CN108004677B - 一种过滤效率高的三维纳米纤维膜的制备方法 - Google Patents
一种过滤效率高的三维纳米纤维膜的制备方法 Download PDFInfo
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Abstract
一种过滤效率高的三维纳米纤维膜的制备方法，将聚甲基丙烯酸甲酯粉末溶解于有机溶剂中形成纺丝液；将纺丝液加入到储液罐中，并在接收电极板上附上一层无纺布，并控制所述接收电极板到发射极的距离为16～18cm；在发射极上施加32‑35kv的正电压，并在接收电极板施加负电压，负电压逐渐增大，并控制流速为1.6～1.8ml/h，温度为35～38℃、相对湿度为25％～35％，进行静电纺丝20～30分钟获得所述三维纳米纤维膜。该产品呈蓬松的立体纤维结构，有助于实现高效过滤。
Description
技术领域
本发明涉及新材料技术领域，且特别涉及一种过滤效率高的三维纳米纤维膜的制备方法。
背景技术
空气细颗粒物(PM2.5)是指空气动力学当量直径小于或等于2.5μm的颗粒物。细颗粒物粒径小，在大气中的停留时间长、输送距离远，且可含大量有毒、有害物质，对人体健康危害巨大。细颗粒物直径越小，进入呼吸道的部位越深，10μm直径的颗粒物通常沉积在上呼吸道，而2μm以下的细颗粒物则可深入到细支气管和肺泡。进入肺泡后的细颗粒物将直接影响肺的通气功能。因此，生产PM2.5过滤膜具有重要意义。
传统过滤材料由纳米纤维膜组成，纳米纤维膜一般都是平面结构，只能对小范围粒径(如粒径为2.5μm左右的颗粒)的PM2.5进行过滤，难以对大范围粒径，如粒径为0.1μm～10μm的PM2.5都进行有效过滤进行过滤。
静电纺丝是一种特殊的纤维制造工艺，聚合物溶液或熔体在强电场中进行喷射纺丝。在电场作用下，针头处的液滴会由球形变为圆锥形(即“泰勒锥”)，并从圆锥尖端延展得到纤维细丝。这种方式可以生产出纳米级直径的聚合物细丝。
发明内容
本发明的目的在于提供一种过滤效率高的三维纳米纤维膜的制备方法，此制备方法简单，易于操作，能够构建立体多层次纳米纤维膜结构，有效提高对PM2.5的过滤性能。
本发明解决其技术问题是采用以下技术方案来实现的。
本发明提出一种过滤效率高的三维纳米纤维膜的制备方法，包括以下步骤：
S1，将聚甲基丙烯酸甲酯粉末溶解于易挥发的有机溶剂中形成纺丝液，其中，所述聚甲基丙烯酸甲酯的质量分数为17％～19％；
S2，将所述纺丝液加入到储液罐中，并在接收电极板上附上一层无纺布，并控制所述接收电极板到发射极的距离为16～18cm；
S3，在所述发射极上施加32-35kv的正电压，并在所述接收电极板施加负电压，所述负电压逐渐增大，并控制流速为1.6～1.8ml/h，温度为35～38℃、相对湿度为25％～35％，进行静电纺丝20～30分钟获得所述三维纳米纤维膜。
本发明实施例的过滤效率高的三维纳米纤维膜的制备方法有益效果是：
由于射流将携带走聚集于发射电极处的自由电荷，电荷随着射流朝接收电极板迁移，并将在接收电极板上累积。由于纳米纤维膜与接收电极板导电率的限制，纳米纤维膜表面将产生残余电荷积累。纺丝射流上携带有自由电荷。接收电极板上的残余电荷会对带电射流产生一个电荷排斥作用，从而驱使纺丝射流发生偏移，出现螺旋弯曲等不稳定现象，改变了运动轨迹。本发明通过在接收电极板上施加负电压，并调控接收电极板到发射极距离、流速、温度、相对湿度等相关参数的大小，从而使得接收电极板对带电射流产生适中的排斥力，既可避免后续纤维被排斥而无法累加沉积，又可保持相对适中的排斥力避免了团聚，从而有利于获得蓬松的三维纳米纤维膜结构。且本发明根据接收电极板上残余电荷的积累过程，施加逐渐变大的负电压，有效调控排斥力的大小，更好获得能够形成多层次膜结构的立体纤维膜，有助于实现高效过滤。
具体实施方式
为使本发明实施例的目的、技术方案和优点更加清楚，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。实施例中未注明具体条件者，按照常规条件或制造商建议的条件进行。所用试剂或仪器未注明生产厂商者，均为可以通过市售购买获得的常规产品。
下面对本发明实施例的一种过滤效率高的三维纳米纤维膜进行具体说明。
本发明实施例提供的一种过滤效率高的三维纳米纤维膜的制备方法，包括以下步骤：
S1，将聚甲基丙烯酸甲酯粉末溶解于易挥发的有机溶剂中形成纺丝液，其中，所述聚甲基丙烯酸甲酯的质量分数为17％～19％；
S2，将所述纺丝液加入到储液罐中，并在接收电极板上附上一层无纺布，并控制所述接收电极板到发射极的距离为16～18cm；
S3，在所述发射极上施加32-35kv的正电压，并在所述接收电极板施加负电压，所述负电压逐渐增大，并控制流速为1.6～1.8ml/h，温度为35～38℃、相对湿度为25％～35％，进行静电纺丝20～30分钟获得所述三维纳米纤维膜。
进一步地，在本发明较佳的实施例中，所述易挥发的有机溶剂选自四氯化碳、苯、甲苯二氯乙烷、三氯甲烷、冰醋酸、乙酸乙酯、醋酸乙烯酯中的一种或多种。进一步优选地，有机溶剂选自冰醋酸、乙酸乙酯或醋酸乙烯酯，更为安全环保。
进一步地，步骤S3中，正电压为34kV。电压的选择是纳米纤维成型控制的主要参数，采用34kV的正电压时，能够使得纺丝射流喷射的速度适宜，纤维落于收集板上的速度达到104m/s左右，纳米纤维的直径小于100nm。
进一步地，步骤S3中，负电压的取值范围为-20V～-50V，负电压的变化速率为1～1.5V/min。例如初始负电压为-22V，以1V/min速率逐渐变大，纺丝10min后，负电压达到-32V。在接收电极板上施加动态的负电压，与接收电极板上的残余电荷的积累程度相适应，使得对带电射流的排斥力始终维持在较为恒定的范围，更有利于形成形态规整的三维纳米线纤维膜，进一步提高过滤性能。
进一步地，步骤S3，流速为1.7ml/h，温度为36℃、相对湿度为30％。在适宜的流速下，温度较高，相对湿度较低，能够使得聚合物纺丝的有机溶剂迅速挥发。
进一步地，在本发明较佳的实施例中，在步骤S1中，所述纺丝液中还加入改性成分，所述改性成分包括质量比为1:0.2～0.5的壳聚糖季铵盐和单宁酸的混合物。
进一步地，壳聚糖季铵盐为季铵根取代度为40％～80％的环氧丙基三甲基氯化铵壳聚糖季铵盐或季铵根取代度为40％～80％的N,N,N-三甲基壳聚糖季铵盐。
进一步地，在本发明较佳的实施例中，所述改性成分按以下步骤制备：将单宁酸溶解在水中，配置成0.5～1g/L的单宁酸水溶液中，然后将一定质量的壳聚糖季铵盐加入到所述单宁酸水溶液中，升温至40～50℃，搅拌反应3～5min后，过滤、洗涤、冷冻干燥得到所述改性成分。该条件下，单宁酸和壳聚糖季铵盐能够形成良好的交联作用。
进一步地，在本发明较佳的实施例中，步骤S1中，先将所述改性成分分散于所述有机溶剂中，再加入所述聚甲基丙烯酸甲酯粉末，微波反应2min后，超声处理20～30min得到所述纺丝液。先进行微波反应再超声分散，能够使得改性成分对聚甲基丙烯酸甲酯形成良好的包覆效果，得到核壳结构的纺丝液。
进一步的，改性成分和聚甲基丙烯酸甲酯粉末的质量比为2～8:100。
壳聚糖是一种结构多糖，是地球上可利用的巨大自然资源，壳聚糖的年产量巨大，仅次于纤维素。壳聚糖季铵盐的水溶性好，且具有非常明显的杀菌作用，能够与纤维素通过氢键结合，使得聚合物纤维能够与无纺布形成良好的结合。此外，壳聚糖分子能够和单宁酸发生交联反应，在壳聚糖分子中引入了单宁酸的多酚羟基和羧基，改善壳聚糖的溶解性能和吸附性能，得到两性高分子改性液。在纺丝液中加入改性成分，能够进一步增强纳米纤维对于PM2.5的过滤效果，特别是能够增强对铬、铜等重金属离子的吸附螯合作用。
进一步地，在本发明较佳的实施例中，步骤S4之后，还进行以下步骤：
S5，保持静电纺丝结束后的负电压不变，用热风刀对所述三维纳米纤维膜进行干燥处理5～7min，热风刀产生的热气流的流向大致平行于所述接收电极板。
进一步地，在本发明较佳的实施例中，所述热气流的流速为50～80m/s，温度为90～100℃。
在纺丝完成后，用高温热气流对三维纳米纤维膜进行处理，进一步干燥聚合物纤维中的溶剂。由于热气流平行于接收电极板，即平行于纳米纤维的层叠方向，在热气流的作用下，能够使得纳米纤维膜进一步蓬松，形成孔隙更多的立体结构。
进一步地，在本发明较佳的实施例中，步骤S2中，所述无纺布在使用前，对所述无纺布进行预处理：将所述无纺布在阳离子溶液中浸渍0.5～1h，干燥。
进一步地，在本发明较佳的实施例中，所述阳离子溶液为质量分数为0.5～2％的十四烷基甲基二羟乙基溴化铵水溶液。
对无纺布进行预处理，使得无纺布的表面附着一定的阳离子，能够在纺丝的初始阶段，对于带电射流产生排斥力，避免纳米纤维过于致密，从而影响产品的蓬松程度。
本发明还提供一种过滤效率高的三维纳米纤维膜，其根据上述的制备方法制备得到。
以下结合实施例对本发明的特征和性能作进一步的详细描述。
实施例1
本实施例提供的一种过滤效率高的三维纳米纤维膜，其根据以下步骤制得：
(1)将聚甲基丙烯酸甲酯粉末溶解于冰醋酸中形成纺丝液，其中，聚甲基丙烯酸甲酯的质量分数为18％。
(2)将纺丝液加入到储液罐中，并在接收电极板上附上一层无纺布，并控制接收电极板到发射极的距离为17cm。
(3)在发射极上施加34kV的正电压，并在接收电极板施加第-20V的负电压，负电压以1V/min的速率逐渐增大，并控制流速为1.7ml/h，温度为36℃、相对湿度为30％，进行静电纺丝22min获得。
制得的三维纳米纤维膜的直径分布为20～90nm，对0.03～10μm颗粒物的过滤效率为99.6％，阻力压降为41Pa。
实施例2
本实施例提供的一种过滤效率高的三维纳米纤维膜，其根据以下步骤制得：
(1)将聚甲基丙烯酸甲酯粉末溶解于冰醋酸中形成纺丝液，其中，聚甲基丙烯酸甲酯的质量分数为18％。
(2)将纺丝液加入到储液罐中，并在接收电极板上附上一层无纺布，并控制接收电极板到发射极的距离为17cm。
(3)在发射极上施加34kV的正电压，并在接收电极板施加第-20V的负电压，负电压以1V/min的速率逐渐增大，并控制流速为1.7ml/h，温度为36℃、相对湿度为30％，进行静电纺丝22min。
(5)保持纺丝结束后的负电压不变，用热风刀对三维纳米纤维膜处理6min，热风刀产生的热气流的流向大致平行于接收电极板，热气流的温度为90℃，流速为70m/s。
制得的三维纳米纤维膜的直径分布为20～90nm，对0.03～10μm颗粒物的过滤效率为99.8％，阻力压降为19Pa。
实施例3
本实施例提供的一种过滤效率高的三维纳米纤维膜，其根据以下步骤制得：
(1)改性成分的配置：将壳聚糖季铵盐加入到1g/L的单宁酸水溶液中，升温至45℃，搅拌反应4min后，过滤、洗涤、冷冻干燥，其中壳聚糖季铵盐与单宁酸的质量比为1:0.4。
(2)将0.9％的改性成分分散于冰醋酸中，加入聚甲基丙烯酸甲酯粉末，微波2min后，超声处理25min，形成纺丝液，其中，聚甲基丙烯酸甲酯的质量分数为18％。
(3)将纺丝液加入到储液罐中，并在接收电极板上附上一层无纺布，并控制接收电极板到发射极的距离为17cm，其中该无纺布预先在质量分数为0.8％的十四烷基甲基二羟乙基溴化铵水溶液中处理1h。
(4)在发射极上施加34kV的正电压，并在接收电极板施加第-20V的负电压，负电压以1V/min的速率逐渐增大，并控制流速为1.7ml/h，温度为36℃、相对湿度为30％，进行静电纺丝22min。
(5)保持纺丝结束后的静电压不变，用热风刀对三维纳米纤维膜处理6min，热风刀产生的热气流的流向大致平行于接收电极板，热气流的温度为90℃，流速为70m/s。
制得的三维纳米纤维膜的直径分布为5～40nm，对0.03～10μm颗粒物的过滤效率为99.9％，阻力压降为16Pa。
对比例1
本实施例提供的一种过滤效率高的三维纳米纤维膜，其根据以下步骤制得：
(1)将聚甲基丙烯酸甲酯粉末溶解于冰醋酸中形成纺丝液，其中，聚甲基丙烯酸甲酯的质量分数为18％。
(2)将纺丝液加入到储液罐中，并在接收电极板上附上一层无纺布，并控制接收电极板到发射极的距离为17cm。
(3)在发射极上施加34kV的正电压，并控制流速为1.7ml/h，温度为36℃、相对湿度为30％，进行静电纺丝22min。
制得的纳米纤维膜的直径分布为180～300nm，对0.03～10μm颗粒物的过滤效率为89.7％，阻力压降为270Pa。
以上所描述的实施例是本发明一部分实施例，而不是全部的实施例。本发明的实施例的详细描述并非旨在限制要求保护的本发明的范围，而是仅仅表示本发明的选定实施例。基于本发明中的实施例，本领域普通技术人员在没有作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。
Claims (9)
1.一种三维纳米纤维膜的制备方法，其特征在于，包括以下步骤：
S1，将聚甲基丙烯酸甲酯粉末溶解于易挥发的有机溶剂中形成纺丝液，其中，所述聚甲基丙烯酸甲酯的质量分数为17％～19％；
S2，将所述纺丝液加入到储液罐中，并在接收电极板上附上一层无纺布，并控制所述接收电极板到发射极的距离为16～18cm；
S3，在所述发射极上施加32-35kv的正电压，并在所述接收电极板施加负电压，所述负电压逐渐增大，并控制流速为1.6～1.8ml/h，温度为35～38℃、相对湿度为25％～35％，进行静电纺丝20～30分钟获得所述三维纳米纤维膜；所述负电压的取值范围为-20V～-50V，所述负电压的变化速率为1～1.5V/min。
2.根据权利要求1所述的制备方法，其特征在于，所述易挥发的有机溶剂选自四氯化碳、苯、甲苯二氯乙烷、三氯甲烷、冰醋酸、乙酸乙酯、醋酸乙烯酯中的一种或多种。
3.根据权利要求1所述的制备方法，其特征在于，在步骤S1中，所述纺丝液中还加入改性成分，所述改性成分包括质量比为1:0.2～0.5的壳聚糖季铵盐和单宁酸的混合物。
4.根据权利要求3所述的制备方法，其特征在于，所述改性成分按以下步骤制备：将单宁酸溶解在水中，配置成0.5～1g/L的单宁酸水溶液中，然后将一定质量的壳聚糖季铵盐加入到所述单宁酸水溶液中，升温至40～50℃，搅拌反应3～5min后，过滤、洗涤、冷冻干燥得到所述改性成分。
5.根据权利要求4所述的制备方法，其特征在于，步骤S1中，先将所述改性成分分散于所述有机溶剂中，再加入所述聚甲基丙烯酸甲酯粉末，微波反应2min后，超声处理20～30min得到所述纺丝液。
6.根据权利要求1所述的制备方法，其特征在于，步骤S4之后，还进行以下步骤：
S5，保持静电纺丝结束后的负电压不变，用热风刀对所述三维纳米纤维膜进行干燥处理5～7min，热风刀产生的热气流的流向大致平行于所述接收电极板。
7.根据权利要求6所述的制备方法，其特征在于，所述热气流的流速为50～80m/s。
8.根据权利要求1所述的制备方法，其特征在于，步骤S2中，所述无纺布在使用前，对所述无纺布进行预处理：将所述无纺布在阳离子溶液中浸渍0.5～1h，干燥。
9.根据权利要求8所述的制备方法，其特征在于，所述阳离子溶液为质量分数为0.5～2％的十四烷基甲基二羟乙基溴化铵水溶液。
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| CN101144196A (zh) * | 2007-09-20 | 2008-03-19 | 东华大学 | 一种规则化静电纺中空纤维的制备方法 |
| CN101413183A (zh) * | 2007-10-16 | 2009-04-22 | 国家纳米科学中心 | 一种高分子静电纺丝薄膜及制法和在生物检测中的应用 |
| US8518320B2 (en) * | 2009-05-21 | 2013-08-27 | University Of Cincinnati | Methods for electrospinning hydrophobic coaxial fibers into superhydrophobic and oleophobic coaxial fiber mats |
| CN101671853A (zh) * | 2009-09-29 | 2010-03-17 | 吉林大学 | 添加电场屏蔽装置的多喷头高压静电纺丝设备 |
| CN102586901A (zh) * | 2012-01-11 | 2012-07-18 | 东华大学 | 一种三维静电纺非织造支架材料的制备方法及其装置 |
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