CN107326659B - 基于聚乙烯醇纳米纤维的非织造吸声材料及制备方法 - Google Patents
基于聚乙烯醇纳米纤维的非织造吸声材料及制备方法 Download PDFInfo
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Abstract
本发明涉及一种基于聚乙烯醇纳米纤维的非织造吸声材料的制备方法,包括以下步骤:对聚乙烯醇纳米纤维进行抗水溶性处理,得到抗水溶聚乙烯醇纳米纤维;将抗水溶聚乙烯醇纳米纤维浸入含第一催化剂的水溶液中,将经催化剂处理的纳米纤维转移至含有吡咯的体系中,通过气相沉淀法使所述吡咯在纳米纤维表面发生聚合反应,得到基于聚乙烯醇纳米纤维的非织造吸声材料。本发明还提供了一种采用上述方法所制备的基于聚乙烯醇纳米纤维的非织造吸声材料。本发明的方法所制备的吸声材料具有宽吸声频带和高吸声性能。
Description
技术领域
本发明涉及高聚物功能材料技术领域,尤其涉及一种基于聚乙烯醇纳米纤维的非织造吸声材料及制备方法。
背景技术
随着社会工业化的发展,噪声污染成为了现代化生活中的一个重大的污染源,在降低人们工作效率的同时,对人们的身心健康也有很多不好的影响,导致各种心血管疾病,与空气污染、水质污染和固体废料污染并列称为当代四大污染源。目前,人们主要通过两个途径进行噪音控制:一是从噪声源入手,减少噪声的发生;二是从噪声的传播途径上入手,使噪声在传播过程中减弱。在第二条途径中,吸声防噪材料的开发和应用是主要的研究内容。
近年来,人们在非织造吸声材料方面的研究主要集中在非织造复合材料方面,并通过改变材料、成网方法和固网方法等来探究影响非织造材料吸声性能的因素。非织造吸声材料纤网内纤维随机杂乱排列,使其纤网内部具有很多孔隙,具有良好的吸声性能。非织造材料由于其具有丰富的孔隙、原料来源广、价格低廉、易于制作生产而成为具有很好前景的多孔吸声材料。
高频声波可使非织造材料内空隙间空气质点的振动速度加快,空气与孔壁的热交换也加快,因此现有多孔非织造吸声材料已经能成功吸收大部分高频处的吸声性能。而现有吸声材料在低频处的吸声性能并不佳。因此,开发宽频吸声带或改善中低频吸声性能的吸声材料是今后发展的趋势。
发明内容
为解决上述技术问题,本发明的目的是提供一种基于聚乙烯醇纳米纤维的非织造吸声材料及制备方法。
本发明提供了一种基于聚乙烯醇纳米纤维的非织造吸声材料的制备方法,包括以下步骤:
(1)对聚乙烯醇纳米纤维进行抗水溶性处理,处理时间为10-120min,得到抗水溶聚乙烯醇纳米纤维;
(2)将抗水溶聚乙烯醇纳米纤维浸入含第一催化剂的水溶液中处理1-10h,取出处理后的纳米纤维,干燥后将经催化剂处理的纳米纤维转移至含有吡咯的密闭环境中,通过气相沉淀法使吡咯在纳米纤维表面发生聚合反应,反应时间为0.5-10h,得到基于聚乙烯醇纳米纤维的非织造吸声材料。
进一步地,在步骤(1)中,抗水溶性处理包括以下步骤:
将戊二醛、第二催化剂、水和有机溶剂混匀,然后将聚乙烯醇纳米纤维在其中浸泡10-120min。
进一步地,第二催化剂为盐酸、硫酸和硝酸中的一种或几种。
进一步地,有机溶剂为丙酮、乙腈和乙醚中的一种或几种。
进一步地,在步骤(1)中,通过静电纺丝方法得到聚乙烯醇纳米纤维。采用螺旋片式静电纺丝机进行静电纺丝。
步骤(1)中,纤维经抗水溶性处理后,其直径会发生改变,纤维直径的改变会改变纤维的振动方式和振动频率,纤维振动和声波振动之间的弛豫作用发生改变,从而导致材料吸声性能的改变。当纤维直径增大时,纤维的振动频率降低,从而使复合材料的吸声性能向中低频处移动。随着处理时间的增加,PVA纤维毡内纤维直径因溶胀作用而逐渐增大,孔径相对变小。这使得复合材料的吸声性能发生了变化,尤其是在中低频处,大体在声波频率为500Hz-2500Hz处有所提高。并且当处理时间为1h时,复合材料的吸声性能提高的声波频率的范围最大。但当处理时间超过1h达到2h时,吸声系数下降,在声波频率为1250Hz-2500Hz的范围内更加明显。将吸声系数提高的频率范围和吸声系数的大小综合考虑,可得最优的平均孔径和纤维直径分别为0.44μm和0.45μm,最佳处理时间为1h。
进一步地,在步骤(2)中,第一催化剂为氯化铁(FeCl3)、双氧水(H2O2)、过硫酸铵((NH4)2S2O8)和碘化钾(KIO3)中的一种或几种。第一催化剂的作用是化学氧化。
进一步地,在步骤(2)中,水溶液中第一催化剂的质量百分比为5wt.%-20wt.%。随着催化剂浓度的增加,纤维毡表面形成更多的不规则结构。
进一步地,在步骤(2)中,气相沉淀法在避光的密闭条件下进行。采用气相沉淀法对PVA纤维毡进行聚吡咯处理时,聚吡咯形成不规则结构,通过改变催化剂的量,可以改变纤维表面聚吡咯的量,从而改变材料的吸声性能。
本发明还公开了一种采用上述方法所制备的基于聚乙烯醇纳米纤维的非织造吸声材料。
借由上述方案,本发明至少具有以下优点:
(1)本发明通过静电纺方法制备纳米纤维非织造吸声材料,拓宽了材料的吸声频带;
(2)对纤维进行抗水溶性处理,该方法操作简单,且不会对纤维形态造成破坏;
(3)利用聚吡咯对纤维表面进行改性,使得纤维的吸声性能在中低频处有所提高;
(4)本发明的基于聚乙烯醇纳米纤维的非织造吸声材料具有广泛的应用领域,可用于建筑墙体、运输车辆、轮船等内饰吸声材料,给人们营造安静舒适的环境。
上述说明仅是本发明技术方案的概述,为了能够更清楚了解本发明的技术手段,并可依照说明书的内容予以实施,以下以本发明的较佳实施例并配合附图详细说明如后。
附图说明
图1是抗水溶性处理不同时间后PVA纤维毡的SEM图;
图2是抗水溶性处理时间对纤维直径、材料平均孔径和平均吸声系数的影响结果;
图3是不同浓度FeCl3溶液处理的纤维毡表面的SEM图谱;
图4是不同浓度FeCl3溶液对复合材料吸声性能的影响结果;
图5是不同浓度FeCl3溶液对复合材料吸声性能的影响结果。
具体实施方式
下面结合附图和实施例,对本发明的具体实施方式作进一步详细描述。以下实施例用于说明本发明,但不用来限制本发明的范围。
本发明以下实施例中,所使用的PVA纤维毡是采用螺旋片式静电纺丝机对PVA进行静电纺丝得到,其中,螺旋片式静电纺丝机由螺旋片式发生器,移动接收屏和高压电源组成。螺旋片发生器匀速旋转,提供离心力,源源不断地为静电纺丝过程提供纺丝液。与传统针头式静电纺丝相比,在螺旋片式静电纺丝过程中,泰勒锥在螺旋叶片上形成,而不是在针头上形成。移动接收屏上放有基布,在高压电源形成的电场的作用下,随机纤维射流喷射到基布上,射流溶剂挥发,形成纤网。
实施例1
将戊二醛(50%水溶液)与丙酮以质量比1:9混合在玻璃容器中,滴入0.5ml盐酸(HCl)作为催化剂。将PVA纤维毡放置到混合溶液中,分别放置0min,10min,30min,1h,2h,再在通风橱中风干至恒重,得到抗水溶PVA纤维毡。当抗水溶性处理的时间超过10min时,纤维毡的重量保留率在99%以上,因此当抗水溶性处理时间超过10min时,纤维毡具有较好的抗水溶性能,可用来做进一步的实验探究。在抗水溶性处理过程中,戊二醛的作用为交联剂,使PVA大分子链产生交联,从而使其不溶于水,具有抗水溶性能。
图1是处理不同时间后,PVA纤维毡的SEM图,图1a、b、c、d、e分别对应处理0min,10min,30min,1h,2h的结果,从图中可以看出,经过戊二醛抗水溶性处理后,纤维形貌并没有发生太大的改变。这说明戊二醛浸渍法对PVA纤维毡进行抗水溶性处理不会对纤维形态造成破坏。
图2是随着抗水溶性处理时间的变化,纤维直径、材料平均孔径和平均吸声系数(500Hz-3000Hz)结果。从图中可以看出,随着抗水溶性处理时间增加,PVA纤维毡中的纤维直径逐渐增大而纤维毡的平均孔径逐渐减小。当抗水溶性处理时间从0min增加到2h时,纤维直径从0.25μm增加到0.59μm,纤维毡平均孔径从0.54μm减小到0.39μm。当处理时间为1h时,纤维直径和孔径数值几乎相等。这种变化可能是由于纤维在抗水溶性处理的浸渍过程中发生溶胀现象造成的。
实施例2
将FeCl3粉末溶于蒸馏水中,配制质量分数分别为0wt.%,5wt.%,8wt.%,11wt.%,14wt.%,17wt.%,20wt.%的FeCl3溶液。按照实施例4的方法制得多块抗水溶性处理30min后的抗水溶PVA纤维毡,分别放置在不同浓度的FeCl3溶液中,放置4h。拿出处理后的抗水溶PVA纤维毡,自然风干,放入密闭容器中。在密闭容器中滴入适量的吡咯单体溶液,盖上盖子,放置在避光的地方,放置时间为2h。密闭容器中的吡咯单体溶液挥发,在抗水溶PVA纤维毡表面发生聚合反应,形成不规则的聚吡咯结构,得到基于聚乙烯醇纳米纤维的非织造吸声材料。在这个过程中,抗水溶PVA纤维毡内的FeCl3作为催化剂,催化吡咯的聚合反应。
分别将处理后的基于聚乙烯醇纳米纤维的非织造吸声材料取样(样品为圆形,直径为3mm,厚度为2mm)称重,每种样品取十个,重量取平均值。结果见表1,从表1可看出,FeCl3浓度增加时,处理后样品的质量增大,当FeCl3浓度达到20wt.%时,纤维毡中聚吡咯的聚合量可以达到1.38g。说明FeCl3浓度增加,经相同时间的气相沉淀法处理,纤维毡表面会聚集更多的聚吡咯。
表1 不同浓度的FeCl3处理后的样品平均重量
图3为经过不同浓度FeCl3溶液处理的纤维毡表面的SEM图谱。图3a、b、c、d、e、f分别对应FeCl3溶液浓度为5wt.%,8wt.%,11wt.%,14wt.%,17wt.%,20wt.%时的结果,从图3可看出,随着FeCl3浓度的增加,纤维毡表面有更多的不规则结构。当FeCl3浓度为5wt.%时,如图3a,纤维毡表面没有明显的聚吡咯聚集现象;但随着FeCl3浓度增加,纤维表面的聚集增加。这是由于当纤维毡浸渍在不同浓度的FeCl3溶液中时,PVA纤维毡中所含FeCl3的量不同,FeCl3浓度越高,纤维毡充所含FeCl3的量越多,因此,吡咯在纤维毡表面的聚集速度越快,相同时间内聚集的量越多,导致了更加不规则的结构。
选取以上制备的厚度均为2mm的基于聚乙烯醇纳米纤维的非织造吸声材料与涤纶针刺非织造材料进行复合,涤纶针刺非织造材料的厚度为8mm,得到复合材料。对复合材料的吸声性能进行测试,结果如图4-5所示,图中,a、b、c、d、e、f、g曲线分别代表FeCl3溶液浓度为5wt.%,8wt.%,11wt.%,14wt.%,17wt.%,20wt.%时的结果,当FeCl3浓度为5wt.%,8wt.%和11wt.%时(如图4),吸声系数在声波频率大于2250Hz处有所提高,在中低频处的吸声性能却没有改善,甚至在声波频率为1600Hz-2250Hz时还有所降低。当FeCl3浓度升高到14wt.%时(如图5),吸声曲线朝低频处移动,且随着FeCl3浓度的提高,在声波频率为500Hz-1250Hz时复合材料的吸声性能越好。当FeCl3浓度为20wt.%时,吸声系数的曲线分别在2000Hz和800Hz处达到了峰值,分别为0.89和0.92。这是主要由于当处理过程中FeCl3的浓度升高时,PVA纤维毡中聚吡咯的聚合量增多(表1)。当聚吡咯的量增加时,由图3可知,纤维表面有更多的不规则结构,使材料内的比表面积增加,声波与材料间的摩擦机会增多,导致通过粘滞性内摩擦消耗的声能增多,从而吸声系数更高。此外,聚吡咯聚合量的增加也导致了纤维变粗,纤维毡孔径变小,这对复合材料在中低频处的吸声性能的提高也有一定的积极作用。
实施例3
将戊二醛(50%水溶液)与乙腈以质量比1:9混合在玻璃容器中,滴入0.5ml硫酸作为催化剂。将PVA纤维毡放置到混合溶液中,放置30min,再在通风橱中风干至恒重,得到抗水溶PVA纤维毡。
将双氧水(H2O2)与蒸馏水混合,配制质量分数为5wt.%的H2O2溶液。将上述抗水溶PVA纤维毡放入H2O2溶液中放置10h。拿出处理后的抗水溶PVA纤维毡,自然风干,放入密闭容器中。在密闭容器中滴入适量的吡咯单体溶液,盖上盖子,放置在避光的地方,放置时间为10h。密闭容器中的吡咯单体溶液挥发,在抗水溶PVA纤维毡表面发生聚合反应,形成不规则的聚吡咯结构,得到基于聚乙烯醇纳米纤维的非织造吸声材料。
实施例4
将戊二醛(50%水溶液)与乙醚以质量比1:9混合在玻璃容器中,滴入0.5ml硝酸作为催化剂。将PVA纤维毡放置到混合溶液中,放置100min,再在通风橱中风干至恒重,得到抗水溶PVA纤维毡。
将过硫酸铵((NH4)2S2O8)溶于蒸馏水,配制质量分数为20wt.%的(NH4)2S2O8溶液。将上述抗水溶PVA纤维毡放入(NH4)2S2O8溶液中放置1h。拿出处理后的抗水溶PVA纤维毡,自然风干,放入密闭容器中。在密闭容器中滴入适量的吡咯单体溶液,盖上盖子,放置在避光的地方,放置时间为0.5h。密闭容器中的吡咯单体溶液挥发,在抗水溶PVA纤维毡表面发生聚合反应,形成不规则的聚吡咯结构,得到基于聚乙烯醇纳米纤维的非织造吸声材料。
实施例5
将戊二醛(50%水溶液)与丙酮以质量比1:9混合在玻璃容器中,滴入0.5ml盐酸作为催化剂。将PVA纤维毡放置到混合溶液中,放置1h,再在通风橱中风干至恒重,得到抗水溶PVA纤维毡。
将碘化钾(KIO3)溶于蒸馏水,配制质量分数为10wt.%的KIO3溶液。将上述抗水溶PVA纤维毡放入KIO3溶液中放置6h。拿出处理后的抗水溶PVA纤维毡,自然风干,放入密闭容器中。在密闭容器中滴入适量的吡咯单体溶液,盖上盖子,放置在避光的地方,放置时间为5h。密闭容器中的吡咯单体溶液挥发,在抗水溶PVA纤维毡表面发生聚合反应,形成不规则的聚吡咯结构,得到基于聚乙烯醇纳米纤维的非织造吸声材料。
以上所述仅是本发明的优选实施方式,并不用于限制本发明,应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明技术原理的前提下,还可以做出若干改进和变型,这些改进和变型也应视为本发明的保护范围。
Claims (5)
1.一种基于聚乙烯醇纳米纤维的非织造吸声材料的制备方法,其特征在于,包括以下步骤:
(1)对聚乙烯醇纳米纤维进行抗水溶性处理,得到抗水溶聚乙烯醇纳米纤维;所述抗水溶聚乙烯醇纳米纤维所制备的纤维毡的平均孔径和纤维直径分别为0.44μm和0.45μm;其中,抗水溶性处理包括以下步骤:
将戊二醛、第二催化剂、水和有机溶剂混匀,然后将所述聚乙烯醇纳米纤维浸入其中;
(2)将所述抗水溶聚乙烯醇纳米纤维浸入含第一催化剂的水溶液中,将经催化剂处理的纳米纤维转移至含有吡咯的体系中,通过气相沉淀法使所述吡咯在纳米纤维表面发生聚合反应,得到所述基于聚乙烯醇纳米纤维的非织造吸声材料;所述第一催化剂为氯化铁、双氧水、过硫酸铵和碘化钾中的一种或几种;水溶液中所述第一催化剂的质量百分比为5wt.%-20wt.%。
2.根据权利要求1所述的基于聚乙烯醇纳米纤维的非织造吸声材料的制备方法,其特征在于:所述第二催化剂为盐酸、硫酸和硝酸中的一种或几种。
3.根据权利要求1所述的基于聚乙烯醇纳米纤维的非织造吸声材料的制备方法,其特征在于:所述有机溶剂为丙酮、乙腈和乙醚中的一种或几种。
4.根据权利要求1所述的基于聚乙烯醇纳米纤维的非织造吸声材料的制备方法,其特征在于:在步骤(1)中,通过静电纺丝方法得到所述聚乙烯醇纳米纤维。
5.权利要求1-4中任一项所述的方法所制备的基于聚乙烯醇纳米纤维的非织造吸声材料。
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