CN109281161B - 一种多功能粘胶纤维复合材料的制备方法 - Google Patents

一种多功能粘胶纤维复合材料的制备方法 Download PDF

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CN109281161B
CN109281161B CN201811174152.8A CN201811174152A CN109281161B CN 109281161 B CN109281161 B CN 109281161B CN 201811174152 A CN201811174152 A CN 201811174152A CN 109281161 B CN109281161 B CN 109281161B
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张春晓
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Abstract

本发明实施例公开了一种多功能粘胶纤维复合材料的制备方法，所制备的粘胶纤维复合材料可以实现对染料(如甲基橙、次甲基蓝等)的选择性吸附，而且可以吸附空气中的甲醛、二氧化碳、细菌等污染物，同时实现对污染物的杀菌及催化分解。

Description

一种多功能粘胶纤维复合材料的制备方法
技术领域
本发明涉及高分子材料技术领域，具体涉及一种多功能粘胶纤维复合材料的制备方法。
背景技术
1891年，Cross和他的同事发现，纤维素可以在碱性二硫化溶液中转化为水溶性磺酸盐，并通过还原得到粘胶纤维。1905年，Muller进一步改进了粘胶纤维的生产工艺，实现了粘胶纤维的产业化，并很快得到了广泛的应用。近年来，出现了Lycell、Modal、Richcel等新品种。在所有的再生纤维素纤维中，粘胶纤维的吸湿性最适合人类皮肤的生理要求。同时，粘胶纤维具有透气、耐磨、不容易产生静电等优点。另外，粘胶纤维还可以与各种天然纤维和化学纤维混纺。因此，粘胶纤维不仅可以作为一个优秀的服用材料，而且在吸附抗菌材料、高吸水医疗卫生产品等领域也得到了广泛的应用。但粘胶纤维也有湿强度低、高伸长率、易燃性等缺点。
为了提高粘胶纤维的性能，拓展粘胶纤维的应用领域，常采用化学方法对粘胶纤维进行改性。粘胶纤维每个葡萄糖单元有三个羟基，因此可以发生一系列与羟基有关的化学反应，包括酯化反应、醚化反应、交联和接枝反应。此外，以壳聚糖、聚乳酸和纳米银粒子等为原料制备的粘胶纤维复合材料也得到了广泛的研究和应用。
目前，粘胶纤维的改性主要集中在阻燃、抗菌、吸湿性、染色、吸附等方面。
国内学者对粘胶纤维的改性及应用开展了大量的研究并取得了一定的进展。陈胜研究了烷氧基环三磷腈共混改性阻燃粘胶纤维的燃烧性能和热性能。结果表明，所制备的共混改性纤维具有凝聚相阻燃机理，同时具有吸热阻燃和气相阻燃等多重的阻燃作用。王雪以粘胶纤维为基体，通过接枝含季铵基烯类单体制备了一种季铵盐型抗菌纤维材料。抗菌试验显示，该改性抗菌纤维对大肠杆菌、金黄色葡萄球菌及白色念珠菌有优越的抗菌性能，抗菌率均达到了99.99％。朱平将粘胶纤维进行了羧甲基化改性，并对改性后纤维的吸水性、拉伸强力等物理性能进行了测试，结果表明：改性后粘胶纤维强力有一定下降，吸水率大大提高，达到原干重的4.5倍以上。黄韬采用阳离子改性剂CR2000对粘棉交织物进行改性处理，改性粘棉交织物活性染色得色量高、染色牢度好，染料利用率大大提高，染色残液的COD值大幅降低。荣海琴将粘胶基活性碳纤维(Rayon-ACFs)用一定浓度的对氨基苯甲酸(p-PABA)溶液进行改性，通过低温氮气吸附方法发现，随着PABA浓度的增加，样品的比表面积、微孔孔容和总孔容都有所降低。改性后的Rayon-ACFs样品对甲醛的动态穿透时间和吸附容量都明显高于未改性的Rayon-ACFs样品。
国外科研工作者采用化学改性、等离子体改性、混纺复合等方法对粘胶纤维的改性及应用进行了广泛、系统的研究。Bychkova用磷酸二甲酯对粘胶纤维进行了改性，并对其结构和防火性能进行了研究，改性后的粘胶纤维展现了良好的阻燃性能。Totolin研究了粘胶剂的等离子体改性，改性纤维素纤维具有显著的阻燃性能。Akbari研究了两种不同再生纤维素纤维(Lyocell和粘胶)的酶处理对水悬液中细菌吸附能力的影响。经处理后的Lyocell和粘胶，从水悬浮液中提取大肠杆菌的最大吸附量分别为38％和37％。Vrabic研究了用于卫生和医疗产品的粘胶纤维的物理性能和吸附特性。研究表明，经过5分钟等离子体表面处理，改性粘胶纤维的聚合度和机械性能有一定的下降，但是吸水性能和保湿性能都到了提高。zeng研究了粘胶/甲壳素双组分纤维的染色性能，与普通粘胶纤维相比，粘胶/甲壳素双组分纤维由于其部分脱乙酰组分，对染料的吸附性能更好。Bairagi用不同剂量的聚二烯基二甲基氯化铵对粘胶纤维进行改性。然后采用不同活性染料对改性纤维进行染色，在不使用电解液和低盐浓度的情况下，获得了90％以上的染色效果。Salwa利用柠檬酸三钠作为多功能剂(还原剂、稳定剂和链接剂)，将银纳米粒子(AgNPs)原位合成到粘胶纤维的表面。负载AgNPS的粘胶纤维着色和抗菌性能显著提高。Kebede将粘胶纤维被选择性地氧化，然后引入聚酰胺-胺树枝状大分子，改性后的粘胶纤维对甲醛展现了良好的吸附性能，比改性前提高了84倍。
综合国内外的研究现状，对粘胶纤维进行物理化学改性或与其它材料进行复合，是目前功能化粘胶纤维性能的主要方法。目前，对粘胶纤维的改性主要集中在单一化学改性。随着研究的的深入，多功能、智能化改性粘胶纤维产品，能够解决生产、生活中的实际问题，如广谱性抗菌、染料及甲醛污染物吸附与降解、阻燃性能、染色及固色性能将是未来的发展趋势。
发明内容
本发明实施例的目的在于提供一种多功能粘胶纤维复合材料的制备方法，所制备的粘胶纤维复合材料可以实现对染料(如甲基橙、次甲基蓝等)的选择性吸附，而且可以吸附空气中的甲醛、二氧化碳、细菌等污染物，同时实现对污染物的杀菌及催化分解。
为实现上述目的，本发明实施例提供一种多功能粘胶纤维复合材料的制备方法，所述方法包括下列步骤：
(1)以粘胶纤维为母体，氯乙酸钠为阴离子改性试剂，在氢氧化钠的催化下，制备阴离子改性粘胶纤维；
(2)以步骤(1)的阴离子改性粘胶纤维为原料，超支化聚乙烯亚胺(HPEI)为大分子改性试剂，以1-(3-二甲氨基丙基)-3-乙基碳二亚胺(EDC)和N-羟基琥珀酰亚胺(NHS)为缩合剂，通过酰胺化反应得到同时接枝有羧基和HPEI的两性粘胶纤维；
(3)将步骤(2)的两性粘胶纤维放入到HAuCl4溶液中，在NaBH4的还原作用下，得到负载金纳米粒子的多功能粘胶纤维复合材料。
进一步的，步骤(1)中，可以采用NMR、IR等手段对步骤(1)获得的阴离子改性粘胶纤维进行表征。
进一步的，步骤(2)中，可以采用NMR、IR等手段对步骤(2)获得的两性粘胶纤维进行表征，同时采用化学法测定所述两性粘胶纤维上接枝羧基和氨基的数量。
进一步的，步骤(3)中，可以采用IR、TG、TEM等手段对步骤(3)获得的多功能粘胶纤维复合材料进行表征，以进一步分析所述多功能粘胶纤维复合材料的精细结构。
进一步的，步骤(3)中，所获得的多功能粘胶纤维复合材料的负载金纳米粒子的粒径小于10nm，例如1-6nm。
进一步的，所述方法还包括下列步骤：
(4)以甲基橙(阴离子型)和次甲基蓝(阳离子型)的混合溶液为研究模型，在不同pH条件下评价所述多功能粘胶纤维复合材料对染料的选择性吸附和释放。
本发明实施例的技术方案以粘胶纤维为母体，以氯乙酸钠为小分子改性试剂，在NaOH的催化作用下，得到羧甲基粘胶纤维；接着通过酰胺化反应实现超支化聚乙烯亚胺(HPEI)在粘胶纤维上的接枝，得到同时具有羧基和氨基的两性粘胶纤维；然后将两性粘胶纤维放入到HAuCl4溶液中，在NaBH4还原作用下，得到负载金纳米粒子的多功能粘胶纤维复合材料。
本发明实施例的技术方案具有如下优点：
1、该多功能改性粘胶纤维复合材料，由于表面含有大量的羧基和氨基基团，同时负载有金纳米粒子，不但可以实现对染料(如甲基橙、次甲基蓝等)的选择性吸附，而且可以吸附空气中的甲醛、二氧化碳、细菌等污染物，同时实现对污染物的杀菌及催化分解，在服用材料、催化、污水处理、空气净化以及伤口医用材料等领域有着广泛的应用前景。
2、制备工艺稳定，效率高，对环境影响小，便于推广。
附图说明
图1为本发明实施例1提供的所述多功能粘胶纤维复合材料的合成工艺技术路线图。
具体实施方式
以下由特定的具体实施例说明本发明的实施方式，熟悉此技术的人士可由本说明书所揭露的内容轻易地了解本发明的其他优点及功效。
须知，本说明书所附图式所绘示的结构、比例、大小等，均仅用以配合说明书所揭示的内容，以供熟悉此技术的人士了解与阅读，并非用以限定本发明可实施的限定条件，故不具技术上的实质意义，任何结构的修饰、比例关系的改变或大小的调整，在不影响本发明所能产生的功效及所能达成的目的下，均应仍落在本发明所揭示的技术内容得能涵盖的范围内。同时，本说明书中所引用的如“上”、“下”、“左”、右”、“中间”等的用语，亦仅为便于叙述的明了，而非用以限定本发明可实施的范围，其相对关系的改变或调整，在无实质变更技术内容下，当亦视为本发明可实施的范畴。
实施例1
参见图1，显示了本发明实施例提供的所述多功能粘胶纤维复合材料的合成工艺技术路线图。所述技术路线包括：
第一步：以粘胶纤维为母体，以氯乙酸钠为阴离子改性试剂，在氢氧化钠的催化下，制备阴离子改性粘胶纤维；
第二步：以制备的阴离子改性粘胶纤维为原料，超支化聚乙烯亚胺(HPEI)为大分子改性试剂，以1-(3-二甲氨基丙基)-3-乙基碳二亚胺(EDC)和N-羟基琥珀酰亚胺(NHS)为缩合剂，通过酰胺化反应得到同时接枝有羧基和HPEI的两性粘胶纤维；
第三步：将两性粘胶纤维放入到HAuCl4溶液中，在NaBH4还原作用下，得到负载金纳米粒子(粒径小于10nm)的多功能粘胶纤维复合材料。
实施例2
本实施例中多功能粘胶纤维复合材料的制备方法具体包括下列步骤：
(1)在水溶液体系中，先加入2.76g的粘胶纤维，然后加入3.3克10％氢氧化钠，搅拌反应2小时，然后加入1.1g氯乙酸钠，升温至70℃，搅拌反应2小时，然后用盐酸中和到中性，洗涤干燥得到阴离子改性粘胶纤维，实现羧基的引入；
(2)在水溶液体系中加入制备的阴离子改性粘胶纤维(1g，1wt％)，调整体系的pH值至pH10左右，然后按照比例加入缩合剂EDC和NHS(与羧基的摩尔比为1:1:1)，轻微搅拌1小时，然后加入1.5g的超支化聚乙烯亚胺(HPEI)，反应2个小时，过滤，洗涤干燥，得到同时接枝有羧基和HPEI的两性粘胶纤维，同时采用化学法测定粘胶纤维上接枝羧基和氨基的数量；
(3)取定量的两性粘胶纤维放入到450ml的HAuCl4溶液中(2×10-4M)，保持搅拌0.5小时，然后过滤，用去离子水洗涤，得到吸附HAuCl4的改性粘胶纤维，接着将纤维放入到450ml的NaBH4溶液中(2×10-2M)，反应0.5小时后，过滤洗涤，干燥得到负载金纳米粒子的多功能粘胶纤维复合材料。
本技术方案以小分子的氯乙酸钠和大分子的超支化聚乙烯亚胺(HPEI)为改性试剂，得到两性粘胶纤维，然后利用大分子超支化聚乙烯亚胺(HPEI)的稳定作用，实现对金纳米粒子的负载，最终得到多功能的粘胶纤维复合材料。该多功能粘胶纤维复合材料可以实现对染料(如甲基橙、次甲基蓝等)的选择性吸附，而且可以吸附空气中的甲醛、二氧化碳、细菌等污染物，同时实现对污染物的杀菌及催化分解。
虽然，上文中已经用一般性说明及具体实施例对本发明作了详尽的描述，但在本发明基础上，可以对之作一些修改或改进，这对本领域技术人员而言是显而易见的。因此，在不偏离本发明精神的基础上所做的这些修改或改进，均属于本发明要求保护的范围。

Claims (6)

1.一种多功能粘胶纤维复合材料的制备方法，其特征在于，所述方法包括下列步骤：
(1)以粘胶纤维为母体，氯乙酸钠为阴离子改性试剂，在氢氧化钠的催化下，制备阴离子改性粘胶纤维；
(2)以步骤(1)的阴离子改性粘胶纤维为原料，超支化聚乙烯亚胺(HPEI)为大分子改性试剂，以1-(3-二甲氨基丙基)-3-乙基碳二亚胺(EDC)和N-羟基琥珀酰亚胺(NHS)为缩合剂，通过酰胺化反应得到同时接枝有羧基和超支化聚乙烯亚胺的两性粘胶纤维；
(3)将步骤(2)的两性粘胶纤维放入到HAuCl4溶液中，在NaBH4的还原作用下，得到负载金纳米粒子的多功能粘胶纤维复合材料。
2.根据权利要求1所述的多功能粘胶纤维复合材料的制备方法，其特征在于，步骤(1)中，采用NMR或IR对步骤(1)获得的阴离子改性粘胶纤维进行表征。
3.根据权利要求1所述的多功能粘胶纤维复合材料的制备方法，其特征在于，步骤(2)中，采用NMR或IR对步骤(2)获得的两性粘胶纤维进行表征，同时采用化学法测定所述两性粘胶纤维上接枝羧基和氨基的数量。
4.根据权利要求1所述的多功能粘胶纤维复合材料的制备方法，其特征在于，步骤(3)中，采用IR、TG或TEM对步骤(3)获得的多功能粘胶纤维复合材料进行表征，以进一步分析所述多功能粘胶纤维复合材料的精细结构。
5.根据权利要求1所述的多功能粘胶纤维复合材料的制备方法，其特征在于，步骤(3)中，所获得的多功能粘胶纤维复合材料的负载金纳米粒子的粒径小于10nm。
6.根据权利要求1所述的多功能粘胶纤维复合材料的制备方法，其特征在于，所述方法还包括下列步骤：
(4)以甲基橙和次甲基蓝的混合溶液为研究模型，在不同pH条件下评价所述多功能粘胶纤维复合材料对染料的选择性吸附和释放。
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