CN116691085A - 一种多层复合医用面料 - Google Patents

一种多层复合医用面料 Download PDF

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Publication number
CN116691085A
CN116691085A CN202310496399.6A CN202310496399A CN116691085A CN 116691085 A CN116691085 A CN 116691085A CN 202310496399 A CN202310496399 A CN 202310496399A CN 116691085 A CN116691085 A CN 116691085A
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China
Prior art keywords
mass
layer
hours
fabric
washing
Prior art date
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Pending
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CN202310496399.6A
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English (en)
Inventor
王伟历
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Individual
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Individual
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Priority to CN202310496399.6A priority Critical patent/CN116691085A/zh
Publication of CN116691085A publication Critical patent/CN116691085A/zh
Pending legal-status Critical Current

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    • 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
    • B32B5/022—Non-woven fabric
    • 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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    • B32B37/06—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the heating method
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    • B32B37/10—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the pressing technique, e.g. using action of vacuum or fluid pressure
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    • 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
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    • D01D5/003—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
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    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
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    • D01D5/0092—Electro-spinning characterised by the electro-spinning apparatus characterised by the electrical field, e.g. combined with a magnetic fields, using biased or alternating fields
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    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
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Abstract

本发明公开了一种多层复合医用面料，涉及纺织技术领域。本发明在制备的多层复合医用面料，由内到外包括亲肤层、交联层和保护层；亲肤层为改性棉纤维面料；交联层为交联聚酰亚胺面料；保护层是经过等离子体处理的聚丙烯无纺布，经过等离子体处理的聚丙烯无纺布，表面亲润性提高，能够与交联层的连接性；经过改性的棉纤维，使得亲肤层具有抗菌性；内部为交联结构的聚酰亚胺进行静电纺丝制成的交联层，增强多层复合医用面料的断裂韧性。

Description

一种多层复合医用面料
技术领域
本发明涉及面料技术领域，具体为一种多层复合医用面料。
背景技术
随着时代的发展，人们对面料的要求越来越高，开发出能够满足消费者需求的面料，在面料生产领域占据着越来越重要的作用。现有单层结构纺织面料已经无法满足人们日常需求，尤其在防水、透气性能方面，单层结构面料效果甚微，尤其是医用面料。
棉面料具有天然纤维的特点，手感柔软，穿着舒适，但抗氧化性差、不具备抗菌性的缺点。因此本申请以棉纤维面料为基料进行多层复合医用面料的制备，具有优异的抗菌性和断裂韧性。
发明内容
本发明的目的在于提供一种多层复合医用面料及其制备方法，以解决上述背景技术中提出的问题。
一种多层复合医用面料，由内到外包括亲肤层、交联层和保护层；所述亲肤层为改性棉纤维面料；所述交联层为交联聚酰亚胺面料；所述保护层是经过等离子体处理的聚丙烯无纺布。
优选的，所述改性棉纤维是在醛基棉纤维上接枝改性壳聚糖，再与水合肼反应制得。
优选的，所述交联聚酰亚胺面料是由2,2’-双(3,4-二羧苯基)六氟丙烷四酸二酐与3,5-二(2-三氟甲基-4-氨基苯氧基)苯酚共混制得静电纺丝液，进行静电纺丝制成聚酰亚胺纤维，编织成面料制得。
优选的，所述多层复合医用面料的制备方法为：亲肤层制备，交联层制备，保护层制备，多层复合医用面料制备。
优选的，所述一种多层复合医用面料的制备方法，包括以下具体步骤：
（1）将醛基棉纤维分散在醛基棉纤维质量5~10倍的去离子水中，加入醛基棉纤维质量0.4~0.6倍的改性壳聚糖，在50~100rpm下搅拌，并滴加醛基棉纤维质量2~3倍的饱和碳酸钠溶液，滴加完成后继续搅拌，反应8~12h，捞出并用去离子水洗涤3~5次，转移至醛基棉纤维质量5~10倍的无水乙醇中，加入醛基棉纤维质量倍的0.25~0.3倍的水合肼，继续搅拌反应3~5h，捞出并用去离子水洗涤5~8次，置于烘箱中在40~60℃下干燥6~8h，制得改性棉纤维；将改性棉纤维进经倍捻、纺线、机织后，制得克重为80~120g/m2的亲肤层；
（2）将3,5-二(2-三氟甲基-4-氨基苯氧基)苯酚与二甲基甲酰胺按质量比1:5~1:8混合，充分溶解后每隔10~12min加入2,2’-双(3,4-二羧苯基)六氟丙烷四酸二酐，控制加料时间为1.5~2h，2,2’-双(3,4-二羧苯基)六氟丙烷四酸二酐与3,5-二(2-三氟甲基-4-氨基苯氧基)苯酚的质量比为1:1~1.12:1，加料完成后在50~100rpm下搅拌均化4~6h，制得静电纺丝液，进行静电纺丝，制得交联聚酰亚胺纤维，将交联聚酰亚胺纤维进经倍捻、纺线、机织后，制得克重为40~60g/m2的交联层；
（3）将克重为30~60g/m2聚丙烯无纺布浸泡在无水乙醇中，24~28h后捞出晾干，再浸泡在丙酮中，在40~60kHz下进行超声洗涤20~40min，捞出后用去离子水洗涤3~5次，置于40~60℃烘箱中干燥至恒重，制得预处理聚丙烯无纺布；将预处理聚丙烯无纺布悬挂于等离子体仪的处理腔中，抽真空至5~10Pa后，通氧气至真空度为15~30Pa，在80~100W下进行等离子体处理，时间为4~6min，制得保护层；
（4）依次放置亲肤层、交联层和保护层，用热压机进行压合，压合温度为150～180℃，剪裁，制得多层复合医用面料。
优选的，上述步骤（1）中：醛基棉纤维的制备方法为：室温下将棉纤维浸泡在棉纤维质量20~30倍质量分数为18~20%的氢氧化钠溶液中，反应2~4h后捞出，用去离子水洗涤5~8次，再浸泡在棉纤维质量40~50倍质量分数为5~10%的高碘酸钾溶液中，避光反应4~6h后捞出，转移至棉纤维质量10~20倍的甘油中，反应1~2h后捞出，用去离子水洗涤5~8次，烘干至恒重，制得醛基棉纤维。
优选的，上述步骤（1）中：改性壳聚糖的制备方法为：在氮气氛围下，将壳聚糖与N-甲基吡咯烷酮按质量比1:20~1:30混合，再以1~2ml/min的速率滴加壳聚糖质量2~3倍质量分数为2~5%的氯丁酰氯的N-甲基吡咯烷酮溶液，反应3~5h后，浓缩至用乙醚洗涤无沉淀生成，再用甲醇洗涤3~5次，加入壳聚糖质量1.5~1.8倍的2,4,6-三(4-羟基苯基)吡啶，在50~100rpm下搅拌反应72~78h，浓缩得沉淀，再依次用乙醚、甲醇洗涤3~5次，干燥至恒重，制得改性壳聚糖。
优选的，所述2,4,6-三(4-羟基苯基)吡啶的制备方法为：将4-羟基苯基甲醛、4-羟基苯乙酮、乙酸铵和冰乙酸按质量比1:2:3:4.5~1:2.2:3.5:5混合加热至80~90℃，回流反应3~5h，冷却至室温后，加入4-羟基苯基甲醛8~10倍质量分数为50~60%的乙酸溶液进行沉析，并以100~200rpm搅拌10~15min后，过滤并用无水乙醇重结晶，最后在真空65～70℃下干燥12h，制得2,4,6-三(4-羟基苯基)吡啶。
优选的，上述步骤（2）中：3,5-二(2-三氟甲基-4-氨基苯氧基)苯酚的制备方法为：将间苯三酚、3-三氟甲基-4-氯硝基苯和污水碳酸钾按质量比3:11:4~3:11.3~4.2混合，并加入间苯三酚质量3.2~3.4倍的甲苯和间苯三酚质量16~18倍的N,N-二甲基甲酰胺，升温至115~120℃并在100~200rpm下搅拌反应5~5.5h，升温至150~155℃继续反应8~9h，冷却至室温后用去离子水洗涤3~5次，加入间苯三酚质量3.1~3.3倍的铁粉，再加入间苯三酚质量16~18倍的混合溶剂，混合溶剂中丙酮、乙醇和去离子水质量比为1:1:1，在氮气氛围下，升温至80~100℃并在50~100rpm下搅拌回流5~6h，加入间苯三酚质量0.08~0.1倍的氢氧化钠，继续搅拌5~8min后趁热过滤，再进行减压蒸馏，并用水和无水乙醇进行重结晶，制得3,5-二(2-三氟甲基-4-氨基苯氧基)苯酚。
优选的，静电纺丝时，注射器到铝箔的距离为15～20cm，纺丝液的推注速度为0.24～0.5mL/h，相对湿度为5～10%，温度为40～60℃，两极电压为15～35kV。
与现有技术相比，本发明所达到的有益效果是：
本发明在制备的多层复合医用面料，由内到外包括亲肤层、交联层和保护层；亲肤层为改性棉纤维面料；交联层为交联聚酰亚胺面料；保护层是经过等离子体处理的聚丙烯无纺布，经过等离子体处理的聚丙烯无纺布，表面亲润性提高，能够与交联层的连接性；
改性棉纤维是在醛基棉纤维上接枝改性壳聚糖，再与水合肼反应制得；改性壳聚糖是壳聚糖与2,4,6-三(4-羟基苯基)吡啶反应制得，引入吡啶的同时引入大量羟基；将棉纤维进行碱处理，再进行氧化，将棉纤维上的羟基氧化为醛基，改性壳聚糖上的羟基与醛基反应形成缩醛，再与水合肼反应，形成席夫碱，将改性壳聚糖聚合在棉纤维表面，并使得亲肤层具有抗菌性；
交联聚酰亚胺面料是由2,2’-双(3,4-二羧苯基)六氟丙烷四酸二酐与3,5-二(2-三氟甲基-4-氨基苯氧基)苯酚共混制得静电纺丝液进行静电纺丝制成聚酰亚胺纤维，编织成面料制得；2,2’-双(3,4-二羧苯基)六氟丙烷四酸二酐与3,5-二(2-三氟甲基-4-氨基苯氧基)苯酚共混形成交联聚酰亚胺，剩余的苯酚与聚酰亚胺侧链中的羧酸发生反应形成酯基，还能够与羧基反应，形成内部为交联结构的聚酰亚胺，增强交联层的强度和断裂韧性，同时2,2’-双(3,4-二羧苯基)六氟丙烷四酸二酐与3,5-二(2-三氟甲基-4-氨基苯氧基)苯酚制得的聚酰亚胺带有微孔结构，与亲肤层和保护层进行压合时，可在两层之间吸附，使得层间连接紧密，增强面料的断裂韧性。
具体实施方式
下面将结合本发明的实施例，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，将实施例和对比例中制备的多层复合医用面料的各指标测试方法如下：
抗菌性：将实施例与对比例制得的多层复合医用面料参照GB/T20944.3进行抗菌性测试。
断裂韧性：将实施例与对比例制得的多层复合医用面料参照B/T3923.1进行拉伸强度测试。
实施例1
一种多层复合医用面料的制备方法，所述多层复合医用面料的制备方法为：
（1）室温下将棉纤维浸泡在棉纤维质量20倍质量分数为18%的氢氧化钠溶液中，反应2h后捞出，用去离子水洗涤5次，再浸泡在棉纤维质量40倍质量分数为5%的高碘酸钾溶液中，避光反应4h后捞出，转移至棉纤维质量10倍的甘油中，反应1h后捞出，用去离子水洗涤5次，烘干至恒重，制得醛基棉纤维；将4-羟基苯基甲醛、4-羟基苯乙酮、乙酸铵和冰乙酸按质量比1:2:3:4.5混合加热至80℃，回流反应3h，冷却至室温后，加入4-羟基苯基甲醛8倍质量分数为50%的乙酸溶液进行沉析，并以100rpm搅拌10min后，过滤并用无水乙醇重结晶，最后在真空65℃下干燥12h，制得2,4,6-三(4-羟基苯基)吡啶；在氮气氛围下，将壳聚糖与N-甲基吡咯烷酮按质量比1:20混合，再以1ml/min的速率滴加壳聚糖质量2倍质量分数为2%的氯丁酰氯的N-甲基吡咯烷酮溶液，反应3h后，浓缩至用乙醚洗涤无沉淀生成，再用甲醇洗涤3次，加入壳聚糖质量1.5倍的2,4,6-三(4-羟基苯基)吡啶，在50rpm下搅拌反应72h，浓缩得沉淀，再依次用乙醚、甲醇洗涤3次，干燥至恒重，制得改性壳聚糖；
（2）将醛基棉纤维分散在醛基棉纤维质量5倍的去离子水中，加入醛基棉纤维质量0.4倍的改性壳聚糖，在50rpm下搅拌，并滴加醛基棉纤维质量2倍的饱和碳酸钠溶液，滴加完成后继续搅拌，反应8h，捞出并用去离子水洗涤3次，转移至醛基棉纤维质量5倍的无水乙醇中，加入醛基棉纤维质量倍的0.25倍的水合肼，继续搅拌反应3h，捞出并用去离子水洗涤5次，置于烘箱中在40℃下干燥6h，制得改性棉纤维；将改性棉纤维进经倍捻、纺线、机织后，制得克重为80g/m2的亲肤层；
（3）将间苯三酚、3-三氟甲基-4-氯硝基苯和污水碳酸钾按质量比3:11:4混合，并加入间苯三酚质量3.2倍的甲苯和间苯三酚质量16倍的N,N-二甲基甲酰胺，升温至115℃并在100rpm下搅拌反应5h，升温至150℃继续反应8h，冷却至室温后用去离子水洗涤3次，加入间苯三酚质量3.1倍的铁粉，再加入间苯三酚质量16倍的混合溶剂，混合溶剂中丙酮、乙醇和去离子水质量比为1:1:1，在氮气氛围下，升温至80℃并在50rpm下搅拌回流5h，加入间苯三酚质量0.08倍的氢氧化钠，继续搅拌5min后趁热过滤，再进行减压蒸馏，并用水和无水乙醇进行重结晶，制得3,5-二(2-三氟甲基-4-氨基苯氧基)苯酚；
（4）将3,5-二(2-三氟甲基-4-氨基苯氧基)苯酚与二甲基甲酰胺按质量比1:5混合，充分溶解后每隔10min加入2,2’-双(3,4-二羧苯基)六氟丙烷四酸二酐，控制加料时间为1.5h，2,2’-双(3,4-二羧苯基)六氟丙烷四酸二酐与3,5-二(2-三氟甲基-4-氨基苯氧基)苯酚的质量比为1:1，加料完成后在50rpm下搅拌均化4h，制得静电纺丝液，进行静电纺丝，静电纺丝时，注射器到铝箔的距离为15cm，纺丝液的推注速度为0.24mL/h，相对湿度为5%，温度为40℃，两极电压为15kV，制得交联聚酰亚胺纤维，将交联聚酰亚胺纤维进经倍捻、纺线、机织后，制得克重为40g/m2的交联层；
（5）将克重为30g/m2聚丙烯无纺布浸泡在无水乙醇中，24h后捞出晾干，再浸泡在丙酮中，在40kHz下进行超声洗涤20min，捞出后用去离子水洗涤3次，置于40℃烘箱中干燥至恒重，制得预处理聚丙烯无纺布；将预处理聚丙烯无纺布悬挂于等离子体仪的处理腔中，抽真空至5Pa后，通氧气至真空度为15Pa，在90W下进行等离子体处理，时间为4min，制得保护层；
（6）依次放置亲肤层、交联层和保护层，用热压机进行压合，压合温度为150℃，剪裁，制得多层复合医用面料。
实施例2
一种多层复合医用面料的制备方法，所述多层复合医用面料的制备方法为：
（1）室温下将棉纤维浸泡在棉纤维质量25倍质量分数为19%的氢氧化钠溶液中，反应3h后捞出，用去离子水洗涤6次，再浸泡在棉纤维质量45倍质量分数为8%的高碘酸钾溶液中，避光反应5h后捞出，转移至棉纤维质量15倍的甘油中，反应1h后捞出，用去离子水洗涤6次，烘干至恒重，制得醛基棉纤维；将4-羟基苯基甲醛、4-羟基苯乙酮、乙酸铵和冰乙酸按质量比1:2:3.2:4.8混合加热至85℃，回流反应4h，冷却至室温后，加入4-羟基苯基甲醛9倍质量分数为55%的乙酸溶液进行沉析，并以150rpm搅拌13min后，过滤并用无水乙醇重结晶，最后在真空68℃下干燥12h，制得2,4,6-三(4-羟基苯基)吡啶；在氮气氛围下，将壳聚糖与N-甲基吡咯烷酮按质量比1:25混合，再以1ml/min的速率滴加壳聚糖质量2倍质量分数为3%的氯丁酰氯的N-甲基吡咯烷酮溶液，反应4h后，浓缩至用乙醚洗涤无沉淀生成，再用甲醇洗涤4次，加入壳聚糖质量1.6倍的2,4,6-三(4-羟基苯基)吡啶，在80rpm下搅拌反应75h，浓缩得沉淀，再依次用乙醚、甲醇洗涤4次，干燥至恒重，制得改性壳聚糖；
（2）将醛基棉纤维分散在醛基棉纤维质量8倍的去离子水中，加入醛基棉纤维质量0.5倍的改性壳聚糖，在80rpm下搅拌，并滴加醛基棉纤维质量2~3倍的饱和碳酸钠溶液，滴加完成后继续搅拌，反应10h，捞出并用去离子水洗涤4次，转移至醛基棉纤维质量8倍的无水乙醇中，加入醛基棉纤维质量倍的0.28倍的水合肼，继续搅拌反应4h，捞出并用去离子水洗涤6次，置于烘箱中在50℃下干燥7h，制得改性棉纤维；将改性棉纤维进经倍捻、纺线、机织后，制得克重为100g/m2的亲肤层；
（3）将间苯三酚、3-三氟甲基-4-氯硝基苯和污水碳酸钾按质量比3:11.2:4.1混合，并加入间苯三酚质量3.3倍的甲苯和间苯三酚质量17倍的N,N-二甲基甲酰胺，升温至118℃并在150rpm下搅拌反应5h，升温至153℃继续反应8h，冷却至室温后用去离子水洗涤4次，加入间苯三酚质量3.2倍的铁粉，再加入间苯三酚质量17倍的混合溶剂，混合溶剂中丙酮、乙醇和去离子水质量比为1:1:1，在氮气氛围下，升温至90℃并在70rpm下搅拌回流5h，加入间苯三酚质量0.09倍的氢氧化钠，继续搅拌6min后趁热过滤，再进行减压蒸馏，并用水和无水乙醇进行重结晶，制得3,5-二(2-三氟甲基-4-氨基苯氧基)苯酚；
（4）将3,5-二(2-三氟甲基-4-氨基苯氧基)苯酚与二甲基甲酰胺按质量比1:6混合，充分溶解后每隔11min加入2,2’-双(3,4-二羧苯基)六氟丙烷四酸二酐，控制加料时间为1.5h，2,2’-双(3,4-二羧苯基)六氟丙烷四酸二酐与3,5-二(2-三氟甲基-4-氨基苯氧基)苯酚的质量比为1.1:1，加料完成后在70rpm下搅拌均化5h，制得静电纺丝液，进行静电纺丝，静电纺丝时，注射器到铝箔的距离为18cm，纺丝液的推注速度为0.4mL/h，相对湿度为8%，温度为50℃，两极电压为25kV，制得交联聚酰亚胺纤维，将交联聚酰亚胺纤维进经倍捻、纺线、机织后，制得克重为50g/m2的交联层；
（5）将克重为40g/m2聚丙烯无纺布浸泡在无水乙醇中，26h后捞出晾干，再浸泡在丙酮中，在50kHz下进行超声洗涤40min，捞出后用去离子水洗涤4次，置于50℃烘箱中干燥至恒重，制得预处理聚丙烯无纺布；将预处理聚丙烯无纺布悬挂于等离子体仪的处理腔中，抽真空至8Pa后，通氧气至真空度为20Pa，在90W下进行等离子体处理，时间为5min，制得保护层；
（6）依次放置亲肤层、交联层和保护层，用热压机进行压合，压合温度为165℃，剪裁，制得多层复合医用面料。
实施例3
一种多层复合医用面料的制备方法，所述多层复合医用面料的制备方法为：
（1）室温下将棉纤维浸泡在棉纤维质量30倍质量分数为20%的氢氧化钠溶液中，反应4h后捞出，用去离子水洗涤8次，再浸泡在棉纤维质量50倍质量分数为10%的高碘酸钾溶液中，避光反应6h后捞出，转移至棉纤维质量20倍的甘油中，反应2h后捞出，用去离子水洗涤8次，烘干至恒重，制得醛基棉纤维；将4-羟基苯基甲醛、4-羟基苯乙酮、乙酸铵和冰乙酸按质量比1:2.2:3.5:5混合加热至90℃，回流反应5h，冷却至室温后，加入4-羟基苯基甲醛10倍质量分数为60%的乙酸溶液进行沉析，并以200rpm搅拌10~15min后，过滤并用无水乙醇重结晶，最后在真空70℃下干燥12h，制得2,4,6-三(4-羟基苯基)吡啶；在氮气氛围下，将壳聚糖与N-甲基吡咯烷酮按质量比1:30混合，再以2ml/min的速率滴加壳聚糖质量3倍质量分数为5%的氯丁酰氯的N-甲基吡咯烷酮溶液，反应3~5h后，浓缩至用乙醚洗涤无沉淀生成，再用甲醇洗涤5次，加入壳聚糖质量1.8倍的2,4,6-三(4-羟基苯基)吡啶，在100rpm下搅拌反应78h，浓缩得沉淀，再依次用乙醚、甲醇洗涤5次，干燥至恒重，制得改性壳聚糖；
（2）将醛基棉纤维分散在醛基棉纤维质量10倍的去离子水中，加入醛基棉纤维质量0.6倍的改性壳聚糖，在100rpm下搅拌，并滴加醛基棉纤维质量3倍的饱和碳酸钠溶液，滴加完成后继续搅拌，反应12h，捞出并用去离子水洗涤5次，转移至醛基棉纤维质量10倍的无水乙醇中，加入醛基棉纤维质量倍的0.3倍的水合肼，继续搅拌反应5h，捞出并用去离子水洗涤8次，置于烘箱中在60℃下干燥8h，制得改性棉纤维；将改性棉纤维进经倍捻、纺线、机织后，制得克重为120g/m2的亲肤层；
（3）将间苯三酚、3-三氟甲基-4-氯硝基苯和污水碳酸钾按质量比3:11:4~3:11.3~4.2混合，并加入间苯三酚质量3.4倍的甲苯和间苯三酚质量16~18倍的N,N-二甲基甲酰胺，升温至120℃并在200rpm下搅拌反应5.5h，升温至155℃继续反应9h，冷却至室温后用去离子水洗涤5次，加入间苯三酚质量3.3倍的铁粉，再加入间苯三酚质量18倍的混合溶剂，混合溶剂中丙酮、乙醇和去离子水质量比为1:1:1，在氮气氛围下，升温至100℃并在100rpm下搅拌回流6h，加入间苯三酚质量0.1倍的氢氧化钠，继续搅拌8min后趁热过滤，再进行减压蒸馏，并用水和无水乙醇进行重结晶，制得3,5-二(2-三氟甲基-4-氨基苯氧基)苯酚；
（4）将3,5-二(2-三氟甲基-4-氨基苯氧基)苯酚与二甲基甲酰胺按质量比1:8混合，充分溶解后每隔12min加入2,2’-双(3,4-二羧苯基)六氟丙烷四酸二酐，控制加料时间为2h，2,2’-双(3,4-二羧苯基)六氟丙烷四酸二酐与3,5-二(2-三氟甲基-4-氨基苯氧基)苯酚的质量比为1.12:1，加料完成后在100rpm下搅拌均化6h，制得静电纺丝液，进行静电纺丝，静电纺丝时，注射器到铝箔的距离为20cm，纺丝液的推注速度为0.5mL/h，相对湿度为10%，温度为60℃，两极电压为35kV，制得交联聚酰亚胺纤维，将交联聚酰亚胺纤维进经倍捻、纺线、机织后，制得克重为60g/m2的交联层；
（5）将克重为60g/m2聚丙烯无纺布浸泡在无水乙醇中，28h后捞出晾干，再浸泡在丙酮中，在60kHz下进行超声洗涤40min，捞出后用去离子水洗涤5次，置于60℃烘箱中干燥至恒重，制得预处理聚丙烯无纺布；将预处理聚丙烯无纺布悬挂于等离子体仪的处理腔中，抽真空至10Pa后，通氧气至真空度为30Pa，在100W下进行等离子体处理，时间为6min，制得保护层；
（6）依次放置亲肤层、交联层和保护层，用热压机进行压合，压合温度为180℃，剪裁，制得多层复合医用面料。
对比例1
对比例1的处方组成同实施例2。该多层复合医用面料的制备方法与实施例2的区别仅在于步骤（2）的不同，将步骤（2）修改为：（2）将醛基棉纤维分散在醛基棉纤维质量8倍的去离子水中，加入醛基棉纤维质量0.5倍的改性壳聚糖，在80rpm下搅拌，并滴加醛基棉纤维质量2~3倍的饱和碳酸钠溶液，滴加完成后继续搅拌，反应10h，捞出并用去离子水洗涤4次，置于烘箱中在50℃下干燥7h，制得改性棉纤维；将改性棉纤维进经倍捻、纺线、机织后，制得克重为100g/m2的亲肤层。
对比例2
对比例2的处方组成同实施例2。该多层复合医用面料的制备方法与实施例2的区别仅在于不进行步骤（1）的处理，并将步骤（2）修改为：将醛基棉纤维分散在醛基棉纤维质量8倍的去离子水中，加入醛基棉纤维质量0.5倍的壳聚糖，在80rpm下搅拌，并滴加醛基棉纤维质量2~3倍的饱和碳酸钠溶液，滴加完成后继续搅拌，反应10h，捞出并用去离子水洗涤4次，转移至醛基棉纤维质量8倍的无水乙醇中，加入醛基棉纤维质量倍的0.28倍的水合肼，继续搅拌反应4h，捞出并用去离子水洗涤6次，置于烘箱中在50℃下干燥7h，制得改性棉纤维；将改性棉纤维进经倍捻、纺线、机织后，制得克重为100g/m2的亲肤层。
对比例3
对比例3的处方组成同实施例2。该多层复合医用面料的制备方法与实施例2的区别仅在于步骤（1）（2）的不同，将步骤（1）（2）修改为：（1）室温下将棉纤维浸泡在棉纤维质量25倍质量分数为19%的氢氧化钠溶液中，反应3h后捞出，用去离子水洗涤6次，再浸泡在棉纤维质量45倍质量分数为8%的高碘酸钾溶液中，避光反应5h后捞出，转移至棉纤维质量15倍的甘油中，反应1h后捞出，用去离子水洗涤6次，烘干至恒重，制得改性棉纤维；（2）将改性棉纤维进经倍捻、纺线、机织后，制得克重为100g/m2的亲肤层。
对比例4
对比例4的处方组成同实施例2。该多层复合医用面料的制备方法与实施例2的区别仅在于不进行步骤（3）的处理，并将步骤（4）修改为：将对苯二胺与二甲基甲酰胺按质量比1:6混合，充分溶解后每隔11min加入2,2’-双(3,4-二羧苯基)六氟丙烷四酸二酐，控制加料时间为1.5h，2,2’-双(3,4-二羧苯基)六氟丙烷四酸二酐与对苯二胺的质量比为1.1:1，加料完成后在70rpm下搅拌均化5h，制得静电纺丝液，进行静电纺丝，静电纺丝时，注射器到铝箔的距离为18cm，纺丝液的推注速度为0.4mL/h，相对湿度为8%，温度为50℃，两极电压为25kV，制得交联聚酰亚胺纤维，将交联聚酰亚胺纤维进经倍捻、纺线、机织后，制得克重为50g/m2的交联层。
对比例5
对比例5的处方组成同实施例2。该多层复合医用面料的制备方法与实施例2的区别仅在于步骤（4）的不同，将步骤（4）修改为：将3,5-二(2-三氟甲基-4-氨基苯氧基)苯酚与二甲基甲酰胺按质量比1:6混合，充分溶解后每隔11min加入均苯四甲酸酐，控制加料时间为1.5h，均苯四甲酸酐与3,5-二(2-三氟甲基-4-氨基苯氧基)苯酚的质量比为1.1:1，加料完成后在70rpm下搅拌均化5h，制得静电纺丝液，进行静电纺丝，静电纺丝时，注射器到铝箔的距离为18cm，纺丝液的推注速度为0.4mL/h，相对湿度为8%，温度为50℃，两极电压为25kV，制得交联聚酰亚胺纤维，将交联聚酰亚胺纤维进经倍捻、纺线、机织后，制得克重为50g/m2的交联层
效果例1
下表1给出了采用本发明实施例1、2、3与对比例1、2、3、4、5的多层复合医用面料的各性能分析结果。
表1
抗菌率（%） 断裂伸长率（%）
实施例1 95.9 38.4
实施例2 94.3 37.2
实施例3 96.8 36.9
对比例1 78.2 35.7
对比例2 54.3 36.1
对比例3 21.4 37.3
对比例4 94.0 25.4
对比例5 93.7 21.6
通过表1中实施例与对比例的实验数据比较可以明显发现，实施例1、2、3制备的多层复合医用面料的抗菌性和断裂韧性较好；
从实施例1、2、3和对比例1、2、3的实验数据比较可发现，制备改性棉纤维时，醛基棉纤维上接枝壳聚糖与2,4,6-三(4-羟基苯基)吡啶反应制得的改性壳聚糖，再与水合肼反应，引入吡啶的同时引入大量羟基，改性壳聚糖上的羟基与棉纤维上的醛基反应形成缩醛，再与水合肼反应，形成席夫碱，将改性壳聚糖聚合在棉纤维表面，使得亲肤层具有优异的抗菌性；从实施例1、实施例2、实施例3和对比例4、5的实验数据比较可发现，由2,2’-双(3,4-二羧苯基)六氟丙烷四酸二酐与3,5-二(2-三氟甲基-4-氨基苯氧基)苯酚共混制得静电纺丝液进行静电纺丝制成聚酰亚胺纤维，编织成面料制得交联聚酰亚胺面料作为交联层，不仅形成内部为交联结构的聚酰亚胺，增强交联层的强度和断裂韧性，同时还带有微孔结构，与亲肤层和保护层进行压合时，可在两层之间吸附，使得层间连接紧密，增强面料的断裂韧性。
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 (1)

1.一种多层复合医用面料，由内到外包括亲肤层、交联层和保护层；其特征在于，所述亲肤层为改性棉纤维面料；所述交联层为交联聚酰亚胺面料；所述保护层是经过等离子体处理的聚丙烯无纺布；
所述改性棉纤维是在醛基棉纤维上接枝改性壳聚糖，再与水合肼反应制得；
所述交联聚酰亚胺面料是由2,2’-双(3,4-二羧苯基)六氟丙烷四酸二酐与3,5-二(2-三氟甲基-4-氨基苯氧基)苯酚共混制得静电纺丝液，进行静电纺丝制成聚酰亚胺纤维，编织成面料制得；
所述多层复合医用面料的制备方法为：亲肤层制备，交联层制备，保护层制备，多层复合医用面料制备；
所述多层复合医用面料的制备方法为：
（1）室温下将棉纤维浸泡在棉纤维质量20倍质量分数为18%的氢氧化钠溶液中，反应2h后捞出，用去离子水洗涤5次，再浸泡在棉纤维质量40倍质量分数为5%的高碘酸钾溶液中，避光反应4h后捞出，转移至棉纤维质量10倍的甘油中，反应1h后捞出，用去离子水洗涤5次，烘干至恒重，制得醛基棉纤维；将4-羟基苯基甲醛、4-羟基苯乙酮、乙酸铵和冰乙酸按质量比1:2:3:4.5混合加热至80℃，回流反应3h，冷却至室温后，加入4-羟基苯基甲醛8倍质量分数为50%的乙酸溶液进行沉析，并以100rpm搅拌10min后，过滤并用无水乙醇重结晶，最后在真空65℃下干燥12h，制得2,4,6-三(4-羟基苯基)吡啶；在氮气氛围下，将壳聚糖与N-甲基吡咯烷酮按质量比1:20混合，再以1ml/min的速率滴加壳聚糖质量2倍质量分数为2%的氯丁酰氯的N-甲基吡咯烷酮溶液，反应3h后，浓缩至用乙醚洗涤无沉淀生成，再用甲醇洗涤3次，加入壳聚糖质量1.5倍的2,4,6-三(4-羟基苯基)吡啶，在50rpm下搅拌反应72h，浓缩得沉淀，再依次用乙醚、甲醇洗涤3次，干燥至恒重，制得改性壳聚糖；
（2）将醛基棉纤维分散在醛基棉纤维质量5倍的去离子水中，加入醛基棉纤维质量0.4倍的改性壳聚糖，在50rpm下搅拌，并滴加醛基棉纤维质量2倍的饱和碳酸钠溶液，滴加完成后继续搅拌，反应8h，捞出并用去离子水洗涤3次，转移至醛基棉纤维质量5倍的无水乙醇中，加入醛基棉纤维质量倍的0.25倍的水合肼，继续搅拌反应3h，捞出并用去离子水洗涤5次，置于烘箱中在40℃下干燥6h，制得改性棉纤维；将改性棉纤维进经倍捻、纺线、机织后，制得克重为80g/m2的亲肤层；
（3）将间苯三酚、3-三氟甲基-4-氯硝基苯和污水碳酸钾按质量比3:11:4混合，并加入间苯三酚质量3.2倍的甲苯和间苯三酚质量16倍的N,N-二甲基甲酰胺，升温至115℃并在100rpm下搅拌反应5h，升温至150℃继续反应8h，冷却至室温后用去离子水洗涤3次，加入间苯三酚质量3.1倍的铁粉，再加入间苯三酚质量16倍的混合溶剂，混合溶剂中丙酮、乙醇和去离子水质量比为1:1:1，在氮气氛围下，升温至80℃并在50rpm下搅拌回流5h，加入间苯三酚质量0.08倍的氢氧化钠，继续搅拌5min后趁热过滤，再进行减压蒸馏，并用水和无水乙醇进行重结晶，制得3,5-二(2-三氟甲基-4-氨基苯氧基)苯酚；
（4）将3,5-二(2-三氟甲基-4-氨基苯氧基)苯酚与二甲基甲酰胺按质量比1:5混合，充分溶解后每隔10min加入2,2’-双(3,4-二羧苯基)六氟丙烷四酸二酐，控制加料时间为1.5h，2,2’-双(3,4-二羧苯基)六氟丙烷四酸二酐与3,5-二(2-三氟甲基-4-氨基苯氧基)苯酚的质量比为1:1，加料完成后在50rpm下搅拌均化4h，制得静电纺丝液，进行静电纺丝，静电纺丝时，注射器到铝箔的距离为15cm，纺丝液的推注速度为0.24mL/h，相对湿度为5%，温度为40℃，两极电压为15kV，制得交联聚酰亚胺纤维，将交联聚酰亚胺纤维进经倍捻、纺线、机织后，制得克重为40g/m2的交联层；
（5）将克重为30g/m2聚丙烯无纺布浸泡在无水乙醇中，24h后捞出晾干，再浸泡在丙酮中，在40kHz下进行超声洗涤20min，捞出后用去离子水洗涤3次，置于40℃烘箱中干燥至恒重，制得预处理聚丙烯无纺布；将预处理聚丙烯无纺布悬挂于等离子体仪的处理腔中，抽真空至5Pa后，通氧气至真空度为15Pa，在90W下进行等离子体处理，时间为4min，制得保护层；
（6）依次放置亲肤层、交联层和保护层，用热压机进行压合，压合温度为150℃，剪裁，制得多层复合医用面料。
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