CN115233441B - 一种用于室内空气净化的多功能壁布的制备方法 - Google Patents

一种用于室内空气净化的多功能壁布的制备方法 Download PDF

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CN115233441B
CN115233441B CN202210526276.8A CN202210526276A CN115233441B CN 115233441 B CN115233441 B CN 115233441B CN 202210526276 A CN202210526276 A CN 202210526276A CN 115233441 B CN115233441 B CN 115233441B
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孙松美
邹宇鹏
彭欣怡
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Abstract

本发明提供了用于室内空气净化的多功能壁布的制备方法。本发明的制备方法包括:首先配制PVA或PEO溶液,取适量的光催化纳米粉末加入PVA或PEO溶液中,然后加入硅烷偶联剂,混合搅拌均匀,得到光催化前驱液,而后将所得的光催化前驱液通过静电纺丝喷涂在玻璃布的基底上,经过烘干后煅烧处理,最后冷却至室温便得到了多功能壁布。本发明利用静电纺丝技术进行催化剂的负载便于精确调控催化层厚度与基底材料结合强度,采用玻璃纤维布做基底,在传统的方法上加入了硅烷偶联剂,使得催化剂与玻璃布基底上结合的更加紧密,延长了壁布的使用寿命。该壁布在自然光下或是室内节能灯光下可有效去除室内有机污染物,具有良好的应用前景。

Description

一种用于室内空气净化的多功能壁布的制备方法
技术领域
本发明涉及一种用于室内空气净化的多功能壁布的制备方法,属于室内空气净化技术领域。
背景技术
甲醛的强挥发性使其成为了室内空气污染的主要成分。当室内的甲醛浓度达到0.08mg/m3时便可以引起眼睛红肿、瘙痒、咽喉不适或疼痛、声音嘶哑、喷嚏、胸闷、气喘、皮炎等症状。长期接触高浓度甲醛,甚至会出现身体中毒现象等。
针对上述的室内甲醛危害,发展出了多种去除甲醛的方法。目前主流的室内除甲醛的技术主要是物理法和化学法,物理法包括通风和物理吸附。其中通风除甲醛的方法耗时长,一般需要3-6个月时间,虽然对于室内的甲醛去除有效但是耗时较长而且不能从根本上解决后续甲醛污染问题。物理吸附法通过吸附介质的多孔结构来实现对空气中甲醛的吸附去除,例如采用活性炭等介质,这个过程中的甲醛仅仅被吸附储存到了介质中,长时间使用可能会导致甲醛的可逆析出,重新进入室内空气中。化学法主要是利用喷洒化学类试剂来针对性的分解室内的甲醛,但是这类化学试剂具有强氧化性会氧化家具等室内装修,同时喷洒化学试剂对于甲醛的治理仅是暂时性的,待室内甲醛积累到一定程度时需要重新喷洒处理,费时费力。
光催化作为一种新兴的污染气体去除技术,利用光催化剂在自然光或紫外光的照射下将包括甲醛在内的所有挥发性有机污染物(VOCs)分解为二氧化碳和水等无污染介质,相比其他化学药剂的使用,光催化法的条件更加温和、简单,对于居室内的家具等影响更小。除此之外,光催化剂表面产生的氧化性自由基还能对居室内的细菌、病毒等起到氧化分解的作用,使其在实际应用中起到去除VOCs和分解病菌的多重功能。同时,得益于催化剂本身的稳定性,光催化材料可以保证长时间对室内的有机污染物和病菌的分解去除。
壁布作为一种新型的装修材料,因为它色彩丰富,质感柔和,所以被广泛的使用在现代装修中。而作为壁布基底的玻璃布或高硅氧布因其高燃点,更是一种防火材料,如果将光催化材料成功集成到玻璃布或高硅氧布表面并保持其高的催化活性及材料稳定性,使其由原来的装修污染材料变成多功能健康环保材料,则可以大大改进目前壁布在家居装修中的市场占有率。
虽然在玻璃纤维布表面负载光催化材料的研究已经报道很多,目前能够实际应用的很少。究其原因主要是受限于材料负载技术。比如,常用的采用原位生长法在玻璃布表面负载光催化材料,玻璃布需要经过酸洗,碱洗以及后续原位化学生长过程,不但处理成本高还很难保证负载材料生长过程的稳定性。另外一种常见负载方法是采用涂覆模式,该方法获得的催化剂涂层较厚,机械强度低,光催化膜材料在玻璃布表面会因为碰撞等外力因素脱落,虽然胶黏剂的使用可以改善该类材料脱落状况,但是不能根本上解决材料在有外界摩擦碰撞环境下的应用问题,而且高分子胶黏剂还会在使用过程中被光催化材料逐渐降解,最终导致光催化涂层完全脱落。
综上所述,基于玻璃纤维基底的光催化空气净化用膜材料用途广泛,其制备方法近年来已经成为该领域研究热点,但是受限于目前该类材料制备技术,获得的玻璃纤维负载产品在成本,性能及使用稳定性方面尚不能满足市场化应用需求,因此亟需发展一种简单易行的低成本制备高活性及高稳定性玻璃纤维负载光催化材料的技术。
发明内容
本发明的目的是:克服现有玻璃布上负载光催化材料技术的不足,采用电纺丝喷涂技术制备具有高活性、高机械强度、耐曲揉的光催化空气净化用壁布产品,能够在自然光下或是室内节能灯照射下,对空气中挥发性有机物氧化去除,并且由于通过静电纺丝参数设置可严格控制光催化材料厚度及与玻璃布层的结合强度,该壁布在长期使用过程中可避免光催化材料脱落问题。
为了实现上述目的,本发明提供了一种用于室内空气净化的多功能壁布的制备方法,包括:首先配制一定浓度的聚乙烯醇(PVA)或聚氧化乙烯(PEO)溶液,取适量的光催化纳米粉末加入PVA或PEO溶液中,得到混合溶液,然后在混合溶液中加入硅烷偶联剂,混合搅拌均匀,得到光催化前驱液,而后将所得的光催化前驱液通过静电纺丝喷涂在玻璃布的基底上,经过烘干后煅烧处理,最后冷却至室温便得到了多功能壁布。
优选地,所述的光催化纳米粉末为钨酸铋、钒酸铋、钼酸铋、氧化铋、氧化钨、氧化钼、氧化锌、二氧化钛、氮化碳等半导体类纳米光催化粉末,所述玻璃布基底为普通玻璃布或高硅氧布,所述硅烷偶联剂为环氧基硅烷偶联剂 C9H20O5Si(KH-560)、C9H20O4Si(KH-781)、C11H22O4Si(KH-1771)、C12H26O5Si (KH-561)、C14H28O4Si(KH-1770)等;甲基丙烯酰氧基硅烷偶联剂C10H20O5Si (KH-570)、C16H32O5Si(KH-571)、C10H20O4Si(KH-572)、C16H38O5Si4(KH-573)、C13H26O5Si(KH-574)等;乙烯基硅烷偶联剂C5H12O3Si(KH-171)、C8H18O3Si (KH-151)、C11H24O6Si(KH-172)、C8H12O6Si(KH-188)等。其中,高硅氧布是一种耐热、柔软的特种晶体纤维织物,其SiO2含量达到96%以上,其具有更优秀的耐热特性。
优选地,所述PVA溶液的质量分数为1~20%,PEO溶液的质量分数为 0.1~15%,所述光催化剂粉末与PVA溶液的质量比为1:1~100,所述光催化剂粉末与PEO溶液的质量比为1:1~50,所述硅烷偶联剂与混合溶液的质量比为 1:5~1000。
更优选地,所述PVA溶液的质量分数为5~10%,所述PEO溶液的质量分数为1~8%,所述光催化剂粉末与PVA溶液的质量比为1:10~50,所述硅烷偶联剂与混合溶液的质量比为1:10~500。
优选地,所述静电纺丝的工艺条件为:电纺电压12~20KV,相对空气湿度 15~45%,环境温度为15~35℃。
更优选地,所述静电纺丝的工艺条件为:电纺电压15~20KV,相对空气湿度20~30%,环境温度为25~30℃。
优选地,所述煅烧的温度为300~850℃,升温速率为0.1~20℃/min,保温时间为1~6h。
更优选地,所述煅烧的温度为400~600℃,升温速率为2~8℃/min,保温时间为2~4h。
本发明还提供了上述的制备方法制备得到的多功能壁布在净化室内空气中的应用。
本发明与现有技术相比,具有如下有益效果:
(1)本发明采用静电纺丝技术来进行催化剂的负载,使得生产过程更加简便且可控;本发明在传统的方法上加入了硅烷偶联剂,使得催化剂与玻璃布基底结合的更加紧密,延长了壁布的使用寿命,而且催化剂效率及与壁布贴合强度可通过硅烷偶联剂加入量调控;
(2)本发明通过对工艺条件的优化,包括对底物的浓度和比例、煅烧温度和静电纺丝参数的优化,可使得所制备的多功能壁布具有更高的催化降解效率,从而能够更好地起到净化室内空气的作用;
(2)本发明采用玻璃纤维布做基底,能够同时实现防火功能,同时所采用的光催化剂对于空气中的细菌病毒也有氧化分解效果,集多重功能与一体,更符合现在市场需求;本发明对于挥发性有机污染物去除效果好,所需条件简单,易于日常使用,相比同类型产品具有更高的实用性。
附图说明
图1为实施例1中获得的多功能壁布的扫描电镜图片;
图2为实施例1和实施例2中获得的单位面积的壁布在实验室条件下对于甲醛的降解曲线;
图3为实施例1和实施例3中获得的单位面积的壁布在实验室条件下对于甲醛的降解曲线;
图4为实施例1和实施例4中获得的单位面积的壁布在实验室条件下对于甲醛的降解曲线;
图5为实施例1中制得的壁布样品分别在不同光源条件下对于甲醛的降解率对比曲线图;其中,A代表样品在实验室光源条件下的甲醛降解曲线,B代表样品在80W家用节能灯条件下的甲醛降解曲线;
图6为实施例1中制得的壁布样品在实验室光源下对于甲苯的降解效率曲线图;
图7为实施例5中更换7wt%PVA为5wt%PEO后获得的钨酸铋负载玻璃布样品在300W氙灯下对甲醛的降解效果图;
图8为实施例6与实施例7中更换硅烷偶联剂为甲基丙烯酰氧基硅烷偶联剂C10H20O5Si(KH-570)与乙烯基硅烷偶联剂C5H12O3Si(KH-171)后获得的钨酸铋负载玻璃布样品在300W氙灯下对甲醛的降解效果图;
图9为实施例8与实施例9获得的钒酸铋负载玻璃布(BiVO4/GF)、钼酸铋负载玻璃布(Bi2MoO6/GF)、氧化铋负载玻璃布(Bi2O3/GF)、氧化钨负载玻璃布(WO3/GF)、氧化钼负载玻璃布(MoO3/GF)、氧化锌负载玻璃布(ZnO/GF)、二氧化钛负载玻璃布(TiO2/GF)、C3N4负载玻璃布样品(C3N4/GF)在300W 氙灯下对甲醛的降解效果图。
具体实施方式
为使本发明更明显易懂,兹以优选实施例,并配合附图作详细说明如下。
实施例中采用的实施条件可以根据具体厂家的条件做进一步调整,未注明的实施条件通常为常规实验中的条件。实施例中使用的甲醛为国药产的分析纯甲醛溶液,经恒温烘箱60℃保持30分钟以保证甲醛完全挥发。降解测试实验采用模拟实验,通过提高反应中的环境条件,如光照强度、甲醛浓度以及反应器内的氧氮浓度等,来缩短反应所需要的时间。
实施例1
取质量分数为7wt%的PVA(聚乙烯醇)溶液,取钨酸铋:PVA质量比为1: 10的钨酸铋(Bi2WO6)纳米粉末加入PVA溶液中,而后向混合溶液中加入2wt%的硅烷偶联剂C9H20O5Si(KH-560),用搅拌器将三者混合搅拌均匀,而后将混合好的溶液在电压17.5KV,环境温度28℃,湿度25%的条件下在玻璃布的基底上进行静电纺丝,得到负载的玻璃布;将负载的玻璃布经烘干后置于马弗炉中空气氛围下煅烧,以5℃/min的升温速率升温至450℃保温2小时,待冷却后得到钨酸铋负载玻璃布(Bi2WO6/GF)壁布样品。将其裁剪为面积约为20cm2的长条状,固定到容积为300毫升的光催化反应器内,密封反应器保证整个容器运行过程中不漏气。用反应器的采样口向反应器内部通入氧氮混合气(氧气75%)20 分钟,随后取分析纯甲醛,用精密注射器量取10μL甲醛,通过反应器的注射口注射进反应器内。将反应器置于60℃的恒温烘箱中,保持30分钟保证甲醛的完全挥发,接着取出反应器。通过注射口采样,经色谱分析测得反应器内甲醛的初始浓度,后对反应器在300W氙灯下光照,每隔2小时采样一次,以此绘制间隔两小时的甲醛降解曲线。
实施例2
本实施例与实施例1的不同之处仅在于:提高了光催化壁布制备实验中PVA (聚乙烯醇)溶液,改用15%的PVA(聚乙烯醇)溶液。
其余内容均与实施例1中所述完全相同,获得样品钨酸铋与玻璃布之间结合力较实施例1低,外力摩擦下纳米薄膜有脱落。
实施例3
本实施例与实施例1的不同之处仅在于:改变了光催化壁布制备实验中的煅烧条件,在空气气氛下于管式炉中350℃煅烧2小时。
其余内容均与实施例1中所述完全相同。
实施例4
本实施例与实施例1的不同之处仅在于:改变了光催化壁布制备实验中静电纺丝的条件,调整静电纺丝时环境湿度为35%的,在增加环境湿度的条件下进行静电纺丝负载。
其余内容均与实施例1中所述完全相同。
实施例5
本实施例与实施例1的不同之处仅在于:将实施例1中7wt%的PVA溶液换成5wt%的PEO溶液。
其余内容均与实施例1中所述完全相同。
实施例6
本实施例与实施例1的不同之处仅在于:将硅烷偶联剂从环氧基硅烷偶联剂C9H20O5Si(KH-560)改为甲基丙烯酰氧基硅烷偶联剂C10H20O5Si(KH-570)。
其余内容均与实施例1中所述完全相同。
实施例7
本实施例与实施例1的不同之处仅在于:将硅烷偶联剂从环氧基硅烷偶联剂C9H20O5Si(KH-560)改为乙烯基硅烷偶联剂C5H12O3Si(KH-171),并且硅烷偶联剂添加量从2wt%提高至3wt%。
其余内容均与实施例1中所述完全相同。
实施例8
本实施例与实施例1的不同之处仅在于:添加的光催化纳米粉末由钨酸铋分别改为钒酸铋、钼酸铋、氧化铋、氧化钨、氧化钼、氧化锌、二氧化钛等氧化物半导体纳米光催化粉末。
其余内容均与实施例1中所述完全相同,获得了钒酸铋负载玻璃布、钼酸铋负载玻璃布、氧化铋负载玻璃布、氧化钨负载玻璃布、氧化钼负载玻璃布、氧化锌负载玻璃布、二氧化钛负载玻璃布样品,玻璃布与光催化粉末材料之间结合牢固。
实施例9
本实施例与实施例1的不同之处仅在于:添加的光催化纳米粉末由钨酸铋改为纳米C3N4粉末,煅烧气氛改为管式炉中氮气。
其余内容均与实施例1中所述完全相同,获得C3N4负载的玻璃布样品,C3N4与玻璃布之间结合牢固。
表征与测试结果:
图1为实施例1中获得的多功能壁布的扫描电镜图片;从图1可以看出,光催化纳米颗粒均匀负载于玻璃布基底上;
图2为实施例1和实施例2中获得的单位面积的壁布在实验室条件300W氙灯下对于甲醛的降解曲线,从图2可以看出,在相同条件下实施例1中制得的样品在8小时内对于甲醛得降解达到了72%左右,而实施例2中制得样品8小时对于甲醛得降解只有43%左右;
对比实施例1和实施例2的降解测试结果可知:实施例2中将所用的PVA (聚乙烯醇)溶液浓度提高到15%时,过高的PVA溶液浓度使得静电纺丝膜更难负载到玻璃布基底上,因此实施例2中制得的样品对于甲醛的降解率明显下降,性能较差,而且发现催化剂颗粒容易从玻璃布基底上脱落。
图3为实施例1和实施例3中获得的单位面积的壁布在实验室条件下对于甲醛的降解曲线,由图3可以看出,在相同条件下实施例1中制得的样品在8小时内对于甲醛的降解达到72%,而实施例3中制得样品8小时对于甲醛的降解只有 42%左右;
对比实施例1和实施例3的降解测试结果可知::实施例3中降低了煅烧温度,较低的温度不足以使得样品中的PVA模板剂被氧化去除,所以实施例3中的样品对于甲醛气体的光催化降解能力下降。
图4为实施例1和实施例4中获得的单位面积的壁布在实验室条件下对于甲醛的降解曲线;由图3可以看出,在相同条件下实施例1中制得的样品在8小时内对于甲醛的降解达到72%,而实施例4中制得样品8小时对于甲醛的降解只有41%左右;
对比实施例1和实施例4的降解测试结果可知:实施例4中增加了静电纺丝时的环境湿度,较高的湿度导致静电纺丝过程中纺丝液的水分蒸发较慢,使得静电纺丝膜更难负载到玻璃布基底上,因此实施例4中的样品对于甲醛的降解率明显下降,性能较差,而且光催化材料容易从玻璃布基底脱落。
图5为实施例1中制得的壁布样品分别在不同光源条件下对于甲醛的降解率对比曲线图,可见样品在模拟日常使用条件下也能高效的降解空气中的甲醛;
此外,还对实施例1所制备的多功能壁壁布进行了甲苯降解效率的测试,测试过程和条件与甲醛降解测试一致,不同的是,将其中的甲醛替换为甲苯,两者浓度相同,并绘制甲苯降解曲线。
图6为实施例1中制得的壁布样品对于甲苯的降解效率曲线图,由图可知,制得的壁布样品对于空气中的甲苯也能有效的去除。
图7为实施例5中更换7wt%PVA为5wt%PEO后获得的钨酸铋负载玻璃布样品在300W氙灯下对甲醛的降解效果图;
图8为实施例6与实施例7中更换硅烷偶联剂为甲基丙烯酰氧基硅烷偶联剂C10H20O5Si(KH-570)与乙烯基硅烷偶联剂C5H12O3Si(KH-171)后获得的钨酸铋负载玻璃布样品在300W氙灯下对甲醛的降解效果图;
图9为实施例8与实施例9获得的钒酸铋负载玻璃布(BiVO4/GF)、钼酸铋负载玻璃布(Bi2MoO6/GF)、氧化铋负载玻璃布(Bi2O3/GF)、氧化钨负载玻璃布(WO3/GF)、氧化钼负载玻璃布(MoO3/GF)、氧化锌负载玻璃布(ZnO/GF)、二氧化钛负载玻璃布(TiO2/GF)、C3N4负载玻璃布样品(C3N4/GF)在300W 氙灯下对甲醛的降解效果图。
以上所述,仅为本发明的较佳实施例,并非对本发明任何形式上和实质上的限制,应当指出,对于本技术领域的普通技术人员,在不脱离本发明的前提下,还将可以做出若干改进和补充,这些改进和补充也应视为本发明的保护范围。

Claims (3)

1.一种用于室内空气净化的多功能壁布的制备方法,其特征在于,首先配制一定浓度的PVA或PEO溶液,取适量的光催化纳米粉末加入PVA或PEO溶液中,得到混合溶液,然后在混合溶液中加入硅烷偶联剂,混合搅拌均匀,得到光催化前驱液,而后将所得的光催化前驱液通过静电纺丝喷涂在玻璃布的基底上,经过烘干后煅烧处理,最后冷却至室温便得到了多功能壁布;
所述PVA溶液的质量分数为5~10%,所述PEO 溶液的质量分数为1~8%,所述光催化剂粉末与PVA溶液的质量比为1:10~50,所述硅烷偶联剂与混合溶液的质量比为1:10~500;
所述静电纺丝的工艺条件为:电纺电压15~20KV,相对空气湿度20~30%,环境温度为25~30℃;
所述煅烧的温度为400~600℃,升温速率为2~8℃/min,保温时间为2~4h。
2.如权利要求1所述的用于室内空气净化的多功能壁布的制备方法,其特征在于,所述的光催化纳米粉末包括钨酸铋、钒酸铋、钼酸铋、氧化铋、氧化钨、氧化钼、氧化锌、二氧化钛和氮化碳中的至少一种,所述玻璃布基底包含普通玻璃布或高硅氧布,所述硅烷偶联剂为环氧基硅烷偶联剂KH-560、KH-781、KH-1771、KH-561、KH-1770和甲基丙烯酰氧基硅烷偶联剂KH-570、KH-571、KH-572、KH-573、KH-574以及乙烯基硅烷偶联剂KH-171、KH-151、KH-172、KH-188中的至少一种。
3.权利要求1或2所述的制备方法制备得到的多功能壁布在净化室内空气中的应用。
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CN111744549A (zh) * 2020-07-25 2020-10-09 合肥学院 一种玻璃纤维布负载W/BiVO4光催化剂的制备方法及应用
CN113041862A (zh) * 2021-04-02 2021-06-29 上海洁晟环保科技有限公司 一种复合膜材料及其制备方法和过滤膜、收纳装置

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