纤维125份、阻燃复合物20份。
其具体实施方式同实施例1,不同之处在于,所述1-溴-1,3,5-三嗪-2,4,6-三酮与环氧卤代烷的比例为1:0.8。
实施例11
本发明的实施例11提供了一种高阻燃、透气、防静电面料,所述面料由抗菌内层与阻燃外层组成,其中,按重量份计,抗菌内层包括棉纤维100份、抗菌剂1000份,阻燃外层包括棉纤维125份、阻燃复合物20份。
其具体实施方式同实施例1,不同之处在于,所述环氧氯丙烷、(4-氯丁基)环氧乙烷、(8-氯辛基)环氧乙烷的相对浓度比为1:1:1。
实施例12
本发明的实施例12提供了一种高阻燃、透气、防静电面料,所述面料由抗菌内层与阻燃外层组成,其中,按重量份计,抗菌内层包括棉纤维100份、抗菌剂1000份,阻燃外层包括棉纤维125份、阻燃复合物20份。
其具体实施方式同实施例1,不同之处在于,所述阻燃复合物的制备原料不包括硅烷偶联剂、2-丙烯-1-胺。
实施例13
本发明的实施例13提供了一种高阻燃、透气、防静电面料,所述面料由抗菌内层与阻燃外层组成,其中,按重量份计,抗菌内层包括棉纤维100份、抗菌剂1000份,阻燃外层包括棉纤维125份、阻燃复合物20份。
其具体实施方式同实施例1,不同之处在于,所述阻燃复合物的制备原料不包括氧化石墨烯、硅烷偶联剂。
实施例14
本发明的实施例14提供了一种高阻燃、透气、防静电面料,所述面料由抗菌内层与阻燃外层组成,其中,按重量份计,抗菌内层包括棉纤维100份、抗菌剂1000份,阻燃外层包括棉纤维125份、阻燃复合物20份。
其具体实施方式同实施例1,不同之处在于,所述阻燃复合物的制备原料不包括氧化石墨烯、2-丙烯-1-胺。
实施例15
本发明的实施例15提供了一种高阻燃、透气、防静电面料,所述面料由抗菌内层与阻燃外层组成,其中,按重量份计,抗菌内层包括棉纤维100份、抗菌剂1000份,阻燃外层包括棉纤维125份、阻燃复合物20份。
其具体实施方式同实施例1,不同之处在于,所述氧化石墨烯与2-丙烯-1-胺的摩尔比为1:3。
实施例16
本发明的实施例16提供了一种高阻燃、透气、防静电面料,所述面料由抗菌内层与阻燃外层组成,其中,按重量份计,抗菌内层包括棉纤维100份、抗菌剂1000份,阻燃外层包括棉纤维125份、阻燃复合物20份。
其具体实施方式同实施例1,不同之处在于,所述阻燃复合物的制备原料仅为氧化石墨烯与2-丙烯-1-胺。
实施例17
本发明的实施例17提供了一种高阻燃、透气、防静电面料,所述面料由抗菌内层与阻燃外层组成,其中,按重量份计,抗菌内层包括棉纤维100份、抗菌剂1000份,阻燃外层包括棉纤维125份、阻燃复合物20份。
其具体实施方式同实施例1,不同之处在于,所述2-丙烯-1-胺替换为7-辛烯-1-胺(CAS号:82223-49-2)。
性能评价
(1)抗菌性
选用大肠杆菌(O157:H7 ATCC 11229)和金黄色葡萄球菌(ATCC 6538P)作为待测细菌,根据AATCC100-199抗菌性能测试方法。将浓度为107cuf/mL左右的待测细菌置于pH=7磷酸盐缓冲液中,常温下将25ul细菌缓冲液滴加到两片叠加的高阻燃、透气、防静电面料表面,后另将两片叠加的高阻燃、透气、防静电面料置于细菌缓冲液上方并挤压,15min后将四片高阻燃、透气、防静电面料加入20mL无菌pH=7磷酸盐缓冲液中,此缓冲液中加入0.5mL的0.05N Na2S2O3溶液,搅拌洗涤稀释,在37℃条件下培养24h,进行平皿计数确定存活菌落数,计算抑菌率。
(2)耐洗涤性
将高阻燃、透气、防静电面料浸渍在0.5%的洗涤剂中20min后用自来水洗净,然后用蒸馏水冲洗后在45℃条件下干燥2h,每洗涤10次进行一次测试,测试三次,根据AATCC100-199抗菌性能测试方法计算抑菌率。
(3)再生性
高阻燃、透气、防静电面料的氧化态抗菌有效含量可采用间接碘量法测试。精确称取高阻燃、透气、防静电面料,加入到含有80mL 0.025N H2SO4水溶液的锥形瓶中,加入0.1gKI,充分摇匀后,滴加0.5%的淀粉溶液作为指示剂,用0.01N的Na2S2O3溶液滴定,直至蓝色消失即为滴定终点。根据下列公式计算氧化态抗菌有效含量
N和V分别代表Na2S2O3溶液的浓度(mol/L)和体积(L),W为高阻燃、透气、防静电面料的质量(g)。
再生性能测试可以通过使用硫代硫酸钠将高阻燃、透气、防静电面料中的N-X键还原成N-H键,然后再次氯化来考察。将高阻燃、透气、防静电面料用硫代硫酸钠还原后,再在次氯酸钠溶液中氯化,洗涤45℃下鼓风干燥。通过碘量法测定样品中氧化态抗菌有效含量。
(4)阻燃性
参照GB/T 2406.2—2009标准,测定阻燃PBT样品的极限氧指数(LOI)。
(5)拉伸性能
按GB/T 1447—2005测量试样的拉伸性能,仪器测试速度为10mm/min,每组测量4个试样并取其平均值。
通过性能测试发现,本发明制备的高阻燃、透气、防静电面料具有优良的抗菌性能、再生性能与阻燃性能,同时展现了优异的耐洗涤性能,而且面料具有良好的拉伸强度。
以上所述,仅是本发明的较佳实施例而已,并非是对发明作其他形式的限制,任何熟悉本专业的技术人员可能利用上述揭示的技术内容加以变更或更改为等同变化的等效实施例,但是凡是未脱离本发明技术方案内容,依据本发明的技术实质对以上实施例所作的任何简单修改,等同变化与改型,仍属于本发明技术方案的保护范围。
Claims (10)
1.一种高阻燃、透气、防静电面料,其特征在于,所述面料由抗菌内层与阻燃外层组成,其中,按重量份计,抗菌内层包括棉纤维80~120份、抗菌剂800~1200份,阻燃外层包括棉纤维100~150份、阻燃复合物15~25份。
2.根据权利要求1所述高阻燃、透气、防静电面料,其特征在于,所述抗菌剂的制备原料包括单卤代氰尿酸、二氨基卤代烷、烯类卤化物、环氧卤代烷,所述阻燃复合物的制备原料包括氧化石墨烯、氨基烯类化合物、硅烷偶联剂。
3.根据权利要求2所述高阻燃、透气、防静电面料,其特征在于,所述单卤代氰尿酸、二氨基卤代烷、烯类卤化物、环氧卤代烷的摩尔比为1:(0.8~1.2):(0.8~1.2):(1~1.5)。
4.根据权利要求2~3任一项所述高阻燃、透气、防静电面料,其特征在于,所述单卤代氰尿酸包括1-溴-1,3,5-三嗪-2,4,6-三酮和/或1-氯-1,3,5-三嗪-2,4,6-三酮。
5.根据权利要求2~3任一项所述高阻燃、透气、防静电面料,其特征在于,所述二氨基卤代烷包括2-氯-N,N-二甲基乙胺、(2-溴甲基)二甲胺、N,N-二甲基-3-氯丙胺、(3-溴丙基)二甲基胺、2-溴-N,N-二乙基乙胺、3-氯-1-二乙氨基丙烷中至少一种。
6.根据权利要求2~3任一项所述高阻燃、透气、防静电面料,其特征在于,所述烯类卤化物包括3-氯丙烯、3-溴丙烯、4-氯-1-丁烯、4-溴-1-丁烯中至少一种。
7.根据权利要求2~3任一项所述高阻燃、透气、防静电面料,其特征在于,所述环氧卤代烷包括环氧氯丙烷、(4-氯丁基)环氧乙烷、(8-氯辛基)环氧乙烷。
8.根据权利要求7所述高阻燃、透气、防静电面料,其特征在于,所述环氧氯丙烷、(4-氯丁基)环氧乙烷、(8-氯辛基)环氧乙烷的摩尔比为1:(1~2):(2~3)。
9.根据权利要求2所述高阻燃、透气、防静电面料,其特征在于,所述氧化石墨烯、氨基烯类化合物、硅烷偶联剂的质量份比为1:(1~2):(0.3~0.5)。
10.一种根据权利要求1~9任一项所述高阻燃、透气、防静电面料的制备方法,其特征在于,包括以下步骤:所述面料的抗菌内层与阻燃外层通过胶黏剂粘合而成。
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