CN116943621A - 一种皮芯结构复合吸附纳米纤维膜及其制备方法与应用 - Google Patents
一种皮芯结构复合吸附纳米纤维膜及其制备方法与应用 Download PDFInfo
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Abstract
本发明属于功能性纤维技术领域,公开了一种皮芯结构复合吸附纳米纤维膜及其制备方法与应用。该纳米纤维膜是由可天然降解的聚乳酸(PLA)和二醋酸纤维素(CDA)制备而成,其皮层是CDA,芯层是PLA,该纳米纤维膜可用于吸附污染物或有害物质。本发明制备的皮芯结构复合吸附纳米纤维膜具有多孔隙、高比表面积和优异的吸附功能,原料天然可降解,且在生产和使用过程不会产生对环境有害的物质,对环境优好,并且制造工艺简单。
Description
技术领域
本发明属于功能型纤维制备技术领域,特别是涉及一种皮芯结构复合吸附纳米纤维膜及其制备方法与应用。
背景技术
随着纳米技术的发展,越来越多的纳米纤维和纳米纤维膜被开发出来。由于纳米纤维膜拥有较高比表面积,可以吸附废水中的有机废弃物,使其在废水处理领域有良好的应用前景。同时,关注到不可再生资源的过度使用和不可降解材料对环境造成的污染问题,当下寻找可降解材料作为替代材料迫在眉睫。因此,选择完全可生物降解的高分子材料为原料,研究制备具有多孔隙,高比表面积,和良好吸附性能的环保型吸附材料具有重要意义。
聚乳酸(PLA)是一种来源于谷物等生物质材料的高分子材料,无毒,可完全生物降解,不会污染环境,良好的韧性。由PLA所制备的纳米纤维膜力学性能较好,但其吸附性能一般,无法满足吸附材料的使用要求。二醋酸纤维素(CDA)以天然纤维素资源为原料,来源广泛,对环境友好,表面有孔隙,吸附性能优异。然而,CDA纳米纤维膜力学性能价差,作为吸附材料使用受限。将CDA和PLA共混静电纺丝可制备吸附性能改善的纳米纤维膜,但较差的相容性使其力学性能更差。为了同时提高吸附性能和力学性能,将PLA和CDA同轴静电纺以制备PLA吸附纳米纤维膜。
目前吸附纤维的制备方法主要有活化工艺、静电纺丝等等。专利CN109097910A中将癸二酸和丙三醇在氮气下合成聚癸二酸甘油酯,与PLA一起通过同轴静电纺丝成纳米纤维膜,该膜具有较高的比表面积,在生物组织支架工程领域有良好的应用前景。专利CN106607014A中将聚乙二醇化胸腺嘧啶PEG-T修饰到第五代聚酰胺-胺树状大分子G5.NH2表面得到G5-PEG-T,之后将G5-PEG-T与聚乳酸羟基乙酸PLGA利用静电纺丝技术制备纳米纤维膜,该膜有良好的Hg2+吸附效果,但方法制备过程较为复杂,比表面积也较同轴静电纺的纳米纤维膜低。
发明内容
针对以上现有技术存在的缺点和不足之处,本发明提供一种皮芯结构复合吸附纳米纤维膜及其制备方法与应用,该方法制备的复合吸附纳米纤维膜具有易降解,多孔隙,高比表面积,力学性能好,有良好的吸附性能等特点,对环境友好,且工艺简单,成本较低,有利于实现工业化。
为达到上述目的,本发明提供了一种皮芯结构复合吸附纳米纤维膜,所述复合吸附纳米纤维膜的皮层材料为二醋酸纤维素,芯层材料为聚乳酸,所述复合吸附纳米纤维膜的厚度为32-45μm,单纤维直径为480-1320nm,外径为200-800nm,内径为280-520nm。
进一步的,所述复合吸附纳米纤维膜表层孔径为35-750nm,比表面积达到800-2200m2/g,拉伸强度达到0.95-1.57MPa。
本发明还提供了一种皮芯结构复合吸附纳米纤维膜的制备方法,包括如下步骤:
S1.将二醋酸纤维素溶解于丙酮溶液,搅拌均匀,为皮层溶液;
S2.将聚乳酸溶解于三氯甲烷和二甲基甲酰胺混合溶剂,搅拌均匀,为芯层溶液;
S3.将所述皮层溶液和所述芯层溶液以恒定的流速和流速比分别连接到同轴针头的外层和内层,同时将同轴针头连接高压静电发生器进行静电纺丝,干燥,得到复合吸附纳米纤维膜。
进一步的,上述制备方法中,所述皮层溶液中,二醋酸纤维素的质量浓度为6-9wt%。
进一步的,上述制备方法中,所述芯层溶液中,聚乳酸的质量浓度为6-9wt%。
进一步的,上述制备方法中,所述三氯甲烷和二甲基甲酰胺混合溶剂中,三氯甲烷和二甲基甲酰胺的质量比为9:1。
进一步的,上述制备方法中,所述静电纺丝参数为:纺丝电压20kv,纺丝距离20cm,纺丝速度0.8-1.6ml/h,转速65-80r/min。
进一步的,上述制备方法中,所述干燥为采用烘箱干燥,烘箱温度为60℃,时间为30-120min。
本发明还提供了上述的复合吸附纳米纤维膜或上述制备方法制备得到的复合吸附纳米纤维膜在废水处理吸附材料中的应用。
进一步的,所述废水处理吸附材料用于吸附废水中的染料、表面活性剂或重金属离子。
与现有技术相比,本发明克服了CDA与PLA直接共混相容性差的问题,利用同轴静电纺丝技术,采用CDA作为皮层,PLA作为芯层,制备表面具有多孔结构的皮芯结构复合吸附纳米纤维膜,使纤维膜既具有高孔隙率和高比表面积,又具有较好的力学性能,满足吸附材料的使用要求,该复合吸附纳米纤维膜对废水中的染料、表面活性剂以及重金属离子具有较好的吸附作用,使用废弃后可完全生物降解,不会造成二次污染。此外,本发明提供的制备方法工艺简单,无需复杂的改性加工过程,且对环境友好,可以产业化生产。
具体实施方式
下面将对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅是本发明的一部分实施例,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它实施例,都属于本发明保护的范围。
实施例1
(1)称取对应质量的PLA颗粒溶解于CHL/DMF混合溶剂中,配制成6wt%的纺丝液,再称取相对应质量的CDA溶解于CP溶剂中,配置成6wt%的纺丝液。
(2)将步骤(1)配置的纺丝液,皮层CDA溶液和芯层PLA溶液分别连接到同轴针头的外层和内层,同时将同轴针头连接高压静电发生器进行静电纺丝,在纺丝电压20kv,纺丝距离20cm,皮层纺丝速度1.6ml/h,芯层纺丝速度0.8ml/h,接收辊转速65r/min下静电纺成PLA/CDA同轴纳米纤维膜。
(3)将步骤(2)的PLA纳米纤维膜在60℃下烘120min。
所得PLA纳米纤维膜的厚度为32μm,纤维直径480-630nm,比表面积2200m2/g,拉伸强度0.95MPa。
实施例2
(1)称取对应质量的PLA颗粒溶解于CHL/DMF混合溶剂中,配制成7wt%的纺丝液,再称取相对应质量的CDA溶解于CP溶剂中,配置成7wt%的纺丝液。
(2)将步骤(1)配置的纺丝液,皮层CDA溶液和芯层PLA溶液分别连接到同轴针头的外层和内层,同时将同轴针头连接高压静电发生器进行静电纺丝,在纺丝电压20kv,纺丝距离20cm,皮层纺丝速度0.8ml/h,芯层纺丝速度1.6ml/h,接收辊转速80r/min下静电纺成PLA/CDA同轴纳米纤维膜。
(3)将步骤(2)的PLA纳米纤维膜在60℃下烘30min。
所得PLA纳米纤维膜的厚度为38μm,纤维直径680-830nm,比表面积达到800m2/g,拉伸强度1.47MPa。
实施例3
(1)称取对应质量的PLA颗粒溶解于CHL/DMF混合溶剂中,配制成8wt%的纺丝液,再称取相对应质量的CDA溶解于CP溶剂中,配置成8wt%的纺丝液。
(2)将步骤(1)配置的纺丝液,皮层CDA溶液和芯层PLA溶液分别连接到同轴针头的外层和内层,同时将同轴针头连接高压静电发生器进行静电纺丝,在纺丝电压20kv,纺丝距离20cm,皮层纺丝速度1ml/h,芯层纺丝速度1ml/h,接收辊转速65r/min下静电纺成PLA/CDA同轴纳米纤维膜。
(3)将步骤(2)的PLA纳米纤维膜在60℃下烘60min。
所得PLA纳米纤维膜的厚度为36μm,纤维直径690-880nm,比表面积达到1800m2/g,拉伸强度1.52MPa。
实施例4
(1)称取对应质量的PLA颗粒溶解于CHL/DMF混合溶剂中,配制成9wt%的纺丝液,再称取相对应质量的CDA溶解于CP溶剂中,配置成9wt%的纺丝液。
(2)将步骤(1)配置的纺丝液,皮层CDA溶液和芯层PLA溶液分别连接到同轴针头的外层和内层,同时将同轴针头连接高压静电发生器进行静电纺丝,在纺丝电压20kv,纺丝距离20cm,皮层纺丝速度1ml/h,芯层纺丝速度1ml/h,接收辊转速80r/min下静电纺成PLA/CDA同轴纳米纤维膜。
(3)将步骤(2)的PLA纳米纤维膜在60℃下烘60min。
所得PLA纳米纤维膜的厚度为45μm,纤维直径856-1500nm,比表面积达到1600m2/g,拉伸强度1.37MPa。
实施例5
(1)称取对应质量的PLA颗粒溶解于CHL/DMF混合溶剂中,配制成8wt%的纺丝液,再称取相对应质量的CDA溶解于CP溶剂中,配置成8wt%的纺丝液。
(2)将步骤(1)配置的纺丝液,皮层CDA溶液和芯层PLA溶液分别连接到同轴针头的外层和内层,同时将同轴针头连接高压静电发生器进行静电纺丝,在纺丝电压20kv,纺丝距离20cm,皮层纺丝速度1ml/h,芯层纺丝速度0.8ml/h,接收辊转速75r/min下静电纺成PLA/CDA同轴纳米纤维膜。
(3)将步骤(2)的PLA纳米纤维膜在60℃下烘60min。
所得PLA纳米纤维膜的厚度为40μm,纤维直径635-870nm,比表面积达到1540m2/g,拉伸强度1.46MPa。
实施例6
(1)称取对应质量的PLA颗粒溶解于CHL/DMF混合溶剂中,配制成8wt%的纺丝液,再称取相对应质量的CDA溶解于CP溶剂中,配置成8wt%的纺丝液。
(2)将步骤(1)配置的纺丝液,皮层CDA溶液和芯层PLA溶液分别连接到同轴针头的外层和内层,同时将同轴针头连接高压静电发生器进行静电纺丝,在纺丝电压20kv,纺丝距离20cm,皮层纺丝速度1.2ml/h,芯层纺丝速度1ml/h,接收辊转速70r/min下静电纺成PLA/CDA同轴纳米纤维膜。
(3)将步骤(2)的PLA纳米纤维膜在60℃下烘60min。
所得PLA纳米纤维膜的厚度为39μm,纤维直径600-865nm,比表面积达到1980m2/g,拉伸强度1.53MPa。
比较例1
称取CDA,在CP溶剂中配制成8wt%的纺丝溶液,在纺丝电压20kv,纺丝距离20cm,纺丝速度1ml/h,转速65r/min下静电纺成CDA纤维膜。所得CDA纳米纤维膜的厚度为40μm,纤维直径680-970nm,比表面积达到2150m2/g,拉伸强度0.76MPa。
比较例2
称取PLA/CDA对应质量比为1/1,在CHL/DMF溶液中配制成8wt%的纺丝溶液,在纺丝电压20kv,纺丝距离20cm,纺丝速度1ml/h,转速65r/min下静电纺成PLA纤维膜。所得PLA纳米纤维膜的厚度为43μm,纤维直径860-1370nm,比表面积达到540m2/g,拉伸强度0.6MPa。
比较例3
称取PLA,在CHL/DMF溶剂中配制成8wt%的纺丝溶液,在纺丝电压20kv,纺丝距离20cm,纺丝速度1ml/h,转速65r/min下静电纺成PLA纤维膜。所得PLA纳米纤维膜的厚度为41μm,纤维直径900-1300nm,比表面积达到270m2/g,拉伸强度1.58MPa。
比较例4
(1)称取对应质量的PLA颗粒溶解于CHL溶剂中,配制成8wt%的纺丝液,再称取相对应质量的CDA溶解于CP溶剂中,配置成8wt%的纺丝液。
(2)将步骤(1)配置的纺丝液,皮层CDA溶液和芯层PLA溶液分别连接到同轴针头的外层和内层,同时将同轴针头连接高压静电发生器进行静电纺丝,在纺丝电压20kv,纺丝距离20cm,皮层纺丝速度1ml/h,芯层纺丝速度1ml/h,接收辊转速70r/min下静电纺成PLA/CDA同轴纳米纤维膜。
(3)将步骤(2)的PLA纳米纤维膜在60℃下烘60min。
所得PLA纳米纤维膜的厚度为42μm,纤维直径920-1140nm,比表面积达到760m2/g,拉伸强度0.83MPa。
通过上述实施例与比较例对比,可以发现本发明所制备同轴静电纺PLA/CDA纳米纤维膜比表面积和力学性能大大提高,赋予了纤维膜作为吸附材料所必备的吸附性能和使用稳定性。此外,本方法工艺简单,具有产业化应用前景。
Claims (10)
1.一种皮芯结构复合吸附纳米纤维膜,其特征在于,所述复合吸附纳米纤维膜的皮层材料为二醋酸纤维素,芯层材料为聚乳酸,所述复合吸附纳米纤维膜的厚度为32-45μm,单纤维直径为480-1320nm,外径为200-800nm,内径为280-520nm。
2.根据权利要求1所述的皮芯结构复合吸附纳米纤维膜,其特征在于,所述复合吸附纳米纤维膜表层孔径为35-750nm,比表面积达到800-2200m2/g,拉伸强度达到0.95-1.57MPa。
3.一种皮芯结构复合吸附纳米纤维膜的制备方法,其特征在于,包括如下步骤:
S1.将二醋酸纤维素溶解于丙酮溶液,搅拌均匀,为皮层溶液;
S2.将聚乳酸溶解于三氯甲烷和二甲基甲酰胺混合溶剂,搅拌均匀,为芯层溶液;
S3.将所述皮层溶液和所述芯层溶液以恒定的流速和流速比分别连接到同轴针头的外层和内层,同时将同轴针头连接高压静电发生器进行静电纺丝成膜,干燥,得到复合吸附纳米纤维膜。
4.根据权利要求1所述的制备方法,其特征在于,所述皮层溶液中,二醋酸纤维素的质量浓度为6-9%。
5.根据权利要求1所述的制备方法,其特征在于,所述芯层溶液中,聚乳酸的质量浓度为6-9%。
6.根据权利要求1所述的制备方法,其特征在于,所述三氯甲烷和二甲基甲酰胺混合溶剂中,三氯甲烷和二甲基甲酰胺的质量比为9:1。
7.根据权利要求1所述的制备方法,其特征在于,所述静电纺丝参数为:纺丝电压20kv,纺丝距离20cm,纺丝速度0.8-1.6ml/h,转速65-80r/min。
8.根据权利要求1所述的制备方法,其特征在于,所述干燥采用烘箱干燥,烘箱温度为60℃,时间为30-120min。
9.权利要求1或2所述的复合吸附纳米纤维膜或权利要求3-8任一项制备方法制备得到的复合吸附纳米纤维膜在废水处理吸附材料中的应用。
10.根据权利要求9所述的应用,其特征在于,所述废水处理吸附材料用于吸附废水中的染料、表面活性剂或重金属离子。
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