CN116905216A - 一种抗菌透气面料的制备工艺 - Google Patents
一种抗菌透气面料的制备工艺 Download PDFInfo
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- 229920001778 nylon Polymers 0.000 claims abstract description 68
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims abstract description 36
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- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000007788 liquid Substances 0.000 claims abstract description 13
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 10
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- VVJKKWFAADXIJK-UHFFFAOYSA-N Allylamine Chemical compound NCC=C VVJKKWFAADXIJK-UHFFFAOYSA-N 0.000 claims description 54
- FYSNRJHAOHDILO-UHFFFAOYSA-N thionyl chloride Chemical compound ClS(Cl)=O FYSNRJHAOHDILO-UHFFFAOYSA-N 0.000 claims description 42
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 38
- 238000003756 stirring Methods 0.000 claims description 36
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- 238000002156 mixing Methods 0.000 claims description 32
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- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 13
- 239000000243 solution Substances 0.000 claims description 13
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 12
- 239000002253 acid Substances 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 12
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- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 12
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- ZBMGMUODZNQAQI-UHFFFAOYSA-N dimethyl(prop-2-enyl)silicon Chemical compound C[Si](C)CC=C ZBMGMUODZNQAQI-UHFFFAOYSA-N 0.000 claims description 9
- 239000012530 fluid Substances 0.000 claims description 9
- UHUUYVZLXJHWDV-UHFFFAOYSA-N trimethyl(methylsilyloxy)silane Chemical compound C[SiH2]O[Si](C)(C)C UHUUYVZLXJHWDV-UHFFFAOYSA-N 0.000 claims description 9
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- 229910052760 oxygen Inorganic materials 0.000 abstract description 5
- 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 abstract description 3
- HMDDXIMCDZRSNE-UHFFFAOYSA-N [C].[Si] Chemical compound [C].[Si] HMDDXIMCDZRSNE-UHFFFAOYSA-N 0.000 abstract description 3
- 238000009395 breeding Methods 0.000 abstract description 3
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- 239000003063 flame retardant Substances 0.000 abstract description 3
- 238000006459 hydrosilylation reaction Methods 0.000 abstract description 3
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- LOUPRKONTZGTKE-WZBLMQSHSA-N Quinine Chemical compound C([C@H]([C@H](C1)C=C)C2)C[N@@]1[C@@H]2[C@H](O)C1=CC=NC2=CC=C(OC)C=C21 LOUPRKONTZGTKE-WZBLMQSHSA-N 0.000 description 2
- 239000002262 Schiff base Substances 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 201000010099 disease Diseases 0.000 description 2
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 235000001258 Cinchona calisaya Nutrition 0.000 description 1
- 241000588724 Escherichia coli Species 0.000 description 1
- 206010048038 Wound infection Diseases 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- -1 chlorine ions Chemical class 0.000 description 1
- LOUPRKONTZGTKE-UHFFFAOYSA-N cinchonine Natural products C1C(C(C2)C=C)CCN2C1C(O)C1=CC=NC2=CC=C(OC)C=C21 LOUPRKONTZGTKE-UHFFFAOYSA-N 0.000 description 1
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- 229960000948 quinine Drugs 0.000 description 1
- 230000001850 reproductive effect Effects 0.000 description 1
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Classifications
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04C—BRAIDING OR MANUFACTURE OF LACE, INCLUDING BOBBIN-NET OR CARBONISED LACE; BRAIDING MACHINES; BRAID; LACE
- D04C1/00—Braid or lace, e.g. pillow-lace; Processes for the manufacture thereof
- D04C1/02—Braid or lace, e.g. pillow-lace; Processes for the manufacture thereof made from particular materials
-
- 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
- D01D5/0007—Electro-spinning
- D01D5/0015—Electro-spinning characterised by the initial state of the material
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/02—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D01F6/16—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds from polymers of unsaturated carboxylic acids or unsaturated organic esters, e.g. polyacrylic esters, polyvinyl acetate
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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
- D06M11/07—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 halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof
- D06M11/30—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 halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof with oxides of halogens, oxyacids of halogens or their salts, e.g. with perchlorates
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- 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
- D06M11/51—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 sulfur, selenium, tellurium, polonium or compounds thereof
- D06M11/52—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 sulfur, selenium, tellurium, polonium or compounds thereof with selenium, tellurium, polonium or their compounds; with sulfur, dithionites or compounds containing sulfur and halogens, with or without oxygen; by sulfohalogenation with chlorosulfonic acid; by sulfohalogenation with a mixture of sulfur dioxide and free halogens
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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
- D06M13/35—Heterocyclic compounds
- D06M13/355—Heterocyclic compounds having six-membered heterocyclic rings
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- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/643—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
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- D10B2331/00—Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products
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Abstract
本发明涉及纺织材料技术领域,具体为一种抗菌透气面料的制备工艺,S1:辐射聚丙烯酸后静电纺丝制得多孔锦纶;S2:将氨基聚硅碳烷和酰氯化多孔锦纶反应制得预改性多孔锦纶;S3:预改性多孔锦纶经过抗菌剂、次氯酸钠处理制得改性多孔锦纶;S4:多孔锦纶和改性多孔锦纶加捻织编成抗菌透气面料。本发明的优点在于:辐射处理后聚丙烯酸交联形成三维网络,提高了面料的力学形成;静电纺丝时加入聚乙二醇,提高面料的吸湿排液与排湿透气的性能,从而减少细菌与病毒的滋生,提高穿着者肌肤的舒适感;生成硅碳层覆盖在纤维表面隔绝热量和氧气,提高了面料的阻燃性能,通过硅氢加成进行固定抗菌剂,提高了面料的抗菌性能,提高了面料抗菌能力的持久性与稳定性。
Description
技术领域
本发明涉及纺织材料技术领域,具体为一种抗菌透气面料的制备工艺。
背景技术
细菌,作为人类生活环境中分布最广泛的一类微生物,不仅无处不在,而且种类繁多、适应能力强、繁殖能力快。尤其是一些有害致病菌,严重威胁着人类健康,不仅可以通过直接接触,加重伤口感染及病情恶化;而且还可以通过污染周边环境,如水、食物、空气、衣物等,侵入人体,使人致病。
而纺织品作为人类生活必不可少的功能性用品,由于其自身微孔结构,极易吸附沾染微生物,加之,人体表面适宜的温湿度,分泌的油脂、汗液等,在某些特殊情况下为微生物的繁殖、滋生创造了有利条件。如何快速有效杀灭致病菌,阻碍其在纺织品中的代谢滋生,以解决细菌性污染和疾病显得尤为重要。加之,现代纺织科学技术的快速发展和人们对纺织品功能性、舒适性需求的提升,那些具有特殊功能的纺织品往往更容易受到消费者的青睐。因此,研发一种具有良好抗菌效果的面料具有重大的市场价值。
发明内容
本发明的目的在于提供一种抗菌透气面料的制备工艺,以解决现有技术中存在的问题。
一种抗菌透气面料的制备工艺,主要包括以下制备步骤:
(S1)纺丝:将辐射处理后的聚丙烯酸进行静电纺丝制得多孔锦纶;
(S2)预改性:用氯化亚砜对多孔锦纶处理制得酰氯化多孔锦纶;将烯丙基胺和四甲基二硅氧烷反应后再和烯丙基二甲基硅烷反应制得氨基聚硅碳烷;将氨基聚硅碳烷和酰氯化多孔锦纶反应制得预改性多孔锦纶;
(S3)改性:将4-烯丙氧基苯甲醛和N-氨乙基哌嗪反应制得抗菌剂;将预改性多孔锦纶经过抗菌剂处理后,再用次氯酸钠处理,制得改性多孔锦纶;
(S4)织造:将多孔锦纶和改性多孔锦纶加捻后,织编成抗菌透气面料。
作为优化,所述抗菌透气面料的制备工艺主要包括以下制备步骤:
(S1)纺丝:将辐射处理后的聚丙烯酸、聚乙二醇和无水乙醇按质量比按质量比
1:1:2~3混合均匀,进行静电纺丝制得纤维,将纤维在20~30℃的空气环境中静置20~30min,再在40~50℃,30~40kHz的超声波振动下用纯水浸洗3~5min,制得多孔锦纶;
(S2)预改性:将氯化亚砜和四氢呋喃按质量比60~80:1混合均匀,配制成氯化亚砜溶液,将多孔锦纶置于在多孔锦纶质量4~6倍的氯化亚砜溶液中,在40~50℃,300~500r/min搅拌反应50~60min,再升温至60~70℃继续搅拌反应2~3h,离心分离并用无水乙醇洗涤3~5次,在20~30℃,50~100Pa干燥3~4h,制得酰氯化多孔锦纶;将酰氯化多孔锦纶浸没在氨基聚硅碳烷混合液中,在0~5℃,25~35kHz超声反应50~60min,取出并用无水乙醇洗涤3~5次,在20~30℃,50~100Pa干燥3~4h,制得预改性多孔锦纶;
(S3)改性:将预改性多孔锦纶浸没在抗菌处理液中,在64~68℃,25~35kHz超声反应4~6h,取出并用无水乙醇洗涤3~5次,再浸没在质量分数8~10%的次氯酸钠水溶液中,在10~20℃,25~35kHz超声30~40min,取出并用无水乙醇洗涤3~5次,在20~30℃,50~100Pa干燥3~4h,制得改性多孔锦纶;
(S4)织造:将多孔锦纶和改性多孔锦纶按质量比1:1.1~1.3通过纤维编织机加捻至80~100D后,织编成240~300g/m2克重面料,制得抗菌透气面料。
作为优化,步骤(S1)所述辐射处理的方法为:将聚丙烯酸压制成1~2mm薄片,在氮气氛围下用电子束加速器辐射到100~120KGy的辐射剂量。
作为优化,步骤(S1)所述静电纺丝的工艺参数为:电压15~20kV,流体供给速度20~25μL/min,环境湿度10~20%,接收距离15cm,喷丝头内孔径0.5mm,温度30~40℃。
作为优化,步骤(S2)所述氨基聚硅碳烷混合液是将氨基聚硅碳烷、二氯甲烷、三乙胺按质量比1:10~12:0.3~0.4在0~5℃混合均匀配制而成。
作为优化,所述氨基聚硅碳烷的制备方法为:将烯丙基胺和四甲基二硅氧烷按摩尔比1:1加入到烯丙基胺质量60~80倍的正己烷中,再加入烯丙基胺质量0.02~0.03倍的氯铂酸,在70~80℃,500~800r/min搅拌回流2~3h,再加入烯丙基胺质量10~12倍的烯丙基二甲基硅烷,继续搅拌回流6~8h,在20~30℃,1~2kPa静置3~4h,制备而成。
作为优化,步骤(S3)所述抗菌处理液是将抗菌剂、正己烷、氯铂酸按质量比1:6~8:0.02~0.03混合均匀配制而成。
作为优化,所述抗菌剂的制备方法为:将4-烯丙氧基苯甲醛、4A型分子筛、无水乙醇按质量比1:1:30~40混合均匀,在68~72℃,200~300r/min搅拌条件下,在20~25min内匀速添加4-烯丙氧基苯甲醛摩尔量1.1~1.3倍的N-氨乙基哌嗪,并继续搅拌回流16~20h,过滤除分子筛,在30~40℃,50~100Pa干燥4~6h,制备而成。
与现有技术相比,本发明所达到的有益效果是:
本发明在制备抗菌透气面料时,先将辐射处理后的聚丙烯酸进行静电纺丝制得多孔锦纶;用氯化亚砜对多孔锦纶处理制得酰氯化多孔锦纶;将氨基聚硅碳烷和酰氯化多孔锦纶反应制得预改性多孔锦纶;将预改性多孔锦纶经过抗菌剂处理后,再用次氯酸钠处理,制得改性多孔锦纶;将多孔锦纶和改性多孔锦纶混合加捻后,织编成抗菌透气面料。
首先,辐射处理可使聚丙烯酸中产生大量的自由基,在纺丝时相互交联形成三维网络结构,提高面料的力学性能,在静电纺丝时加入聚乙二醇作为致孔剂,形成多孔结构,同时聚丙烯酸具有良好的吸湿性,提高面料的吸湿排液与排湿透气的性能,从而减少细菌与病毒的滋生,提高穿着者肌肤的舒适感;将烯丙基胺和四甲基二硅氧烷反应后再和烯丙基二甲基硅烷反应制得氨基聚硅碳烷,用氨基聚硅碳烷进行预改性,氨基聚硅碳烷在多孔锦纶形成聚硅碳烷长链,在高温时可以生成硅碳层覆盖在纤维表面,隔绝热量和氧气,从而提高了阻燃性能,并且氨基聚硅碳烷末端含有硅氢键,可通过硅氢加成进行固定抗菌剂,使抗菌剂不易流失,提高了面料抗菌性能,提高了面料抗菌能力的持久性与稳定性。
其次,将4-烯丙氧基苯甲醛和N-氨乙基哌嗪反应制得抗菌剂,将预改性多孔锦纶经过抗菌剂处理后,再用次氯酸钠处理,抗菌剂为席夫碱哌嗪结构,具有良好的接触杀菌效果,用次氯酸钠处理后,将抗菌剂上的氮氢键转化为氮氯键可水解缓释出氯离子进行杀菌,从而提高了面料的抗菌性能。
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抗菌透气面料的各指标测试方法如下:
阻燃性性:将各实施例所得的抗菌透气面料与对比例材料取相同大小,按照GB/T5454标准测试极限氧指数。
抗菌性:将各实施例所得的抗菌透气面料与对比例材料取相同大小形状,按奎因试验法进行测试对大肠杆菌的抑菌率。
实施例1
一种抗菌透气面料的制备工艺,所述抗菌透气面料的制备工艺主要包括以下制备步骤:
(S1)纺丝:将聚丙烯酸压制成1mm薄片,在氮气氛围下用电子束加速器辐射到100KGy的辐射剂量,得到辐射处理后的聚丙烯酸;将辐射处理后的聚丙烯酸、聚乙二醇和无水乙醇按质量比按质量比1:1:2混合均匀,进行静电纺丝,电压15kV,流体供给速度20μL/min,环境湿度10%,接收距离15cm,喷丝头内孔径0.5mm,温度30℃,制得纤维,将纤维在20℃的空气环境中静置30min,再在40℃,30kHz的超声波振动下用纯水浸洗5min,制得多孔锦纶;
(S2)预改性:将氯化亚砜和四氢呋喃按质量比60:1混合均匀,配制成氯化亚砜溶液,将多孔锦纶置于在多孔锦纶质量4倍的氯化亚砜溶液中,在40℃,300r/min搅拌反应60min,再升温至60℃继续搅拌反应3h,离心分离并用无水乙醇洗涤3次,在20℃,50Pa干燥4h,制得酰氯化多孔锦纶;将烯丙基胺和四甲基二硅氧烷按摩尔比1:1加入到烯丙基胺质量60倍的正己烷中,再加入烯丙基胺质量0.02倍的氯铂酸,在70℃,500r/min搅拌回流3h,再加入烯丙基胺质量10倍的烯丙基二甲基硅烷,继续搅拌回流8h,在20℃,1kPa静置4h,制得氨基聚硅碳烷;将氨基聚硅碳烷、二氯甲烷、三乙胺按质量比1:10:0.3在0℃混合均匀配制成氨基聚硅碳烷混合液,将酰氯化多孔锦纶浸没在氨基聚硅碳烷混合液中,在0℃,25kHz超声反应60min,取出并用无水乙醇洗涤3次,在20℃,50Pa干燥4h,制得预改性多孔锦纶;
(S3)改性:将4-烯丙氧基苯甲醛、4A型分子筛、无水乙醇按质量比1:1:30混合均匀,在68℃,200r/min搅拌条件下,在20min内匀速添加4-烯丙氧基苯甲醛摩尔量1.1倍的N-氨乙基哌嗪,并继续搅拌回流20h,过滤除分子筛,在30℃,50Pa干燥6h,制得抗菌剂;将抗菌剂、正己烷、氯铂酸按质量比1:6:0.02混合均匀配制成抗菌处理液,将预改性多孔锦纶浸没在抗菌处理液中,在64℃,25kHz超声反应6h,取出并用无水乙醇洗涤3次,再浸没在质量分数8%的次氯酸钠水溶液中,在10℃,25kHz超声40min,取出并用无水乙醇洗涤3次,在20℃,50Pa干燥4h,制得改性多孔锦纶;
(S4)织造:将多孔锦纶和改性多孔锦纶按质量比1:1.1通过纤维编织机加捻至90D后,织编成260g/m2克重面料,制得抗菌透气面料。
实施例2
一种抗菌透气面料的制备工艺,所述抗菌透气面料的制备工艺主要包括以下制备步骤:
(S1)纺丝:将聚丙烯酸压制成1.5mm薄片,在氮气氛围下用电子束加速器辐射到110KGy的辐射剂量,得到辐射处理后的聚丙烯酸;将辐射处理后的聚丙烯酸、聚乙二醇和无水乙醇按质量比按质量比1:1:2.5混合均匀,进行静电纺丝,电压18kV,流体供给速度22μL/min,环境湿度15%,接收距离15cm,喷丝头内孔径0.5mm,温度35℃,制得纤维,将纤维在25℃的空气环境中静置25min,再在45℃,35kHz的超声波振动下用纯水浸洗4min,制得多孔锦纶;
(S2)预改性:将氯化亚砜和四氢呋喃按质量比70:1混合均匀,配制成氯化亚砜溶液,将多孔锦纶置于在多孔锦纶质量5倍的氯化亚砜溶液中,在45℃,400r/min搅拌反应55min,再升温至65℃继续搅拌反应2.5h,离心分离并用无水乙醇洗涤4次,在25℃,70Pa干燥3.5h,制得酰氯化多孔锦纶;将烯丙基胺和四甲基二硅氧烷按摩尔比1:1加入到烯丙基胺质量70倍的正己烷中,再加入烯丙基胺质量0.025倍的氯铂酸,在75℃,600r/min搅拌回流2.5h,再加入烯丙基胺质量11倍的烯丙基二甲基硅烷,继续搅拌回流7h,在25℃,1.5kPa静置3.5h,制得氨基聚硅碳烷;将氨基聚硅碳烷、二氯甲烷、三乙胺按质量比1:11:0.35在2℃混合均匀配制成氨基聚硅碳烷混合液,将酰氯化多孔锦纶浸没在氨基聚硅碳烷混合液中,在2℃,30kHz超声反应55min,取出并用无水乙醇洗涤4次,在25℃,70Pa干燥3.5h,制得预改性多孔锦纶;
(S3)改性:将4-烯丙氧基苯甲醛、4A型分子筛、无水乙醇按质量比1:1:35混合均匀,在70℃,250r/min搅拌条件下,在22min内匀速添加4-烯丙氧基苯甲醛摩尔量1.2倍的N-氨乙基哌嗪,并继续搅拌回流18h,过滤除分子筛,在35℃,70Pa干燥5h,制得抗菌剂;将抗菌剂、正己烷、氯铂酸按质量比1:7:0.025混合均匀配制成抗菌处理液,将预改性多孔锦纶浸没在抗菌处理液中,在66℃,30kHz超声反应5h,取出并用无水乙醇洗涤4次,再浸没在质量分数9%的次氯酸钠水溶液中,在15℃,30kHz超声35min,取出并用无水乙醇洗涤4次,在25℃,70Pa干燥3.5h,制得改性多孔锦纶;
(S4)织造:将多孔锦纶和改性多孔锦纶按质量比1:1.2通过纤维编织机加捻至90D后,织编成260g/m2克重面料,制得抗菌透气面料。
实施例3
一种抗菌透气面料的制备工艺,所述抗菌透气面料的制备工艺主要包括以下制备步骤:
(S1)纺丝:将聚丙烯酸压制成2mm薄片,在氮气氛围下用电子束加速器辐射到120KGy的辐射剂量,得到辐射处理后的聚丙烯酸;将辐射处理后的聚丙烯酸、聚乙二醇和无水乙醇按质量比按质量比1:1:3混合均匀,进行静电纺丝,电压20kV,流体供给速度25μL/min,环境湿度20%,接收距离15cm,喷丝头内孔径0.5mm,温度40℃,制得纤维,将纤维在30℃的空气环境中静置20min,再在50℃,40kHz的超声波振动下用纯水浸洗3min,制得多孔锦纶;
(S2)预改性:将氯化亚砜和四氢呋喃按质量比80:1混合均匀,配制成氯化亚砜溶液,将多孔锦纶置于在多孔锦纶质量6倍的氯化亚砜溶液中,在50℃,500r/min搅拌反应50min,再升温至70℃继续搅拌反应2h,离心分离并用无水乙醇洗涤5次,在30℃,100Pa干燥3h,制得酰氯化多孔锦纶;将烯丙基胺和四甲基二硅氧烷按摩尔比1:1加入到烯丙基胺质量80倍的正己烷中,再加入烯丙基胺质量0.03倍的氯铂酸,在80℃,800r/min搅拌回流2h,再加入烯丙基胺质量12倍的烯丙基二甲基硅烷,继续搅拌回流8h,在30℃,2kPa静置3h,制得氨基聚硅碳烷;将氨基聚硅碳烷、二氯甲烷、三乙胺按质量比1:12:0.4在5℃混合均匀配制成氨基聚硅碳烷混合液,将酰氯化多孔锦纶浸没在氨基聚硅碳烷混合液中,在5℃,35kHz超声反应50min,取出并用无水乙醇洗涤5次,在30℃,100Pa干燥3h,
制得预改性多孔锦纶;
(S3)改性:将4-烯丙氧基苯甲醛、4A型分子筛、无水乙醇按质量比1:1:40混合均匀,在72℃,300r/min搅拌条件下,在20min内匀速添加4-烯丙氧基苯甲醛摩尔量1.3倍的N-氨乙基哌嗪,并继续搅拌回流20h,过滤除分子筛,在40℃,100Pa干燥4h,制得抗菌剂;将抗菌剂、正己烷、氯铂酸按质量比1:8:0.03混合均匀配制成抗菌处理液,将预改性多孔锦纶浸没在抗菌处理液中,在68℃,35kHz超声反应4h,取出并用无水乙醇洗涤5次,再浸没在质量分数10%的次氯酸钠水溶液中,在20℃,35kHz超声40min,取出并用无水乙醇洗涤3次,在30℃,100Pa干燥3h,制得改性多孔锦纶;
(S4)织造:将多孔锦纶和改性多孔锦纶按质量比1:1.1~1.3通过纤维编织机加捻至90D后,织编成260g/m2克重面料,制得抗菌透气面料。
对比例1
一种抗菌透气面料的制备工艺,所述抗菌透气面料的制备工艺主要包括以下制备步骤:
(S1)纺丝:将聚丙烯酸压制成1.5mm薄片,在氮气氛围下用电子束加速器辐射到110KGy的辐射剂量,得到辐射处理后的聚丙烯酸;将辐射处理后的聚丙烯酸、聚乙二醇和无水乙醇按质量比按质量比1:1:2.5混合均匀,进行静电纺丝,电压18kV,流体供给速度22μL/min,环境湿度15%,接收距离15cm,喷丝头内孔径0.5mm,温度35℃,制得纤维,将纤维在25℃的空气环境中静置25min,再在45℃,35kHz的超声波振动下用纯水浸洗4min,制得多孔锦纶;
(S2)改性:将4-烯丙氧基苯甲醛、4A型分子筛、无水乙醇按质量比1:1:35混合均匀,在70℃,250r/min搅拌条件下,在22min内匀速添加4-烯丙氧基苯甲醛摩尔量1.2倍的N-氨乙基哌嗪,并继续搅拌回流18h,过滤除分子筛,在35℃,70Pa干燥5h,制得抗菌剂;将抗菌剂、正己烷、氯铂酸按质量比1:7:0.025混合均匀配制成抗菌处理液,将多孔锦纶浸没在抗菌处理液中,在66℃,30kHz超声反应5h,取出并用无水乙醇洗涤4次,再浸没在质量分数9%的次氯酸钠水溶液中,在15℃,30kHz超声35min,取出并用无水乙醇洗涤4次,在25℃,70Pa干燥3.5h,制得改性多孔锦纶;
(S3)织造:将多孔锦纶和改性多孔锦纶按质量比1:1.2通过纤维编织机加捻至90D后,织编成260g/m2克重面料,制得抗菌透气面料。
对比例2
一种抗菌透气面料的制备工艺,所述抗菌透气面料的制备工艺主要包括以下制备步骤:
(S1)纺丝:将聚丙烯酸压制成1.5mm薄片,在氮气氛围下用电子束加速器辐射到110KGy的辐射剂量,得到辐射处理后的聚丙烯酸;将辐射处理后的聚丙烯酸、聚乙二醇和无水乙醇按质量比按质量比1:1:2.5混合均匀,进行静电纺丝,电压18kV,流体供给速度22μL/min,环境湿度15%,接收距离15cm,喷丝头内孔径0.5mm,温度35℃,制得纤维,将纤维在25℃的空气环境中静置25min,再在45℃,35kHz的超声波振动下用纯水浸洗4min,制得多孔锦纶;
(S2)预改性:将氯化亚砜和四氢呋喃按质量比70:1混合均匀,配制成氯化亚砜溶液,将多孔锦纶置于在多孔锦纶质量5倍的氯化亚砜溶液中,在45℃,400r/min搅拌反应55min,再升温至65℃继续搅拌反应2.5h,离心分离并用无水乙醇洗涤4次,在25℃,70Pa干燥3.5h,制得酰氯化多孔锦纶;将烯丙基胺和四甲基二硅氧烷按摩尔比1:1加入到烯丙基胺质量70倍的正己烷中,再加入烯丙基胺质量0.025倍的氯铂酸,在75℃,600r/min搅拌回流2.5h,再加入烯丙基胺质量11倍的烯丙基二甲基硅烷,继续搅拌回流7h,在25℃,1.5kPa静置3.5h,制得氨基聚硅碳烷;将氨基聚硅碳烷、二氯甲烷、三乙胺按质量比1:11:0.35在2℃混合均匀配制成氨基聚硅碳烷混合液,将酰氯化多孔锦纶浸没在氨基聚硅碳烷混合液中,在2℃,30kHz超声反应55min,取出并用无水乙醇洗涤4次,在25℃,70Pa干燥3.5h,制得预改性多孔锦纶;
(S3)织造:将多孔锦纶和预改性多孔锦纶按质量比1:1.2通过纤维编织机加捻至90D后,织编成260g/m2克重面料,制得抗菌透气面料。
对比例3
一种抗菌透气面料的制备工艺,所述抗菌透气面料的制备工艺主要包括以下制备步骤:
(S1)纺丝:将聚丙烯酸压制成1.5mm薄片,在氮气氛围下用电子束加速器辐射到110KGy的辐射剂量,得到辐射处理后的聚丙烯酸;将辐射处理后的聚丙烯酸、聚乙二醇和无水乙醇按质量比按质量比1:1:2.5混合均匀,进行静电纺丝,电压18kV,流体供给速度22μL/min,环境湿度15%,接收距离15cm,喷丝头内孔径0.5mm,温度35℃,制得纤维,将纤维在25℃的空气环境中静置25min,再在45℃,35kHz的超声波振动下用纯水浸洗4min,制得多孔锦纶;
(S2)织造:将多孔锦纶按质量比1:1.2通过纤维编织机加捻至90D后,织编成260g/m2克重面料,制得抗菌透气面料。
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3的抗菌透气面料的阻燃性和抗菌性的分析结果。
表1
从表1中的实验数据比较可发现,本发明制得的抗菌透气面料具有良好的阻燃性和抗菌性。
从实施例1、2、3和对比例1实验数据比较可发现,实施例1、2、3对比对比例1的极限氧指数和抑菌率高,说明了用氨基聚硅碳烷进行预改性,氨基聚硅碳烷在多孔锦纶形成聚硅碳烷长链,在高温时可以生成硅碳层覆盖在纤维表面,隔绝热量和氧气,从而提高了阻燃性能,并且氨基聚硅碳烷末端含有硅氢键,可通过硅氢加成进行固定抗菌剂,使抗菌剂不易流失,提高了抗菌性能;实施例1、2、3和对比例1实验数据比较可发现,实施例1、2、3对比对比例1的抑菌率高,说明了将预改性多孔锦纶经过抗菌剂处理后,再用次氯酸钠处理,抗菌剂为席夫碱哌嗪结构,具有良好的接触杀菌效果,用次氯酸钠处理后,将抗菌剂上的氮氢键转化为氮氯键可水解缓释出氯离子进行杀菌,从而提高了抗菌性能。
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 (8)
1.一种抗菌透气面料的制备工艺,其特征在于,主要包括以下制备步骤:
(S1)纺丝:将辐射处理后的聚丙烯酸进行静电纺丝制得多孔锦纶;
(S2)预改性:用氯化亚砜对多孔锦纶处理制得酰氯化多孔锦纶;将烯丙基胺和四甲基二硅氧烷反应后再和烯丙基二甲基硅烷反应制得氨基聚硅碳烷;将氨基聚硅碳烷和酰氯化多孔锦纶反应制得预改性多孔锦纶;
(S3)改性:将4-烯丙氧基苯甲醛和N-氨乙基哌嗪反应制得抗菌剂;将预改性多孔锦纶经过抗菌剂处理后,再用次氯酸钠处理,制得改性多孔锦纶;
(S4)织造:将多孔锦纶和改性多孔锦纶加捻后,织编成抗菌透气面料。
2.根据权利要求1所述的一种抗菌透气面料的制备工艺,其特征在于,所述抗菌透气面料的制备工艺主要包括以下制备步骤:
(S1)纺丝:将辐射处理后的聚丙烯酸、聚乙二醇和无水乙醇按质量比按质量比1:1:2~3混合均匀,进行静电纺丝制得纤维,将纤维在20~30℃的空气环境中静置20~30min,再在40~50℃,30~40kHz的超声波振动下用纯水浸洗3~5min,制得多孔锦纶;
(S2)预改性:将氯化亚砜和四氢呋喃按质量比60~80:1混合均匀,配制成氯化亚砜溶液,将多孔锦纶置于在多孔锦纶质量4~6倍的氯化亚砜溶液中,在40~50℃,300~500r/min搅拌反应50~60min,再升温至60~70℃继续搅拌反应2~3h,离心分离并用无水乙醇洗涤3~5次,在20~30℃,50~100Pa干燥3~4h,制得酰氯化多孔锦纶;将酰氯化多孔锦纶浸没在氨基聚硅碳烷混合液中,在0~5℃,25~35kHz超声反应50~60min,取出并用无水乙醇洗涤3~5次,在20~30℃,50~100Pa干燥3~4h,制得预改性多孔锦纶;
(S3)改性:将预改性多孔锦纶浸没在抗菌处理液中,在64~68℃,25~35kHz超声反应4~6h,取出并用无水乙醇洗涤3~5次,再浸没在质量分数8~10%的次氯酸钠水溶液中,在10~20℃,25~35kHz超声30~40min,取出并用无水乙醇洗涤3~5次,在20~30℃,50~100Pa干燥3~4h,制得改性多孔锦纶;
(S4)织造:将多孔锦纶和改性多孔锦纶按质量比1:1.1~1.3通过纤维编织机加捻至80~100D后,织编成240~300g/m2克重面料,制得抗菌透气面料。
3.根据权利要求2所述的一种抗菌透气面料的制备工艺,其特征在于,步骤(S1)所述辐射处理的方法为:将聚丙烯酸压制成1~2mm薄片,在氮气氛围下用电子束加速器辐射到100~120KGy的辐射剂量。
4.根据权利要求2所述的一种抗菌透气面料的制备工艺,其特征在于,步骤(S1)所述静电纺丝的工艺参数为:电压15~20kV,流体供给速度20~25μL/min,环境湿度10~20%,接收距离15cm,喷丝头内孔径0.5mm,温度30~40℃。
5.根据权利要求2所述的一种抗菌透气面料的制备工艺,其特征在于,步骤(S2)所述氨基聚硅碳烷混合液是将氨基聚硅碳烷、二氯甲烷、三乙胺按质量比1:10~12:0.3~0.4在0~5℃混合均匀配制而成。
6.根据权利要求5所述的一种抗菌透气面料的制备工艺,其特征在于,所述氨基聚硅碳烷的制备方法为:将烯丙基胺和四甲基二硅氧烷按摩尔比1:1加入到烯丙基胺质量60~80倍的正己烷中,再加入烯丙基胺质量0.02~0.03倍的氯铂酸,在70~80℃,500~800r/min搅拌回流2~3h,再加入烯丙基胺质量10~12倍的烯丙基二甲基硅烷,继续搅拌回流6~8h,在20~30℃,1~2kPa静置3~4h,制备而成。
7.根据权利要求2所述的一种抗菌透气面料的制备工艺,其特征在于,步骤(S3)所述抗菌处理液是将抗菌剂、正己烷、氯铂酸按质量比1:6~8:0.02~0.03混合均匀配制而成。
8.根据权利要求7所述的一种抗菌透气面料的制备工艺,其特征在于,所述抗菌剂的制备方法为:将4-烯丙氧基苯甲醛、4A型分子筛、无水乙醇按质量比1:1:30~40混合均匀,在68~72℃,200~300r/min搅拌条件下,在20~25min内匀速添加4-烯丙氧基苯甲醛摩尔量1.1~1.3倍的N-氨乙基哌嗪,并继续搅拌回流16~20h,过滤除分子筛,在30~40℃,50~100Pa干燥4~6h,制备而成。
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