CN112301541B - 一种易降解可重复使用高效非织造吸油材料及其制备方法 - Google Patents

一种易降解可重复使用高效非织造吸油材料及其制备方法 Download PDF

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CN112301541B
CN112301541B CN202011122850.0A CN202011122850A CN112301541B CN 112301541 B CN112301541 B CN 112301541B CN 202011122850 A CN202011122850 A CN 202011122850A CN 112301541 B CN112301541 B CN 112301541B
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本德萍
王彩英
黄林涛
李双
吴昭君
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Xian Polytechnic University
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Abstract

本发明公开了一种易降解可重复使用高效非织造吸油材料及其制备方法。该材料由疏水的三维多孔非织造材料和静电纺纳米微孔纤维膜组成。非织造吸油材料制备方法包括几个步骤：首先采用非织造方法制得三维多孔非织造材料，再利用静电纺丝法得到纳米微孔纤维膜，然后应用化学粘合法在三维多孔非织造材料上复合纳米微孔纤维膜，制得微纳梯度孔结构的非织造吸油材料。与现有吸油材料相比，本发明的非织造吸油材料，不仅容易降解，吸油量大，而且保油率高，油水分离效果好，还可以多次重复使用，在陆地、海洋、河流等溢油处理方面具有广泛的应用前景。

Description

一种易降解可重复使用高效非织造吸油材料及其制备方法
技术领域
本发明属于吸附材料技术领域，涉及一种易降解可重复使用高效非织造吸油材料，还涉及该非织造吸油材料的制备方法。
背景技术
随经济快速增长，海上原油开采及运输量增加，频繁发生的石油泄漏事故造成的水体油污染，已经对人类及海洋生物的生命构成一定的威胁，对溢油的处理引起人们的高度关注。吸油材料吸附处理是目前最为有效的方法，非织造吸油材料因其吸油速率快、可多次重复使用、能吸附自身10-20倍油液而被广泛用于油污处理。
聚丙烯熔喷非织造材料具有较强的疏水亲油性，吸油性能优异，但存在结构单一、强度低、保油率低、使用后很难降解，容易增加环境负担等缺点。以荨麻、木棉等天然纤维开发的非织造吸油材料使用后可以降解、吸油速率快、饱和吸油量高、保油率高，但存在吸油的同时吸水、受外力挤压时易漏油等问题。
近年来以可降解的聚乳酸为原料制备的静电纺纤维膜，疏水亲油性能好，使用后可完全降解，吸油量高，但难以重复使用，使用成本高。
综上所述，以天然纤维或可降解聚合物为原料，开发环保型、可多次重复使用的高性能吸油材料十分必要。
发明内容
本发明的目的在于提供一种易降解可重复使用高效非织造吸油材料，解决了现有吸油材料的难降解、吸油量低、结构单一等问题。
本发明的目的还在于提供一种上述易降解可重复使用高效非织造吸油材料的制备方法，以三维多孔非织造材料为基材，采用化学粘合法在三维多孔非织造材料上复合静电纺纳米微孔纤维膜，构建具有微纳梯度孔结构非织造布吸油材料，解决天然纤维油水分离性差、静电纺纤维膜强度低，难以重复使用的问题。
本发明所采用的第一种技术方案是，易降解可重复使用高效非织造吸油材料，易降解可重复使用高效非织造吸油材料是由三维多孔非织造材料和静电纺纳米微孔纤维膜通过化学粘合法复合构成的具有微纳梯度孔结构的非织造布吸油材料，吸油材料的孔隙率为90.37％-93.32％，孔径为23-172μm；三维多孔非织造材料和静电纺纳米微孔纤维膜是疏水的。
本发明的特点还在于，
三维多孔非织造材料包括针刺非织造材料、纺粘非织造材料、熔喷非织造材料或缝编非织造材料，三维多孔非织造材料优选为针刺非织造材料。
三维多孔非织造材料所用纤维包括木棉、棉、麻、荨麻、丝、毛或聚乳酸纤维。
静电纺纳米微孔纤维膜所用原料为聚乳酸，聚乳酸分子量为10万。
本发明所采用的第二种技术方案是，一种易降解可重复使用高效非织造吸油材料的制备方法，具体操作步骤如下：
步骤1：采用非织造加工法制得三维多孔非织造材料
以木棉纤维和聚乳酸纤维为原料，通过混合、开松、梳理、铺网、针刺加工得到针刺三维多孔非织造材料；
步骤2：利用静电纺丝法得到纳米微孔纤维膜
将聚乳酸溶于二氯甲烷和乙醇中，得到聚乳酸纺丝液，然后进行静电纺丝，设置纺丝电压为28～30kV，接受距离为15～17cm，相对湿度为60～70％，制得聚乳酸静电纺纳米微孔纤维膜；
步骤3：应用化学粘合法将三维多孔非织造材料与纳米微孔纤维膜复合，制得微纳梯度孔结构的非织造吸油材料.
将粘合剂溶液喷洒在步骤1制备的三维多孔非织造材料上，再将静电纺纳米微孔纤维膜覆盖在上面，放入烘箱干燥，制得微纳梯度孔结构非织造吸油材料。
本发明的特点还在于，
步骤1木棉和聚乳酸纤维混合比为30/70～60/40，三维多孔非织造材料克重为100～180g/m2、针刺密度为180～300刺/cm2。
步骤2乙醇可以用二甲基甲酰胺代替；二氯甲烷与乙醇或二甲基甲酰胺的体积比为8:1，聚乳酸纺丝液质量浓度为7％～10％。
步骤3粘合剂溶液质量浓度为1～3％，喷洒量为三维多孔非织造材料质量的6～10％；烘燥温度为40～55℃，烘燥时间为1～2h。
步骤3粘合剂包括水性聚氨酯、聚乙烯醇、磷酸酯变性淀粉中任意一种。
与现有技术相比，本发明具有以下有益效果：
(1)本发明的吸油材料是以中空率高、浮力好、吸油性能优异的木棉纤维和疏水亲油性好、可降解的聚乳酸为原料，利用木棉/聚乳酸纤维三维多孔针刺非织造材料与聚乳酸静电纺纳米微孔纤维膜复合，制得具有微纳梯度孔结构的非织造吸油材料，该材料的吸油量大，保油率高，亲油疏水性好，容易降解，可以多次重复使用。
(2)本发明的吸油材料采用针刺法制得三维多孔非织造材料，利用静电纺丝法得到纳米微孔纤维膜，应用化学粘合法将三维多孔非织造材料与纳米微孔纤维膜复合，制得微纳梯度孔结构的非织造吸油材料。该方法所用原料来源广泛，制备简单易行。
实验表明，本发明的吸油材料吸油量高达38.12g/g，保油率为96.01％，吸水率为3.45％，能重复使用五次以上。
附图说明
图1为本发明的易降解可重复使用高效非织造吸油材料的结构示意图。
图中，1.三维多孔非织造材料，2.静电纺纳米微孔纤维膜。
具体实施方式
下面结合附图和具体实施方式对本发明进行详细说明。下列实施例仅用于说明本发明，而不应视为限制本发明的范围。
本发明的易降解可重复使用高效非织造吸油材料，是由三维多孔非织造材料和静电纺纳米微孔纤维膜通过化学粘合法复合构成的具有微纳梯度孔结构的非织造布吸油材料，吸油材料的孔隙率为90.37％-93.32％，孔径为23-172μm；三维多孔非织造材料和静电纺纳米微孔纤维膜是疏水的。其中三维多孔非织造材料的孔隙率为88.14％-96.57％，孔径为42-320μm；静电纺纳米微孔纤维膜孔隙率为90.55％-91.25％，孔径为6-72μm。
如图1所示，本发明一种易降解可重复使用高效非织造吸油材料由三维多孔非织造材料(1)和静电纺纳米微孔纤维膜(2)复合组成。
实施例1
按照木棉/聚乳酸纤维混合比为30/70称取纤维100g，经过混合、开松、梳理、铺网、针刺加工制得木棉/聚乳酸纤维针刺非织造材料，克重为150g/m2，针刺密度为200刺/cm2，厚度为3.8mm。
称取0.83g的聚乳酸溶于9mL的二氯甲烷与无水乙醇共混溶剂中，二氯甲烷/无水乙醇体积比为8:1，配制成7wt％的聚乳酸纺丝液，室温下磁力搅拌24h，在纺丝电压为28kV，接收距离为16cm，环境湿度为60％RH条件下进行纺丝，制得聚乳酸静电纺纳米微孔纤维膜，微孔直径大于50nm，孔隙覆盖率为23.1％，克重为9.8～30g/m2，厚度为0.08～0.23mm。
采用空气喷枪在木棉/聚乳酸纤维针刺非织造材料上喷洒2％的水性聚氨酯溶液，喷洒量6％，将聚乳酸静电纺纳米微孔纤维膜覆盖在其上，烘燥1.5h，烘燥温度为40℃，得到微纳梯度孔结构复合非织造吸油材料，吸油量为25.85～37.28g/g，保油率为91.25～95.71％，吸水率为5.31～11.74％。
实施例2
按照木棉/聚乳酸纤维混合比为60/40称取纤维100g，经过混合、开松、梳理、铺网、针刺加工制得木棉/聚乳酸纤维针刺非织造材料，克重为100g/m2，针刺密度为240刺/cm2，厚度为3.5mm。
称取0.85g的聚乳酸溶于9mL的二氯甲烷与无水乙醇共混溶剂中，二氯甲烷/无水乙醇体积比为8:1，配制成8wt％的聚乳酸纺丝液，室温下磁力搅拌24h，在纺丝电压为30kV，接收距离为15cm，环境湿度为70％RH条件下进行纺丝，制得聚乳酸静电纺纳米微孔纤维膜，微孔直径大于50nm，孔隙覆盖率为24.9％，克重为10～30g/m2，厚度为0.09～0.25mm。
采用空气喷枪在木棉/聚乳酸纤维针刺非织造材料上喷洒1.0％的聚乙烯醇溶液，喷洒量10％，将聚乳酸静电纺纳米微孔纤维膜覆盖在其上，烘燥2.0h，烘燥温度为50℃，得到微纳梯度孔结构复合非织造吸油材料，吸油量为26.94～38.12g/g，保油率为91.82～96.01％，吸水率为8.36～11.26％。
实施例3
按照木棉/聚乳酸纤维混合比为40/60称取纤维100g，经过混合、开松、梳理、铺网、针刺加工制得木棉/聚乳酸纤维针刺非织造材料，克重为100g/m2，针刺密度为300刺/cm2，厚度为3.1mm。
称取0.87g的聚乳酸溶于9mL的二氯甲烷与无水乙醇共混溶剂中，二氯甲烷/无水乙醇体积比为8:1，配制成10wt％的聚乳酸纺丝液，室温下磁力搅拌24h，在纺丝电压为29kV，接收距离为17cm，环境湿度为65％RH条件下进行纺丝，制得聚乳酸静电纺纳米微孔纤维膜，微孔直径大于50nm，孔隙覆盖率为22.5％，克重为10.5～30g/m2，厚度为0.11～0.26mm。
采用空气喷枪在木棉/聚乳酸纤维针刺非织造材料上喷洒3％的磷酸酯变性淀粉溶液，喷洒量8.0％，将聚乳酸静电纺纳米微孔纤维膜覆盖在其上，烘燥1.0h，烘燥温度为55℃，得到微纳梯度孔结构复合非织造吸油材料，吸油量为24.58～36.21g/g，保油率为92.81～95.37％，吸水率为3.45～11.06％。
实施例4
按照木棉/聚乳酸纤维混合比为50/50称取纤维100g，经过混合、开松、梳理、铺网、针刺加工制得木棉/聚乳酸纤维针刺非织造材料，克重为180g/m2，针刺密度为180刺/cm2，厚度为3.8mm。
称取0.85g的聚乳酸溶于9mL的二氯甲烷与无水乙醇共混溶剂中，二氯甲烷/无水乙醇体积比为8:1，配制成8wt％的聚乳酸纺丝液，室温下磁力搅拌24h，在纺丝电压为30kV，接收距离为15cm，环境湿度为70％RH条件下进行纺丝，制得聚乳酸静电纺纳米微孔纤维膜，微孔直径大于50nm，孔隙覆盖率为24.9％，克重为10～30g/m2，厚度为0.09～0.25mm。
采用空气喷枪在木棉/聚乳酸纤维针刺非织造材料上喷洒2％的水性聚氨酯溶液，喷洒量7.6％，将聚乳酸静电纺纳米微孔纤维膜覆盖在其上，烘燥1.5h，烘燥温度为50℃，得到微纳梯度孔结构复合非织造吸油材料，吸油量为23.94～30.27g/g，保油率为91.40～95.21％，吸水率为6.51～12.38％。
实施例5
按照木棉/聚乳酸纤维混合比为60/40称取纤维100g，经过混合、开松、梳理、铺网、针刺加工制得木棉/聚乳酸纤维针刺非织造材料，克重为100g/m2，针刺密度为240刺/cm2，厚度为3.5mm。
称取0.85g的聚乳酸溶于9mL的二氯甲烷与二甲基甲酰胺共混溶剂中，二氯甲烷/二甲基甲酰胺体积比为8:1，配制成8wt％的聚乳酸纺丝液，室温下磁力搅拌24h，在纺丝电压为30kV，接收距离为15cm，环境湿度为70％RH条件下进行纺丝，制得聚乳酸静电纺纳米微孔纤维膜，微孔直径为2～10nm，孔隙覆盖率为0.9～10％，克重为10～30g/m2，厚度为0.09～0.25mm。
采用空气喷枪在木棉/聚乳酸纤维针刺非织造材料上喷洒2％的水性聚氨酯溶液，喷洒量7.6％，将聚乳酸静电纺纳米微孔纤维膜覆盖在其上，烘燥1.5h，烘燥温度为50℃，得到微纳梯度孔结构复合非织造吸油材料，吸油量为22.85～29.32g/g，保油率为90.76～95.08％，吸水率为7.43～12.66％。
聚乳酸静电纺纳米微孔纤维膜具有较高的孔隙率、较大的比表面积、优异的疏水亲油性，在油水混合液中，油液通过毛细管作用力进入纤维的间隙，并在纤维内孔隙的芯吸作用下进入聚乳酸纤维孔内，实现快速的油水分离和油液吸附。木棉/聚乳酸针刺非织造材料为三维多孔结构且木棉纤维中空率高，孔隙率高、孔径分布广泛、比表面积大，极利于油液的快速扩散和大量储存，实现油液吸附和储存。
本发明一种易降解可重复使用高效非织造吸油材料完全以天然纤维木棉和可降解聚乳酸纤维、聚乳酸聚合物为原料，利用材料本身的性能及结构特点及不同加工工艺赋予材料的结构特点，开发环保型、高性能、可重复使用非织造吸油材料。
以上是本发明的优选实施方式，实施例仅仅是本发明的一部分实施例，而不是全部的实施例，本发明的实施方式并不受上述实施例的限制，任何未背离本发明原理下所作的改变、修饰、替代、组合、简化，均应为等效的置换方式，都包含在本发明的保护范围之内。

Claims (1)

1.一种易降解可重复使用高效非织造吸油材料的制备方法，其特征在于，包括以下步骤：
步骤1：采用非织造加工法制得三维多孔非织造材料
以木棉纤维和聚乳酸纤维为原料，通过混合、开松、梳理、铺网、针刺加工得到针刺三维多孔非织造材料；
所述木棉和聚乳酸纤维混合比为30/70～60/40，所述三维多孔非织造材料克重为100～180g/m2、针刺密度为180～300刺/cm2；
步骤2：利用静电纺丝法得到纳米微孔纤维膜
将聚乳酸溶于二氯甲烷和乙醇中，得到聚乳酸纺丝液，然后进行静电纺丝，设置纺丝电压为28～30kV，接受距离为15~17cm，相对湿度为60~70%，制得聚乳酸静电纺纳米微孔纤维膜；
步骤2所述乙醇可以用二甲基甲酰胺代替；所述二氯甲烷与乙醇或二甲基甲酰胺的体积比为8:1，所述聚乳酸纺丝液质量浓度为7%～10%；
步骤3：应用化学粘合法将三维多孔非织造材料与纳米微孔纤维膜复合，制得微纳梯度孔结构的非织造吸油材料；所述吸油材料的孔隙率为90.37%-93.32%，孔径为23-172μm；
将粘合剂溶液喷洒在步骤1制备的三维多孔非织造材料上，再将静电纺纳米微孔纤维膜覆盖在上面，放入烘箱干燥，制得微纳梯度孔结构非织造吸油材料；
步骤3所述粘合剂溶液质量浓度为1～3%，喷洒量为三维多孔非织造材料质量的6~10%；烘燥温度为40~55℃，烘燥时间为1~2h；
所述粘合剂包括水性聚氨酯、聚乙烯醇、磷酸酯变性淀粉中任意一种。
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