CN106978732A - 一种基于羽毛改性的表面亲水性纤维及其制备方法 - Google Patents
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Abstract
本发明提供了一种基于废弃羽毛的表面亲水性纤维的制备方法，是将废弃羽毛纤维洗净后，浸于溶解有还原剂和保护剂的水溶液中，在震摇下升温至50~85℃，继续震摇20~90分钟；再加入改性剂和分散剂，继续震摇1~5小时；然后冷却至室温，取出羽毛纤维，用蒸馏水冲洗，干燥，得到表面改性的羽毛纤维。本发明通过对废弃羽毛进行表面改性，使其具有水下超疏油的特殊浸润性，此类特殊浸润性表面材料可应用于防污涂层、防指纹涂层、微液滴传递技术、油水分离等应用领域。另外，改性后羽毛的亲水性能有很大提升，远远超出未改性羽毛的吸水倍率。因此可作为吸水材料应用于微液滴传递技术、油水分离、保水、保鲜及建筑防水等领域。
Description
技术领域
本发明涉及一种具有特殊浸润性天然高分子材料的制备方法，尤其涉及一种基于废弃羽毛的表面亲水性纤维的制备方法，属于功能材料技术领域。
背景技术
随着材料科学的发展，基于特殊润湿性材料的研究受到关注，如：表面超亲水、超疏水、超亲油、超疏油、超双亲、超双疏等材料，并在自清洁表面、防雾涂层、防污涂层、防指纹涂层、微液滴传递技术、油水分离等领域正在或即将获得应用。近年来，发现通过改性等方法，研究了很多亲水性及特殊浸润性材料。如：发明CN201510698160.2中提供一种新的自润滑亲水涂料，解决涂料体系存在的热传导效率较低，亲水性较低的问题。CN201510030697.1发明中采用一步水热法制备了用氟硅烷修饰TiO2膜层，使其具有微纳结构，提供了一种具有紫外防护和耐水洗的特殊浸润性功能表面的构筑方法，从而解决制备超疏水自清洁表面操作工艺复杂、稳定性差、膜层形貌不可控的问题。CN201510968274.4中发明了一种集成两种特殊浸润性材料的T型油水分离设备，从而解决了液层阻碍问题，实现了连续、高效、高通量的油水分离。当然，如何降低成本、提高环境友好性能尚未受到足够重视。
羽毛是禽类的表皮细胞生长出来的一种角质化产物，其中含有角蛋白，蛋白链之间的二硫键使其具有刚性结构，这种刚性结构很难使羽毛具有亲水性。因此，难以将羽毛作为亲水材料使用。羽毛作为天然高分子材料，具有可再生、易获得及储量丰富等特点，因此，从废弃生物质资源再利用角度出发，已有相关研究报道：如：从羽毛中提取角蛋白后，可用于环境敏感的水凝胶（CN201510299512.7，CN201510621974.6）；将羽毛与其他生物质混合纺丝制备成复合纤维材料用于纺织领域（CN201410141073.2）等等。羽毛角蛋白也可以用于制备外敷材料（CN201610378592.X，CN201610378278.1）、羽毛角蛋白修饰光催化剂（201510070774.6）等。但是，由于羽毛纤维疏水亲油的特点，使其应用受到限制。目前，将羽毛经过改性成具有特殊浸润性材料的研究未见报道。
发明内容
本发明目的是提供一种基于废弃羽毛的表面亲水性纤维的制备方法。
一、基于羽毛纤维的表面亲水性材料的制备
本发明表面亲水性纤维材料的制备，是基于羽毛疏水亲油的特点，将其改性为表面亲水性材料。具体方法如下：
将废弃的羽毛纤维洗净后，浸于溶解有还原剂和保护剂的水溶液中，在震摇下升温至50~85℃，继续震摇20~90 分钟；再加入改性剂和分散剂，继续震摇1~5 h；然后冷却至室温，取出羽毛纤维，用蒸馏水冲洗，干燥，得到表面改性的羽毛纤维。
所述废弃的羽毛纤维是指来源于养鸡场或农贸市场中废弃的鸡毛、鸭毛及其他家禽羽毛，将收集的废弃羽毛经过清洗、晾干后，剪切为形貌相对规整的羽毛纤维。
所述还原剂为亚硫酸钠、亚硫酸氢钠、硫化钠中的任意一种或两种，还原剂加入量为羽毛纤维质量的0.1~0.25倍。
所述保护剂为月桂醇硫酸钠、脂肪醇聚氧乙烯醚硫酸酯盐、脂肪醇硫酸酯单乙醇胺盐中的任意一种或两种，保护剂加入量为羽毛纤维质量的0.1~0.15倍
所述改性剂为硅烷偶联剂KH570或氯甲基乙烯基二甲基硅烷，改性剂加入量为羽毛纤维质量的1~1.2倍。
所述分散剂为乙醇或甲醇，分散剂加入量为5~10 mL/g羽毛纤维。
所述干燥是在50℃~80℃下真空干燥6~12小时。
二、表面亲水化改性的羽毛纤维结构表征
通过扫描电子显微镜观察表面亲水化改性羽毛纤维的外观形貌，通过红外光谱考察了其功能基团的变化，说明亲水性能的有效提高使羽毛纤维的亲油性能被掩盖，从而具有水下疏油的特殊浸润性能。
1、扫描电镜
图1为表面亲水化改性羽毛纤维的扫描电镜。可以明显看出，改性后的羽毛纤维表面（b）出现一层包裹物而明显变得粗糙，而未改性的羽毛纤维表面（a）相对光滑平整。另外，观察羽毛纤维在表面改性前后的外观形貌，发现羽毛纤维保持了原来的外观，说明表面改性不破坏整体形貌。
2、红外图谱
图2为表面亲水化改性的羽毛纤维的红外吸收光谱。其中，在1650 cm-1、1528 cm-1、1232 cm-1附近出现了蛋白的特征吸收峰（酰胺I、II、III带），说明蛋白质材料的基本构架得到保持。另外，3550~3750 cm-1的宽泛吸收带和1200 cm-1附近的吸收峰分别代表改性后羽毛表面吸附水的O-H伸缩振动和弯曲振动，905 cm-1附近的吸收峰是Si-OH的伸缩振动；在3280 cm-1附近可看到代表-CH2以及-CH3的C-H伸缩振动吸收峰变得很尖锐；670 cm-1处S-S键的特征吸收峰变得平缓，说明此官能团有所减少。由此说明成功将硅烷偶联剂接枝到羽毛表面，从而使其含有大量的羟基。
三、表面亲水化改性羽毛纤维的性能测试
1、空气中与水的接触角测试
图3为亲水化改性后羽毛纤维在空气中与水的接触角。由图中可以看出，水滴在改性后的羽毛上呈现浸润状态，尤其是水滴在羽轴上几乎平铺。测得改性后的羽毛接触角为25.35°，羽绒为74.11°，表现为亲水性。这与未改性的羽毛纤维疏水性（接触角羽轴134.70°；羽绒150.11°）完全不同。
2、水下与油的接触角测试
实验分别测试了亲水性羽毛在水下对柴油和氯仿的接触角，结果见图4。改性羽毛在水下对柴油的接触角为134.04°（图4a），对氯仿油的接触角为143.84°（图4b）。表明改性羽毛具有水下疏油的特点，该性能可应用于微液滴传递技术、油水分离等领域。
3、油-水混合液中的特殊浸润性能测试
测试了表面亲水化改性羽毛纤维在油-水混合液中的特殊浸润性能，并与未改性羽毛纤维进行对比。图5a、5b为未改性羽毛纤维浸入油-水混合液的前后照片；图5c、5d为表面亲水化改性羽毛纤维浸入油-水混合液的前后照片，其中油相用深色染料标记。可以看出未改性羽毛浸入油-水混合液后，被深色标记染色，颜色较深。而表面亲水化改性的羽毛纤维浸入油-水混合液后没有被染色，说明表面亲水化改性的羽毛纤维具有水下疏油的特殊浸润性能，因此可作为浸润材料应用于防油污、生物黏附等领域。
4、吸水性能测试
为了评价表面亲水化改性羽毛纤维对水的吸附能力，进一步做了如下实验：室温下，取一定量的改性羽毛纤维，分别在30 mL水中浸润30分钟，再静置20分钟，称重，计算吸水倍率（g/g），测试改性羽毛对水的吸附能力，晾干，循环测定。
图6为表面亲水化改性羽毛纤维的吸水性能图。可以看出，表面亲水化改性羽毛纤维的吸水倍率约为7~9 g/g，对比未改性羽毛（吸水倍率小于0.7 g/g），表面亲水化改性后羽毛的吸水性能显著提高。因此，改性羽毛纤维可作为吸水材料应用于保水、保鲜及建筑防水等领域。
综上所述，本发明以废弃羽毛作为天然高分子材料，通过表面改性，在保持原有亲油性能的基础上使其具有了良好的亲水性，从而使其有水下超疏油的特殊浸润性，此类特殊浸润性表面材料可应用于防雾涂层，防污涂层、防指纹涂层、微液滴传递技术、油水分离等领域。另外，改性后羽毛的亲水性有很大提升，对水的吸附倍率可达10倍之多，远远超出未改性羽毛的吸水倍率。因此可作为吸水材料应用于保水、保鲜及建筑防水等领域。
附图说明
图1为表面亲水化改性羽毛纤维（b）与未改性的羽毛纤维（a）的扫描电镜图。
图2为表面亲水化改性羽毛纤维的红外吸收光谱图。
图3为表面亲水化改性羽毛纤维在空气中对水的接触角。
图4为表面亲水化改性羽毛纤维在水下对油的接触角。
图5为改性前后羽毛在油-水混合液中的浸润性能。
图6为表面亲水化改性羽毛纤维的吸水性能。
具体实施方式
下面通过具体实施例对本发明羽毛表面改性的亲水性纤维的制备及其特殊浸润性能做进一步说明。
实施例1
将1 g洗净的废弃羽毛纤维，浸润于50 mL的水溶液中（含0.1 g亚硫酸钠和0.1 g月桂醇硫酸钠）；在震摇下将溶液缓慢升温至50℃，在此温度下继续震摇1.5小时；然后加入1 g硅烷偶联剂KH570、10 mL的甲醇，继续在摇床中震摇3小时。冷却至室温后，取出羽毛纤维，用蒸馏水冲洗5~10次，70℃下真空干燥10小时，得到表面改性的羽毛纤维。
选取相同质量的未改性羽毛和改性羽毛，分别测试羽毛对水的吸附性能。结果表明未改性的羽毛吸水倍率为0.73 g/g，改性后的羽毛吸水倍率为7.85 g/g。
实施例2
将10 g洗净的废弃羽毛纤维，浸润于500 mL水溶液中（含2.5 g亚硫酸氢钠和2.5 g脂肪醇聚氧乙烯醚硫酸酯盐），在震摇下缓慢将溶液升温至70℃，在此温度下继续震摇1小时；然后加入12 g氯甲基乙烯基二甲基硅烷、150 mL的乙醇，继续在摇床中震摇2小时。冷却至室温后，取出表面改性的羽毛纤维，用蒸馏水冲洗5~10次，60℃下真空干燥12小时，得到表面改性的羽毛纤维。
选取相同质量的未改性羽毛和改性羽毛，分别测试羽毛对水的吸附性能。结果表明，未改性的羽毛吸水倍率为0.40 g/g，改性后的羽毛吸水倍率为8.14 g/g。
实施例3
将5 g洗净的废弃羽毛纤维，浸润于300 mL（含1.0 g硫化钠和1.0 g脂肪醇硫酸酯单乙醇胺盐）水溶液中，在震摇下，将溶液缓慢升温至65℃，在此温度下继续震摇80 分钟，然后加入5 g硅烷偶联剂KH570、30 mL的乙醇，继续在摇床中震摇3小时；冷却至室温后，取出表面改性的羽毛纤维，用蒸馏水冲洗5~10次，65℃下真空干燥10小时，得到表面改性的羽毛纤维。
选取相同质量的未改性羽毛和改性羽毛，分别测试羽毛对水的吸附性能。结果表明未改性的羽毛吸水倍率为0.25 g/g，改性后的羽毛吸水倍率为7.81 g/g。
实施例4
将3 g洗净的废弃羽毛纤维，浸润于100 mL（含0.5 g亚硫酸钠-亚硫酸氢钠复配物和0.2 g月桂醇硫酸钠）水溶液中，在震摇下，将溶液缓慢升温至85℃，在此温度下继续震摇20分钟；然后加入4 g硅烷偶联剂KH570、20 mL甲醇，继续在摇床中震摇1小时；冷却至室温后，取出表面改性的羽毛纤维，用蒸馏水冲洗5~10次，65℃下真空干燥12小时，得到表面改性的羽毛纤维。
选取相同质量的未改性羽毛和改性羽毛，分别测试羽毛对水的吸附性能。结果表明未改性的羽毛吸水倍率为0.39 g/g，改性后的羽毛吸水倍率为7.80 g/g。
实施例5
将8 g洗净的废弃羽毛纤维，浸润于400 mL（含2 g亚硫酸氢钠-硫化钠复配物和1 g脂肪醇硫酸酯单乙醇胺盐 ）水溶液中，在震摇下缓慢将溶液升温至80℃，继续震摇40 分钟；然后加入9 g氯甲基乙烯基二甲基硅烷、40 mL的乙醇，继续在摇床中震摇3.5小时；冷却至室温后，取出表面改性的羽毛纤维，用蒸馏水冲洗5~10次，65℃下真空干燥12小时，得到表面改性的羽毛纤维。
选取相同质量的未改性羽毛和改性羽毛，分别测试羽毛对水的吸附性能。结果表明未改性的羽毛吸水倍率为0.15 g/g，改性后的羽毛吸水倍率为7.30 g/g。
Claims (10)
1.一种基于废弃羽毛的表面亲水性纤维的制备方法，是将废弃的羽毛纤维洗净后，浸于溶解有还原剂和保护剂的水溶液中，在震摇下升温至50~85℃，继续震摇20~90 分钟；再加入改性剂和分散剂，继续震摇1~5小时；然后冷却至室温，取出羽毛纤维，用蒸馏水冲洗，干燥，得到表面改性的羽毛纤维。
2.如权利要求1所述基于废弃羽毛的表面亲水性纤维的制备方法，其特征在于：所述还原剂为亚硫酸钠、亚硫酸氢钠、硫化钠中的任意一种或两种。
3.如权利要求2所述基于废弃羽毛的表面亲水性纤维的制备方法，其特征在于：还原剂加入量为羽毛纤维质量的0.1~0.25倍。
4.如权利要求1所述基于废弃羽毛的表面亲水性纤维的制备方法，其特征在于：所述保护剂为月桂醇硫酸钠、脂肪醇聚氧乙烯醚硫酸酯盐、脂肪醇硫酸酯单乙醇胺盐中的任意一种或两种。
5.如权利要求4所述基于废弃羽毛的表面亲水性纤维的制备方法，其特征在于：保护剂加入量为羽毛纤维质量的0.1~0.15倍。
6.如权利要求1所述基于废弃羽毛的表面亲水性纤维的制备方法，其特征在于：所述改性剂为硅烷偶联剂KH570或氯甲基乙烯基二甲基硅烷。
7.如权利要求6所述基于废弃羽毛的表面亲水性纤维的制备方法，其特征在于：改性剂加入量为羽毛纤维质量的1 ~1.2倍。
8.如权利要求1所述基于废弃羽毛的表面亲水性纤维的制备方法，其特征在于：分散剂为乙醇或甲醇。
9.如权利要求1所述基于废弃羽毛的表面亲水性纤维的制备方法，其特征在于：分散剂加入量为5~10 ml/g羽毛纤维。
10.如权利要求1所述方法制备的基于废弃羽毛的表面亲水性纤维，其特征在于：所述干燥是在50℃~80℃下真空干燥6~12小时。
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