CN1312779A - 具有光催化涂层的底材 - Google Patents
具有光催化涂层的底材 Download PDFInfo
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- CN1312779A CN1312779A CN99809531A CN99809531A CN1312779A CN 1312779 A CN1312779 A CN 1312779A CN 99809531 A CN99809531 A CN 99809531A CN 99809531 A CN99809531 A CN 99809531A CN 1312779 A CN1312779 A CN 1312779A
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- coating
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- fiber
- adhesion promoters
- filamentary material
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Abstract
本发明的目的是含有纤维材料并在其至少部分表面和/或其厚度上涂布具有光催化性能的涂料的底材,该涂料含有具有光催化性能的氧化物或硫化物型半导体材料。本发明的另一个目的是其制造方法及其应用。
Description
本发明涉及具有光催化涂层的底材、这种涂料的制造方法及其各种应用。
更具体本发明涉及含有金属氧化物基半导体材料的涂层,特别是含有氧化钛基半导体材料的涂层,在适当波长光线的辐照作用下,其能够引发导致有机化合物氧化的自由基反应。因而,此涂层能够赋予其所覆盖的材料新的功能,特别是防污性、杀真菌、杀菌、杀藻、除臭等性能,任选地兼备亲水或防冷凝等性能。
迄今为止已经设想了许多不同的底材,特别是用于建筑或车辆领域的结构材料(窗户、饰面、贴面层或屋面材料等)中,或者在提纯方法中使用的材料。
在国际专利申请书WO 97/10186和WO 97/10185中已知含具有光催化性能的锐钛矿结晶TiO2的涂层,由适当的金属有机前体经热分解和/或由“预结晶的”TiO2颗粒得到的涂层,特别适合于在玻璃上沉积为一薄层,以保持其光学质量。
还在专利EP-A-0,306,301中已知在用来净化空气的纤维材料上应用光催化TiO2,和通过溶胶-凝胶类的方法实施TiO2的沉积。
因此,本发明的目的是改善此光催化涂层,特别旨在改善其在各种底材上的性能,特别是有更好的粘接性和更好的耐久性,特别是在具有表面粗糙或多孔特征的底材上。
首先,本发明的目的是含有纤维材料的所有底材,而且在其至少一部分表面和/或在其厚度上提供具有光催化性能的涂层,该涂层含具有与所述纤维材料的粘接促进剂相组合的氧化物或硫化物类光催化性能的半导体材料。
按照本发明,对光催化具有“活性”的半导体材料可以基于至少部分结晶的金属氧化物,比如氧化锌、氧化锡或氧化钨。按照本发明优选的例子涉及至少部分结晶的呈锐钛矿型的氧化钛,这是一种赋予TiO2光催化性能的晶相。还可以涉及也是至少部分结晶的属于硫化物族的半导体材料,比如硫化锌或硫化硼(在下面的文字中,为了更简单起见,我们将只叙述氧化钛,不言而喻所给出的指征对上面所举出的其他半导体材料也都是有效的)。
在本发明的意义上,术语“纤维材料”可以理解为任何含纤维的材料,特别是无机纤维,更具体是玻璃纤维或岩石纤维等矿棉纤维。这种材料用于隔热/隔声或构成无土培养基材。术语“纤维材料”还包括一种用于增强的形成纱的纤维/长丝,特别是由玻璃制成的纱。
然后,以不同的形式将这些基础纤维材料加入到在本发明意义上的“底材”中,这可以涉及由矿棉形成的用来为管道保温的毡、垫、纤维网、“模制壳”等、组合为织物的纱纺织品,或者在纸质底材上的非纺织纤维网,等。
光催化涂层能够赋予这些已知底材以很有意义的新功能。比如,主要用于保温的矿棉毡/垫可以只在表面上进行处理,比如在其表面中的一个,或者在表面中的每个上面进行处理,就能够在建筑物的假顶棚上,在公路或铁路两侧的障声板中,等等,至少在被处理过的一个表面(可见的表面或隐藏的表面)上获得抗污/除臭的功能,其条件是,此光催化涂层容易受到天然或人造光源的影响。在保温的领域中,上述的“模制壳”也可以处理其内侧和/或外侧,或者在其整个厚度上处理,比如给其以抗污功能和/或杀菌、杀真菌功能等。当底材呈垫状或模制壳状时,用本发明方法处理的底材最好被布置在整个排风系统或空调系统出口套管附近,但也可以布置在这些管道的内部,这些装置才是真正的细菌繁殖地,条件是应该提供一种手段,使此光催化涂层曝露在足够量的有效紫外线之下:在其可见的外表面,天然的照明就足够了,否则就应该使底材与卤素灯或荧光灯管人工照明设备相连。
另外的一种应用涉及任何天然光或来自人工照明设施的光线的反射和/或漫射系统,比如灯罩、窗帘等,这时的底材是比如呈网状。
除了隔热或隔声以外,按照本发明处理的底材的另一种重要应用涉及流体的过滤或提纯领域。
这涉及各种用于过滤气体,特别是过滤空气的纸网类或滤纸类过滤器,可用在比如上面提到的住宅,或者工业场所、车辆或控制粉尘量的实验室“清洁”房问的通风/空调系统中。
术语“过滤器”在本发明的意义上同时覆盖两个概念,一个概念是真正的过滤,在这里将颗粒与携带它的气体进行机械分离,另一个概念是扩散器的概念,特别是除臭扩散器的概念,在这里不必强迫被处理的气体通过光催化底材,在此,气体能特别简单地与底材接触,并不留下悬浮的颗粒。
还可以举出许多其它按照本发明的气体“过滤器”的例子:它们也可以用于各类工业气流,或给定房间、公共场所大气的净化(比如在地铁中的除臭扩散器)。它们特别可以降低给定气流、给定大气中的有机挥发化合物(VOC)的含量。
在其表面上,或在其整个厚度上进行了处理的过滤器可以变得更有效和更耐久,这是因为,按照本发明进行的处理不仅给它以消除微生物的能力,而且还使脂肪类有机残留物分解,这些残留物一般构成颗粒的相当部分,逐渐它会阻塞过滤器。因而使用本发明,这些过滤器的寿命期就会更长,另外它们还具有除臭的功能。
也可以涉及液体的过滤器。
按照本发明的液体过滤器具有许多用途:它们可以用于废水的循环、无土栽培底材灌溉系统用水的循环(用于水的消毒)。它们还可以担当消除污染的功能,特别是消除土壤的污染的功能,或者工业液流的再处理/消除污染的功能。
我们已经看到了按照本发明处理这些纤维底材的意义。但是,为其提供光催化涂层首先不是很容易的。这是因为,起因于在一般是不平滑的、非平面的、凹凸和多孔底材上沉积涂层的方法的问题,以及此类涂层的耐久性的问题。
本发明的解决办法包括调整在底材上进行涂布的方式,即,根据所要求的功能的应用,在表面上涂布还是在整个厚度上涂布,和借助于适当的粘接促进剂使具有光催化性能的锐钛矿型TiO2涂层与纤维材料成为一体。因此,此促进剂的作用是作为对光催化现象有“活性”的涂层组分的“基质”。
按照第一个可选择的方法,当将氧化钛加入到涂料中时,其以锐钛矿形式已经至少部分预结晶,然后沉积在底材上。它可以呈在胶体悬浮液中的结晶颗粒形式,或者呈干粉的形式加入到涂料中,所述干粉由或多或少在其间任选发生附聚的颗粒组成。此方案的优点包括不需要对要进行沉积的涂层/底材进行特别的高温热处理(呈锐钛矿型的TiO2一般在400℃左右结晶)。
按照第二个可选择的方法(它也可以和第一方法结合使用),氧化钛来自其前体,特别是有机金属或金属卤化物型前体,在涂料中的热分解。因此可以当涂料被涂布在底材上时,通过专门准备的热处理,在涂层中“就地”制造锐钛矿型结晶TiO2,但是此热处理应该与所选择的底材和所选择的粘接促进剂是相容的。
至于所涉及的粘接促进剂,可以是单组分的或者是多组分的,其组成可以是有机的、无机的或者有机-无机杂化物。
因此可以包括呈分子状或聚合物状的含硅组分,比如硅烷类、聚硅氧烷类或硅氧烷类。这些组分与对本发明有意义的大多数矿物纤维、玻璃纤维、岩石纤维,甚至于陶瓷纤维具有良好的亲和性。在某些情况下,甚至可以说通过这类组分将结晶TiO2接枝到无机纤维之上。
粘接促进剂还可以包括一种或几种有机型聚合物。实际上,存在两种情况:可以选择标准的有机聚合物,比如丙烯酸类、酚甲醛类等。在此情况下,此组分的风险是,其由于TiO2的光催化作用而逐渐分解,至少易于暴露在紫外线之下的底材的(表面)区域发生。但是,在某些应用中实际上已经证实该方法有逐渐“释放”活性TiO2的优点。然而,可以优选通过选择适当的聚合物,在仅可能范围内避免或减缓这种分解,一般选择能耐受光催化侵袭的含氟聚合物,比如含氟丙烯酸类聚合物、聚四氟乙烯(PTFE)、聚偏氟乙烯(PVDF)、或四氟乙烯-乙烯共聚物(ETFE)等。
一个可选择的方法包括保留基于有机聚合物的粘接促进剂和通过适当的添加剂阻止其分解,特别是加入抗氧剂(如Ciba公司以商品名Irganox销售的产品)和/或紫外线吸收剂(如同一公司以商品名Tinuvin销售的产品)和/或按英语称之为“位阻胺光稳定剂(hindered amine light stabilizers)”即“HALS”的空间位阻胺形成的稳定剂。
此粘接促进剂还可以含有至少一种金属氧化物,包括TiO2或SiO2型,它们来自在涂层中的含硅的、有机金属或金属卤化物前体的热分解。在此情况下,TiO2或SiO2组分是在涂层中就地产生,特别是一旦其被涂布在底材上时,通过与此底材相容的适当热处理而就地产生。但是,在TiO2的情况下,如果仅仅追求粘接促进剂的功能,就不一定需要锐钛矿结晶所必需的很高的温度:它可以完全是无定形的,或者象SiO2一样是呈不同晶型的部分结晶的。因此可能具有将结晶的光催化氧化物“活性”颗粒固定的无定形金属氧化物类基质的涂层。
此粘接促进剂还可以含有至少一种无机组分,它选自磷酸铝和硅铝酸钾或硅铝酸钙。
本发明的一个可选择的方法包括,使涂层两种基本组分的至少一种成为能够对纤维材料有内在粘接性的粘接剂的一部分,所述基本组分,即一种是“活性”(对光催化而言)组分,另一种是粘接促进剂。
实际上,如果涉及到保温类型的玻璃棉或岩石矿棉,如IsoverSaint-Gobain公司的产品,在许多应用中,它们都带有一般称之为施胶剂的粘接剂,一般是在成纤机器中以液态喷涂在纤维上。溶剂/分散剂一般是水性的,在接触或靠近被加热的纤维时,溶剂/分散剂蒸发。使纤维彼此粘结的施胶剂一般是树脂类的,比如苯酚类树脂,如脲-苯酚-甲醛聚合物,其在加热下固化。这时的一种可能性包括在施胶剂的水介质中加入粘接促进剂和“活性”组分,或者使用/采纳施胶组分,使其同时起到纤维之间粘接剂和纤维/“活性”组分的粘接促进剂在作用。
对于典型施胶组合物及其在纤维上涂布方式的更多的细节,最好见以下专利中的报道,即EP-148,050、EP-246,952、EP-305,249、EP-369,848、EP-403,347、EP-480,778、EP-512,908。但是应该注意到,在一些特定的应用中,矿棉可以不含粘接剂,比如在EP-0267,092和EP-0 430,770中叙述的由用于制造滤纸的比较细的纤维组成的材料,或者针冲毡。
如果更涉及到增强纱、纱织物类的纤维材料,特别是Vetrotex公司制造的产品,在衬套中由成束的单根单丝组成的纱之间的内聚力一般由涂布的粘接剂来保证,这种粘接剂一般称之为施胶组合物。再有,它在液相涂布,并含有一种或几种纤维/单丝的“胶合”试剂。因此可以选择在液体介质中加入本发明的“活性”组分和/或粘接促进剂,或者采用其组合物使其同时起着单丝间粘接剂和纱/“活性”组分粘接促进剂的作用。
对于这些施胶组合物的更多细节,最好参见如下专利:EP-243,275、EP-394,090、EP-635,462、EP-657,396、EP-657,395、EP-678,485、EP-761,619、WO-98/18737。
还可以举出专利WO 98/51633,它涉及在成纤机器上,在两个步骤中沉积施胶剂,此外,施胶剂可以在环境温度下聚合。在此情况下,能够选择加入具有光催化性能的材料,可以加入到施胶剂的第一组分中,或者第二组分中,也可以在两个组分中。
在上面提到的所有这些施胶剂一般都是借助于恰在衬套中的施胶辊来涂布在纱线并合过程中呈单根单丝状的纤维材料上的。还有一些粘接剂是用来保证由玻璃纤维纱线毯得到的毡的内聚力,将其喷在已经施胶的连续或不连续的纱线上。作为例子,可以举出专利WO97/21861。在此粘接剂中可以加入光催化材料,其作用也是粘接促进剂。
上面所列举的施胶剂或粘接剂可以是水相的,也可以是非水相的。在后一种情况下,一般不再须要进行热处理以除去水,这时所选择的各组分的选择方式是能够在环境温度下进行聚合。在此情况下,优先加入与任何热处理无关的预先存在的具有光催化性能的材料,如结晶氧化钛小颗粒。
因此,正如在上面所提到的,本发明的纤维材料可以制造成不同几何形状(比如平的或打皱的纸页、纸板、中空的圆筒形“模制壳”、纺织的或非纺织的织物等)的纤维网(比如成贴边)、毛毡、纸张的形式。此纤维材料还能以散装地任选呈等外纤维或短绒的形式存在。
本发明的光催化涂料最好以如下的方式涂布在纤维材料上,即至少一部分所述材料的“纤维”(包括纤维、长丝和纱的概念),在至少5nm的厚度上,特别是在大约30~50nm的厚度上罩上该涂层。
这样的外罩保证了最大的涂层效果,其光催化活性就因为其分布在更大的比表面上而更加大。优选的厚度要考虑最普遍遇到的锐钛矿型TiO2微晶的平均尺寸。
本发明的另一个目的是制造如上所定义的底材的方法。
按照第一个可选择的方法,在纤维材料的生产线自身上沉积液相的光催化涂层。此可选择的方法的意义在于,能够处理仍是半成品的纤维材料,并能在比如节省时间和制造成本的温度下,得到最好的使用。因此,第一种可选择的方法包括在成纤机器和纤维接受机器之间“热”沉积涂层。此成纤机器可以包括所谓“内离心机器”的玻璃离心盘,如在专利EP-0,189,534和EP-0,519,797中叙述的能够使玻璃类矿棉成纤的机器,或者如专利EP-0,465,310或EP-0,439,385中所述的借助于一系列离心轮的所谓外离心成纤装置,这可以得到玄武岩类的矿棉。还可以涉及,按照先有技术中专业人员已知的方法,借机械拉伸以获得增强玻璃纱、借空气成型或借蒸汽吹制的成纤装置。如此使用是因为纤维还处于比较高的温度,涂布的涂料一般以在比如水溶剂的溶剂中的溶液/分散液的形式,当与纤维接触或靠近时,溶剂会蒸发。如果粘接促进剂是树脂类的话,热还可以使其中的一个或几个组分固化,而如果它们是前面提到过的含硅前体或金属前体的话,热会使它们热分解。
正如在上面所提到的,呈液相的涂料可以在与任选的施胶组合物类“粘接剂”同时涂布,或者甚至成为其一部分。在所述的“粘接剂”之前或之后涂布此纤维材料也可以是优选的。
按照此第一种可选择的方法的第二个实施方案,可以在接受装置收集从成纤装置出来的纤维/复丝或纱“以后”,沉积一般总是呈液相的光催化涂料,特别是在纤维材料的成纤后热处理之前或当中进行。因此,对于保温类的矿棉,接受装置一般包括收集矿棉的、并把它们送入到成形烘箱的吸入传送带。在两个装置(成纤/接受)之间在比如表面上涂布该涂层料,如果需要,再利用烘箱的热使之固化,或得到涂层可能是合理的。
同样,在增强玻璃纤维的领域内,纱线是呈卷筒的形式牵伸和卷绕的,或者在以适当的方式施胶以后在衬套中切断,然后一般是在加热室中干燥,再以后是运输和/或使用。
正如在前面所提到的,因此可以刚好在衬套中沉积光催化涂料,特别是伴随着能加入到其中的施胶料的沉积。也可以在卷筒上的纱整理为最终产品的阶段进行沉积:比如可以涉及随后进行的旨在制造剪切纱垫的转变操作中。也可以在下游生产线上进行沉积,特别是当组合在一起成为毡状的连续的纱线转变为连续纱线的垫的时候。
在这后两种情况下,可以在使用粘接剂之前、期间或同时,用调节的喷雾类的喷射系统来沉积光催化涂料,(或者与同样液相的粘接剂一起使用)。毡垫使用的粘接剂可以是液体的(一般是水乳液),也可以是粉末,粘接剂和在涂层料配方中必需的组分可以一起在同一个液相或粉末状中(比如当活性组分是光催化的TiO2粉末时)。
按照在保温矿棉领域中的一种类似方式,可以在其转变时,特别是当其由玻璃纤维棉层转变为玻璃纱布时处理纤维产品。正如此操作也须要使用应该随后热固化以保证毡的内聚力的第二种施胶料一样,在此第二种施胶料中可以加入适合于赋予其所希望的光催化性能的组分。
按照第二个可选择的方法,在随后操作中,在最终的纤维材料上沉积液相的光催化涂料。这时涉及的是与其“冷”处理,倒不如需要沉积后的热处理,以蒸发掉溶剂和任选固化(如果是在液相,而且当然不是粉末状时)或完成制备,以构成涂层。
无论选择哪一个方法,都可以用不同的技术来沉积涂层。如果该涂层从一开始就含有“活性”的结晶锐钛矿型TiO2颗粒或粉末,则纤维底材就不一定要加得很热,低于300℃,甚至低于200℃的温度,甚至环境温度可能就足够了,因此这是在生产线上碰到的矿物纤维材料的最普遍的温度,另外这是这些一般至少部分是有机材料的施胶料相容的温度。在另一方面,如果应该“就地”产生锐钛矿型TiO2,必须将温度设定在大约400℃左右,而不是,按一般术语的意义在随后的操作中用不合粘接剂的纤维材料,比如用溶胶-凝胶方法。
实际上,可以选择浸渍纤维材料成为芯材,使用“浸涂”类的技术,将至少一部分纤维材料浸入含有液相涂料的浴中。还可以选择适合于表面处理的涂布和喷雾技术。还可以在就术语的一般意义上的非液流体中进行此沉积,比如在超临界流体中。
本发明还有一个目的是此处理的底材在隔热/隔声方面,或者在具有抗污、杀真菌、防细菌、除臭等功能的贴面、或者在纸类或毡类、模制壳状的液体或气体的过滤器方面的应用。
在后面借助于下面的附图,以非限定性的方式通过对下面的辅助实施例的叙述来突出本发明的其它细节和优势的特征:
图1:按照本发明处理的纤维材料表面由扫描电子显微镜(MEB)得到的负片。
所有下面这些实施例都涉及涂层的沉积,这些涂层的光催化“活性”组分是锐钛矿型结晶TiO2。(不言而喻的是,正如在前面所指出的,本发明以同样的方式适合于具有类似于锐钛矿型TiO2的光催化性能的、而且能以同样形式提供的半导体“活性”组分,特别是氧化锌、氧化锡和氧化钨)。
实施例1
一块针刺毡(尺寸210×297×5mm3)由保温型玻璃纤维组成,其是通过无粘接剂内离心得到的,其相对密度为55kg/m3,在毡的整个厚度上喷涂TiO2水溶液,此水溶液是由Saga Céramics公司生产的商品名Tosol的产品。
此溶液含有呈锐钛矿型结晶TiO2颗粒的分散液,很可能由微晶的聚集体构成,这些聚集体的平均尺寸大约为20~80nm。因此用光催化的术语来说,这些颗粒是“活性”组分。此溶液还含有金属有机化合物的TiO2前体,在热处理时它们将分解为主要是无定形的TiO2,将起着粘接促进剂的作用。
将得到的涂层在200℃下烘烤2hr,其中含有在无定形TiO2基质中的锐钛矿型纳米晶体。如此制造的黄色过滤毡表明有来自前体溶液的有机化合物存在。在剂量为4W/m2的紫外A辐射下曝露2hr以后,黄色完全消失,这表明残留的有机物污染物完全分解。
实施例2
由无粘接剂内离心得到的保温型玻璃纤维在纯水中由造纸的方法进行转化。然后对得到的直径100mm、每单位面积重量为150g/m2的圆形玻璃纤维纸进行浸涂,在整个厚度上浸入含有5%(体积)的水、1%的四乙氧基硅烷(粘接促进剂)和1%的平均直径30nm的锐钛矿型结晶TiO2颗粒(“活性”组分)的醇分散液的浸渍液中。在流动空气下干燥此玻璃纤维纸,然后在450℃的烘箱中烘烤30min。然后将此过滤纸放在通风橱的入口处。一个不含有锐钛矿型TiO2的对照过滤纸放在临近的孔上。用紫外A灯照射此过滤纸,剂量是4W/m2。在通风罩操作15天以后,处理过的过滤纸仍然是白色,而未处理的过滤纸则沾上了油污。
实施例3
通过混合如下组分制造通过内离心而得到的保温型玻璃棉的施胶组合物:
-55g由苯酚和甲醛缩合得到的树脂,其初始甲醛/苯酚摩尔比为大约3.2/1,缩合按通常的方式进行操作,催化剂为氢氧化钠,相对于苯酚计,为5.5%(重量);
-45g尿素;
-3g氨丙基三甲氧基硅烷;
-0.3g硫酸铵;
-6g 30%(体积)的氨水;
-1200g锐钛矿型TiO2结晶颗粒水分散液,其浓度为25%(重量);
-34g水。
此TiO2颗粒的平均直径为大约45nm。其粘接促进剂可以认为是施胶剂中所有其它各组分,特别是硅烷。
在由离心盘制造玻璃棉的成纤过程中通过施胶环来喷涂此组合物。然后在生产线上将得到的毡在2min内通过一个180℃的烘箱。该毡的单位面积重量是560g/m2,灼烧损失是1.4%(按先有技术专业人员已知的方法测试,按重量计,在足可以除去所有有机化合物的温度下加热毡)。将一块1×20×40mm3的毡取出,放入20g含有1g/L乙醇和15g/L过氧化氢的水溶液中。用产生4W/m2紫外线的汞灯照射此溶液,用色度计监测过氧化氢的浓度。观察到由紫外线辐照的锐钛矿型TiO2所催化的乙醇被过氧化氢氧化。
通过测量溶液中每克纤维每小时使过氧化氢消失的以mg计的重量来评估毡的光催化活性。结果是4.4mgH2O2/g纤维/hr。
将由相同处理得到的200×300×200mm3的试样经受天然阳光的照射。曝露表面上所用树脂的特征性黄色逐渐消失,一直深入到几厘米深。这样的颜色消失清楚地表明使用的酚醛树脂的降解以及光催化效果深入到材料内部。在24hr内用4W/m2的控制UVA辐照得到类似的结果。
实施例4
在与实施例3类似的施胶组合物中加入280g环氧丙氧丙基三甲氧基硅烷(其它硅烷与前者一起起着粘接促进剂的作用)。通过成纤和用此溶液施胶得到的毡在180℃烘烤2min。此毡的单位面积重量是1kg/m2,灼烧损失是1.4%。如实施例3的操作测试的光催化活性给出的数值是3mgH2O2/g纤维/hr。
图1、2和3以三种不同的比例显示了光催化涂层所覆盖的纤维。图1更具体地表明了,以在表面上的TiO2颗粒的壳为明显特征的纤维,在图2和图3显示了两个相继的放大倍数。
作为结论我们观察到,本发明的涂层在纤维上具有被证实的光催化活性,而无论是采用哪一种选择方法:
实施例1说明在矿棉的生产线以外的“随后操作”的沉积,使用的是“预先结晶”的TiO2颗粒和在毡类纤维底材上就地制造的无机粘接促进剂。
实施例2也是说明在纸类纤维底材上的“随后操作”的沉积,使用的是预先结晶的TiO2颗粒和含硅粘接促进剂。
最后,实施例3和4说明在成纤装置上在线热沉积,这使得可以在纤维材料的整个厚度上进行处理,使用的是“预先结晶”的TiO2颗粒和与标准施胶剂一起使用的硅烷族水相粘接促进剂。
借助于一种装置制造基于无机纤维的光催化纤网,此装置可以将玻璃纤网浸入到施胶剂溶液中,使此纤网得到吸收涂布(为了除去过量的粘接剂)以及最后在烘箱中烘烤此吸收物,这一切都在生产线上连续进行。将此纤网在一输送带上展开,被浸渍辊带到一个施胶剂浴中,从一个减压箱(吸收装置)的上面经过,最后被第二输送带导入烘烤烘箱。
按照符合如下各实施例的方法合成了不同类型的光催化介质:
实施例5:气体提纯介质
将80g/m2的玻璃纤网用含有3.1%的Glymo(环氧丙氧丙基三甲氧基硅烷)和2.9%二氧化钛的纳米颗粒的水溶液浸渍,速度是0.2m/min。
让此纤网经受抽吸能力相当于35mm水柱的吸收,然后在200℃下烘烤10min。得到的灼烧损失是7%。
然后在如下的条件下进行气相效率的测试:
将150×200mm2得到的产品放在一个圆筒形光催化反应器中。此反应器包括一个轴向的UV-A灯(365nm),在其周围以间隔1cm围绕着3层光催化介质和一个铝质套筒。在纤网上的辐照强度是1mW/cm2。将此反应器插入到一个闭合回路中,气体经介质进行循环,它是从封闭的圆筒内侧经纤网向外侧流动。
光催化反应器室的体积为0.9L,整个回路的体积(固定的体积)为1L。实验包括评估正己烷的光催化分解。
为此,在回路中注入不同量的正己烷(最大为在空气中含2000ppm),后者流量调节为1L/min。以固定的时问间隔抽取50μL气体试样,测量在回路中存在的正己烷浓度。
显示出,被紫外线直接分解的正己烷微乎其微,刚好可以被介质吸收。反之,当其通过光催化介质时,即使在很弱的紫外线辐照下,在不到1小时的时间内实际上100%的正己烷被分解。
实施例6:液体提纯介质
按照同样的方法,将60g/m2的玻璃纤网浸渍在由适当的手段保持悬浮的含有1g/L硅烷A1100和5g/L的二氧化钛(Degussa公司商品名为P25的产品)的水溶液中。
以0.6m/min的速度在线浸渍此纤网,在90mm水柱的减压下除掉过量的粘接剂。在300℃下烘烤此物品30min。然后测量液相效果以评定此材料。
将一块圆形纤网试样(直径100mm)放在一个300mL烧杯的一半高度上。该容器的底和侧壁是不透明的,用成排的UV-A灯(365nm)照射烧杯,照到纤网上的功率是3.5mW/cm2。将含有10mg/L苯酚的水溶液(去离子水)倒入此装置,保持在磁力搅拌下。这时通过定时提取试样,用Dr Lange公司的紫外光谱仪监测苯酚浓度的下降。
可以证实,至多大约1小时,实际上100%的苯酚消失殆尽。
更一般化的说,后两个实施例显示出,象在气相中一样,在液相介质中进行的提纯操作,使用诸如所制造的光催化无机纤维形成的纤网,是有意义的。
Claims (18)
1.含有一种纤维材料并在其至少部分表面上和/或在其厚度上涂上具有光催化性能的涂层的底材,该涂层含有一种有光催化性能的氧化物或硫化物类型的半导体材料,特别是呈锐钛矿型的至少部分结晶的氧化钛,所述材料与所述纤维材料的粘接促进剂一起使用。
2.如权利要求1的底材,其特征在于,将氧化钛型半导体材料以胶体悬浮液中的颗粒形式或以粉末形式加入到涂层中。
3.如前面权利要求中之一项的底材,其特征在于,该氧化钛来源于在涂层中的有机金属或金属卤化物前体的热分解。
4.如前面权利要求中之一项的底材,其特征在于,该粘接促进剂是单组分的或多组分的有机物、无机物或有机/无机杂化物。
5.如前面权利要求中之一项的底材,其特征在于,该粘接促进剂包括硅烷类、聚硅氧烷类、硅氧烷类含硅组分。
6.如前面权利要求中之一项的底材,其特征在于,该粘接促进剂包括一种或几种有机聚合物,特别是丙烯酸类聚合物、含氟聚合物,任选与属于抗氧剂和/或紫外线吸收剂和/或HALS类型稳定剂类的添加剂一起使用。
7.如前面权利要求中之一项的底材,其特征在于,该粘接促进剂含有至少一种TiO2或SiO2型金属氧化物,它们来源于在涂层中的含硅、有机金属或金属卤化物前体的热分解。
8.如前面权利要求中之一项的底材,其特征在于,该粘接促进剂含有至少一种选自磷酸铝和硅铝酸钾或硅铝酸钙的无机组分。
9.如前面权利要求中之一项的底材,其特征在于,该粘接促进剂成为使纤维材料有内聚力的粘接剂的一部分,特别是矿棉的施胶剂或增强纱的施胶剂或者由增强纱得到的毡垫的粘接剂。
10.如前面权利要求中之一项的底材,其特征在于,该无机纤维材料包括保温类矿棉和/或增强类玻璃纱。
11.如前面权利要求中之一项的底材,其特征在于,该纤维材料制成纤网状、毡状、模制壳状、纸张状或是散装材料状。
12.如前面权利要求中之一项的底材,其特征在于,该具有光催化性能的涂层在至少5nm的厚度上,特别是在30~50nm的厚度上覆盖该纤维材料的至少一部分纤维。
13.按照前面权利要求中之一项的底材的制造方法,其特征在于,在纤维材料的生产线上,以液相沉积具有光催化性能涂料,所述沉积尤其在离心盘形成纤装置、外离心成纤装置、机械牵伸成纤装置,空气吹制成纤装置或蒸气吹制成纤装置与接受纤维的装置之间进行,任选在施胶组合物型纤维彼此的液相粘结剂进行沉积之前、之后、同时进行。
14.如权利要求1~12中之一项的底材的制造方法,其特征在于,在纤维材料的生产线上,在由成纤装置出来的纤维的接受装置的下游,特别是在任选的热处理装置/烘箱类热调节装置的前面沉积液相的具有光催化性能的涂料。
15.如权利要求1~12中之一项的底材的制造方法,其特征在于,当将纤维材料转变为最终成品时,特别是当将增强纱毯转变为毡时,在生产线上或在生产线外沉积液相的具有光催化性能的涂料。
16.如权利要求1~12中之一项的底材的制造方法,其特征在于,在最终的纤维材料上沉积液相的具有光催化性能的涂料,然后让所述涂料经受热处理。
17.如权利要求13~16中之一项的方法,其特征在于,通过喷涂、涂布或浸涂的方法沉积呈流体相,特别是液相的涂料。
18.如权利要求1~12中之一项的底材在隔热/隔声材料或在液体或气体的过滤器、提纯器、扩散器等方面的应用,为的是赋予其抗污、杀真菌、杀菌、杀藻或除臭等性能。
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CN1198679A (zh) * | 1995-09-06 | 1998-11-11 | 宇宙航空技术股份有限公司 | 光催化空气消毒 |
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-
1999
- 1999-06-10 US US09/719,153 patent/US7309664B1/en not_active Expired - Fee Related
- 1999-06-10 DE DE69917020T patent/DE69917020T2/de not_active Expired - Lifetime
- 1999-06-10 BR BR9911148-9A patent/BR9911148A/pt unknown
- 1999-06-10 ID IDW20002579A patent/ID28287A/id unknown
- 1999-06-10 AU AU40487/99A patent/AU4048799A/en not_active Abandoned
- 1999-06-10 TR TR2001/00078T patent/TR200100078T2/xx unknown
- 1999-06-10 CA CA002334846A patent/CA2334846A1/fr not_active Abandoned
- 1999-06-10 CN CN99809531A patent/CN1312779A/zh active Pending
- 1999-06-10 JP JP2000553378A patent/JP2002517628A/ja active Pending
- 1999-06-10 WO PCT/FR1999/001375 patent/WO1999064364A1/fr not_active Application Discontinuation
- 1999-06-10 ES ES99923715T patent/ES2221384T3/es not_active Expired - Lifetime
- 1999-06-10 EP EP99923715A patent/EP1084086B1/fr not_active Expired - Lifetime
- 1999-06-10 KR KR1020007014016A patent/KR20010071448A/ko not_active Application Discontinuation
-
2006
- 2006-05-12 US US11/432,322 patent/US7786033B2/en not_active Expired - Fee Related
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2007
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Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
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CN1826296B (zh) * | 2003-07-23 | 2012-11-14 | 法国圣戈班玻璃厂 | 纳入窗玻璃热处理中的光催化涂层的制造方法 |
CN104755109A (zh) * | 2012-09-24 | 2015-07-01 | 光谱系统公司 | 用于自清洁钞票的光催化材料的使用 |
CN108787630A (zh) * | 2012-09-24 | 2018-11-13 | 光谱系统公司 | 用于自清洁钞票的光催化材料的使用 |
CN105102138A (zh) * | 2013-04-08 | 2015-11-25 | 里昂高等师范学院 | 沉积光催化涂层的方法和光催化中的相关涂层、纺织材料以及其用途 |
CN106220122A (zh) * | 2016-06-30 | 2016-12-14 | 浙江大学 | 一种光催化抑菌涂料及其方法 |
CN112295421A (zh) * | 2020-10-20 | 2021-02-02 | 天津理工大学 | 一种表面粘接式用于光催化的TiO2/PVDF超滤膜 |
CN112295421B (zh) * | 2020-10-20 | 2022-11-15 | 天津理工大学 | 一种表面粘接式用于光催化的TiO2/PVDF超滤膜 |
Also Published As
Publication number | Publication date |
---|---|
US7309664B1 (en) | 2007-12-18 |
ID28287A (id) | 2001-05-10 |
DE69917020D1 (de) | 2004-06-09 |
BR9911148A (pt) | 2003-03-05 |
WO1999064364A1 (fr) | 1999-12-16 |
DE69917020T2 (de) | 2005-08-11 |
KR20010071448A (ko) | 2001-07-28 |
US7786033B2 (en) | 2010-08-31 |
AU4048799A (en) | 1999-12-30 |
EP1084086B1 (fr) | 2004-05-06 |
FR2779751A1 (fr) | 1999-12-17 |
JP2002517628A (ja) | 2002-06-18 |
US20080053308A1 (en) | 2008-03-06 |
ES2221384T3 (es) | 2004-12-16 |
FR2779751B1 (fr) | 2003-11-14 |
EP1084086A1 (fr) | 2001-03-21 |
TR200100078T2 (tr) | 2001-05-21 |
US20060205304A1 (en) | 2006-09-14 |
CA2334846A1 (fr) | 1999-12-16 |
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