CN109988451A - 一种自清洁预制构件的光催化施工工艺及检测方法 - Google Patents
一种自清洁预制构件的光催化施工工艺及检测方法 Download PDFInfo
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- CN109988451A CN109988451A CN201910284748.1A CN201910284748A CN109988451A CN 109988451 A CN109988451 A CN 109988451A CN 201910284748 A CN201910284748 A CN 201910284748A CN 109988451 A CN109988451 A CN 109988451A
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Abstract
本发明提出一种自清洁预制构件的光催化施工工艺,拟由纳米光催化剂与装配式预制构件相结合,有效地将光催化材料的功能体现在室内外表面的建筑材料中,不仅可作为建筑结构材料也可作为功能材料使用,在应用方面实现改善室内外环境安全性、舒适度和提升建筑节能的效果,使其向功能化、生态化和无害化的方向发展。同时,在其开发过程中,采用绿色建筑节能措施,减少能源和资源的使用,打造生态、可持续的绿色开发环境。
Description
技术领域
本发明涉及光催化领域,尤其涉及一种自清洁预制构件的光催化施工工艺及检测方法。
背景技术
在我国,建筑本身就是能源消耗大户,同时对环境也有重大影响。我国处在经济快速发展时期,人们对高水平的生活的追求越也来越强烈,这种消费升级使得人们对建筑的要求越来越高,人均耗能也越来越高,产生的建筑废弃物越来越多,对环境的污染也不可小觑。同时,随着经济的发展,城市大气污染状况日益严重,汽车和工业排放的氮氧化物和硫化物等对大气污染影响率急剧上升,我国有的城市NOx己达50%以上。这与全球倡导的保护环境的理念相违背。近年来,许多研究表明,光催化技术在环境污染物治理方面有着良好的应用前景,纳米光催化剂在紫外光照射下,以多种建筑材料为载体,如应用于油漆、玻璃、瓷砖、石膏制品和混凝土等基体材料上,利用其具有良好的光催化氧化能力和表面超亲水性能,实现氧化分解大气污染物,可将有机污染物分解成CO2、H2O等小分子物质、抑菌抗菌、防霉、防污、防露、防雾等多种目的,玻璃窗和瓷砖通过添加纳米光催化剂作为光催化薄膜,使得它们的自清洁功能得到改性,其已经应用于中国国家歌剧院的玻璃表面。纳米光催化剂也被添加在混凝土中或用作涂料涂刷在清水混凝土等装饰性混凝土表面,既可以维持建筑材料的本身审美外观,又可以完善空气质量,改善大气环境,保持城市清洁,由于其具有自清洁性能,也可以节省维护成本,从而延长建筑物自身的使用寿命。
催化剂是加速化学反应的化学物质,其本身并不参与反应。光催化剂就是在光子的激发下能够起到催化作用的化学物质的统称。光催化技术是在20世纪70年代诞生的基础纳米技术,在中国大陆我们会用光触媒这个通俗词来称呼光催化剂。典型的天然光催化剂就是我们常见的汁绿素,在植物的光合作用中促进空气中的二氧化碳和水合成为氧气和碳水化合物。总的来说纳米光触媒技术是一种纳米仿生技术,用于环境净化,自清洁材料,先进新能源,癌症医疗,高效率抗菌等多个前沿领域。
世界上能作为光触媒的材料众多,包括二氧化钛(TiO2),氧化锌(ZnO),氧化锡(SnO2),二氧化锆(ZrO2),硫化镉(CdS)等多种氧化物硫化物半导体,二氧化钛(TiO2),因其氧化能力强,化学性质稳定无毒,成为世界上最当红的纳米允触媒材料。在早期,也曾经较多使用氧化锌(ZnO)和硫化镉(CdS)做为光触媒材料,但是由于这两者的化学性质不稳定,会在光催化的同时发生光溶解,溶出有害的金属离子具有一定的生物毒性,故发达国家目前已经很少将它应用作为民用光催化材料。
发明内容
本发明提出一种自清洁预制构件的光催化施工工艺及检测方法,研究出一种适合于工业生产的纳米光催化剂,与装配式预制构件相结合,有效地将光催化材料的功能体现在室内外表面的建筑材料中,不仅可作为建筑结构材料也可作为功能材料使用。
本发明是通过以下技术方案实现:
首先,以金属盐作为金属源,采用水热或水浴合成法,通过调节其反应条件(温度,时间以及浓度等),制得具有不同性质的金属氧化物或多金属复合物。利用XRD、XPS、UV-vis、SEM(FESEM)、TEM等测试手段对所制备样品的组分、形貌结构和光学性质等方面进行表征,并通过光催化性能测试比较分析研究了不同样品的光催化性能,研究其作用机制。
其次,取得一定量纳米光催化剂,通过物理共混、插层、原位聚合和溶胶-凝胶法等方法,均匀分散在传统有机涂料中,形成改性纳米复合涂料。通过测试其紫外-可见吸收光谱图来判断改性涂料的光催化性能。
最后,将配置成一定浓度含有纳米光催化剂的改性涂料浆液喷涂于混凝土预制构件表层,制得纳米涂层。通过涂料涂层耐沾污性试验和涂料涂层耐老化性试验来测定纳米光催化剂对涂料耐沾污性能和耐老化性能的影响。
本发明拟由纳米光催化剂与装配式预制构件相结合,有效地将光催化材料的功能体现在室内外表面的建筑材料中,不仅可作为建筑结构材料也可作为功能材料使用,在应用方面实现改善室内外环境安全性、舒适度和提升建筑节能的效果,使其向功能化、生态化和无害化的方向发展。同时,在其开发过程中,采用绿色建筑节能措施,减少能源和资源的使用,打造生态、可持续的绿色开发环境。相对其他光催化剂来说,本发明中的SnO2和BiOCl无毒无刺激性,反应条件相对温和,能耗低,光催化反应速度快,催化活性高,氧化能力强,无二次污染,是非常有应用前景的绿色光催化剂。
附图说明
图1为本发明中SnO2样品和商业化SnO2在光催化降解有色染料RhB和MB方面的性能对比图。
具体实施方式
为了使本发明的目的、技术方案及优点更加清楚明白,以下结合附图及实施例,对本发明进行进一步详细说明。应当理解,此处所描述的具体实施例仅仅用以解释本发明,并不用于限定本发明。
半导体具有区别于金属或绝缘物质的特别的能带结构。在具有一定能量的光子激发下(光子激发原理参考光触媒反应原理)能使分子轨道中的电子离开价带跃迁至导带,从而在材料价带形成光生空穴,在导带形成光生电子[e-],在体相二氧化钛中由于二氧化钛颗粒很大,光生电子在到达导带开始向颗粒表面活动的过程中很容易与光生空穴复合,从而从宏观上我们无法观察到光子激发的效果:但是纳米的二氧化钛颗粒日于尺寸很小,所以电子比较容易扩散到晶体表面,导致原本不带电的晶体表面的2个不同部分出现了极性相反的2个微区——光生电子和光生空穴。由于光生电子和光生空穴都有很强的能量,远远高出一般有机污染物的分子链的强度,所以可以轻易将有机污染物分解成最原始的状态。同时光生空穴还能与空气中的水分子形成反应,产生氢氧自由基亦可分解有机污染物并且杀灭细菌病毒。
在半导体材料中,二氧化锡是一种禁带宽N型半导体(Eg=3.6ev,300K),本征Sn02材料电阻很大,在合成过程中会存在氧空位因为氧不足,二氧化锡是四方晶系金红石结构,届于P42/mnm空间群,晶胞参数分别是a=4.737,c=3.186,c/a=0.673,每个晶胞内有两个二氧化锡分子,二氧化锡有对称性比较好的非极性结构,本身不具有各向异性生长习性,完美的二氧化锡是绝缘体,而晶态二氧化锡都含有间隙原子和有氧空位,所以通常情况下二氧化锡呈现N型半导体特性。每个Sn原子在六个O原子组成的八面体中心,而且由三个Sn原子组成的等边三角形中心存在一个O原子,呈现6:3的配位结构。各表面能量的大小各不相同,而差异比较小,尽管晶面能量最髙,而c/a=0.673使其在c轴生长成长径比大的一维纳米结构带来困难,外部的环境参数在很大程度上改变了二氧化锡晶体的形貌生成。
本发明中采用醇热法制备二氧化锡纳米粒子。
将氯化亚锡晶体超声溶解于叔丁醇中,形成质量浓度为100-120g/L的溶液,取所述溶液10mL,向其中加入5.OOmL甘油和2.25mL环己烷,搅拌至溶液澄淸透明,装釜,放入200℃烘箱反应8h。自然冷却至室温,用去离子水和乙醉反复洗涤,离心,80℃真空烘干,500℃焙烧4h,即可得到样品2(Sample2)。以控制变量法分别制得其他样品,标记为样品1(Sample1,醇剂为1.OOmL甘油)样品3(Sample3,醇剂为5.OOmL乙二醇)。
上述500℃焙烧时升温速率均为2℃·min-1。
本发明中利用XPS、XRD、XPS、UV-vis、SEM(FESEM)、TEM等测试手段对所制备样品的组分、形貌结构和光学性质等方面进行表征,并通过光催化性能测试比较分析研究了不同样品的光催化性能,研究其作用机制,均得出样品2展现出优异的催化性能。
其中,
XPS:X射线光电子能谱,利用Perkin Elmer公司出产的PHI 5000ESCA X射线光电子能谱仪,激发源为AlKα(1486.6eV)射线,高压14.0kV,功率250W,X射线与样品夹角θ=54°,测童时分析室压力为10-9Torr,以Cls的结合能(284.6eV)为基准进行校正;
XRD:X射线粉末衍射,采用Rigacu公司D 2000型X射线衍射仪进行样品的物相分析,使用Cu Kα辐射为射线源(X=1.54A),石墨单色器,管压40KV,管流20-30mA,扫描速率为1.2°/min;
UV-vis:紫外可见漫反射,在岛津UV-2450型分光光度计上进行,扫描范围200-800nm,以高纯BaS04为标准试剂;
FESEM:场发射扫描电镜,采用日本HITACHI公司生产的S 4800型冷场发射扫描电子显微镜,工作电压为3.0KV;
TEM:透射电镜,采用日本JEM 2010型透射电子显微镜,测试前样品经仔细研磨,并在乙醇中进行超声处理。
虽然所制备样品SnO2在可见光区有部分吸收,但不是很强,光利用率仍不是很高,故这里采用全谱的300W氙灯(λ>200nm)照射激发。为了说明所制SnO2样品在光催化降解有色染料RhB和MB方面的优异性能,我们选取了商业化的SnO2作为对比。如图1(a)所示,在光催化降解RhB时,相比于商业化SnO2及自制其他样品,样品2活性最佳,经4h光催化反应,RhB降解率达60%。降解MB时类似规律如图1(b)所示,样品2仍表现出最佳活性,经4h光催化反应,MB去除率高达96%。从图1(c)可看出,降解RhB时,该反应近似为—级反应,其中速率常数根据计算得出如下规律:
kRhB-Sample2(0.2168h-1)>kRhB-Sample3(0.1874h-1)>kRhB-Sample1(0.1342h-1)>kRhB-Commercial(0.07654h-1)。同样地,在降解MB时候,也得到类似的规律,如图1(d)所示。根据计算,
kMB-Sample2(0.8217h-1)>kMB-Sample3(0.5940h-1)>kMB-Sample1(0.4497h-1)>kMB-Commercial(0.3490h-1)。通过以上数据分析得出无论降解RhB还是MB,自研发的SnO2活性及降解速率均高于于商业化Sn02,同时相比较其他样品,样品2表现出最佳的催化效果。这可归因于以下几点:1)样品2具有较高的结晶度:2)具有较大的比表面积,有利于对底物的吸附:3)较大的孔容孔径,有利于传质;4)较强的光吸收,较高的光利用率。
由此得出,本实施例通过用醇热法制备的SnO2纳米粒子,通过调变相关溶剂的种类和量,控制生成SnO2的生长,基本实现尺寸可控,分散均匀。其中在含有5mL甘油体系下合成的Sn02,由于其较高的结晶度,较大的比表面积以及较高的光利用率,进而呈现最佳的光电催化及光催化性能。阳极极化曲线测试表明,在同等条件下,样品2具有较高的电流密度,进而呈现较优的光电催化性能:光催化测试表明,样品2呈现最佳的催化性能,经4h光催化反应,RhB及MB降解率分别达60%。该法所制备的SnO2纳米粒子在环境催化净化及光电转换方面均具有良好的应用前景。
本发明还提供了一种金属复合物的生产方法。
室温条件下,将240-250g五水合硝酸铋溶解于10L乙二醇中,边搅拌边加入110g氯化亚锡晶体,待溶液澄清后,加入30L乙醇,继续搅拌30min后移入50L反应釜中,于160℃条件下醇热24h,然后经由乙醇洗涤,80℃烘干,500℃焙烧(升温速率为2℃·min-1)4h后制得SnO2/BiOCl复合物。
由于Bi的独特电子结构有利于光生载流子的迁移,铋氧氧化物(BiOX,X=Cl,Br,I)能很好的充当助催化剂的角色(它们是四方相结构,在两个X层之间是(Bi202)2+层,而每个[Bi2O2]X2由5个原子组成,使每个0、X、Bi分别组成一个OBi4四面体,XBi4四角锥和Bi04X4正四角反棱柱。正是由于这种特殊结构,人们发现,光在半透明的BiOX片之间反射并且成倍的增长,粘连的各项异性同样说明除了层的边缘之外没有其他的自由基,且光激发反射不能破坏O-Bi-X,表现出良好的光稳定性。
将上述复合样品利用透射电镜观察,可以清晰的看到,复合物是球状物质,明暗的变化表明其极有可能是微孔结构。样品的微观结构进一步的用高分辨电镜进行观察,SnO2和BiOCl均表现出了清晰的晶格条纹,显示其结晶性质。SiO2纳米颗粒的晶格间距是0.25nm,与四方相的SnO2某一面的晶格间距保持一致;而0.35nm相当于四方相BiOCl表面的晶格间距。即使在超声后,SnO2纳米粒子与BiOCl纳米粒子依然紧紧的粘合在一起,高分辨电镜图清晰的显示在两类不同的晶体接触面形成了牢固的结(异质结),其使得SnO2和BiOCl常牢固的结合成异质结复合型光催化剂,同时所形成的异质结也使界面电子传递更为流畅有效,极大地提高了光催化活性。
复合光催化剂的催化活性的提高是因为复合使得有效催化面积提高了,并且两个半导体的偶合效应也有助于活性的增加。一方面,复合物的比表面积增大有助于提高光催化反应区域。此外,多孔的结构有利于光生载流子从表面到有机分子的传递,并且使得其在反应中的反应物和产物之间得到迅速的扩散。另一方面,众所周知光催化过程依赖于载流子的产生和分离。影响光催化活性的因素一般有电子,空穴,羟基自由基和氧自由基。在光照条件下,光催化剂分散于空气或被污染的水中,价带上的空穴和导带上的电子产生,这些电子-空穴对和基底相互作用,价带的空穴和催化剂表面的水或者氢氧根反应形成羧基自由基,同时,价带的空穴也能氧化有机分子,导带的电子减少氧分子来形成超氧自由基。将上述氧化物或复合物催化机与有机涂料复合,使样品均匀分散在传统有机涂料中,形成改性纳米复合涂料,通过测试其紫外-可见吸收光谱图来判断改性涂料的光催化性能;样品与有机涂料复合方法包括物理共混、插层、原位聚合和溶胶-凝胶法,一般采用物理共混法,物理共混法是将纳米粉体经表面处理或预制成稳定分散的浆料,直接分散于有机成膜物中,是将纳米结构材料引入多元体系涂料中,各组分协同作用,以改进涂料性能。
将所得改性纳米复合涂料喷涂于混凝土预制构件表层,形成纳米涂层;通过涂料涂层耐沾污性试验和涂料涂层耐老化性试验(国际标准号:ASTM D3719:2000)来测定纳米光催化剂对涂料耐沾污性能和耐老化性能的影响。
纳米光催化剂在紫外光照射下,以多种建筑材料为载体,利用其具有良好的光催化氧化能力和表面超亲水性能,实现氧化分解大气污染物,抑菌抗菌、防霉、防污、防露、防雾等多种目的。纳米光催化剂被添加在混凝土中或用作涂料涂刷在清水混凝土等装饰性混凝土表面,既可以维持建筑材料的本身审美外观,又可以完善空气质量,改善大气环境,保持城市清洁,可以节省维护成本,从而延长建筑物自身的使用寿命,达到良好的经济与社会效益。
以上所述仅为本发明的较佳实施例而已,并不用以限制本发明,凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等,均应包含在本发明的保护范围之内。
Claims (6)
1.一种自清洁预制构件的光催化施工工艺及检测方法,包括如下步骤:
(1)以金属盐作为金属源,采用水热或水浴合成法,通过调节其反应条件,制得具有不同性质的金属氧化物或多金属复合物样品;
(2)对步骤(1)所制备样品的组分、形貌结构和光学性质方面进行表征,并通过光催化性能测试比较分析研究了不同样品的光催化性能,研究其作用机制,并做记录;
(3)将步骤(1)所制备样品分别与有机涂料复合,使样品均匀分散在传统有机涂料中,形成改性纳米复合涂料,通过测试其紫外-可见吸收光谱图来判断改性涂料的光催化性能;
(4)将步骤(3)中所得改性纳米复合涂料喷涂于混凝土预制构件表层,形成纳米涂层;通过涂料涂层耐沾污性试验和涂料涂层耐老化性试验来测定纳米光催化剂对涂料耐沾污性能和耐老化性能的影响。
2.根据权利要求1所述的一种自清洁预制构件的光催化施工工艺及检测方法,其特征在于,步骤(1)中所述金属氧化物样品的一种制备方法如下:
将氯化亚锡晶体超声溶解于叔丁醇中,形成质量浓度为100-120g/L的溶液,取所述溶液10L向其中加入5L甘油和2.25L环乙烷,搅拌至溶液澄清透明,装釜,放入200℃烘箱中反应18h;自然冷却至室温,用去离子水和乙醇反复洗涤并离心,然后在80℃条件下真空烘干,将烘干所得于500℃下焙烧4h制得二氧化锡。
3.根据权利要求1所述的一种自清洁预制构件的光催化施工工艺及检测方法,其特征在于,步骤(1)中所述金属复合物样品的一种制备方法如下:
室温条件下,将240-250g五水合硝酸铋溶解于10L乙二醇中,边搅拌边加入110g氯化亚锡晶体,待溶液澄清后,加入30L乙醇,继续搅拌30min后移入50L反应釜中,于160℃条件下醇热24h,然后经由乙醇洗涤,80℃烘干,500℃焙烧4h后制得SnO2/BiOCl复合物。
4.根据权利要求2或3所述的一种自清洁预制构件的光催化施工工艺及检测方法,其特征在于,500℃焙烧时升温速率为2℃·min-1。
5.根据权利要求1所述的一种自清洁预制构件的光催化施工工艺及检测方法,其特征在于,所述步骤(3)中样品与有机涂料复合方法包括物理共混、插层、原位聚合和溶胶-凝胶法。
6.根据权利要求1所述的一种自清洁预制构件的光催化施工工艺及检测方法,其特征在于,所述步骤(2)中对所制备样品的组分、形貌结构和光学性质方面进行表征时采用方法包括XPS、XRD、UV-vis、SEM、TEM。
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