CN105051253A - 生产具有光催化和杀生物性质的含有经金属、尤其贵金属改性的空间定向二氧化钛纳米管的材料的方法 - Google Patents

生产具有光催化和杀生物性质的含有经金属、尤其贵金属改性的空间定向二氧化钛纳米管的材料的方法 Download PDF

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CN105051253A
CN105051253A CN201380070358.5A CN201380070358A CN105051253A CN 105051253 A CN105051253 A CN 105051253A CN 201380070358 A CN201380070358 A CN 201380070358A CN 105051253 A CN105051253 A CN 105051253A
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metals
hours
production
photocatalytic
weight
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维托尔德·迪特里希
阿德里安娜·扎莱斯卡
安娜·泽林斯卡·尤雷克
安娜·赛布拉
安娜·格拉比哇卡
艾薇丽娜·格拉波瓦卡
乔安娜·瑞兹恩卡
马克·克莱恩
迈克尔·尼斯科
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Phu Dytrych Sp Z O O
Politechnika Gdanska
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Phu Dytrych Sp Z O O
Politechnika Gdanska
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Abstract

本发明涉及生产具有光催化和杀生物性质的含有经金属、尤其贵金属改性的空间定向二氧化钛纳米管的材料的方法。生产具有光催化和杀生物性质的含有经金属、尤其贵金属改性的空间定向二氧化钛纳米管的材料的方法在于使放置在含有氟化铵和乙二醇的电解质中的含有钛(优选地，钛箔)的基底产生感应电流，用超声波清洁所获得的材料并且接着干燥和煅烧，根据本发明其特征在于以下事实：所获得的材料是放置在多组分溶液中，优选地在惰性气体氛围中。多组分溶液必须含有30-50重量％的醇(优选地，异丙醇)，以及一种或数种(优选地，两种或三种)各0.05-5重量％的量的选自包括以下各物的群组的金属的离子和/或纳米分子：银、金、铂、钯、钌、铜、锌、镍、铑、钨、钴、铁，以及水。金属的相互重量比确定在1:1与1:10之间。优选地，多组分溶液在暗室条件中混合3-180分钟，优选地120分钟。然后，其用UV发射灯照射0.5-6小时，在60-100℃的温度下干燥0.5-24小时，有利地6-12小时。

Description

生产具有光催化和杀生物性质的含有经金属、尤其贵金属改性的空间定向二氧化钛纳米管的材料的方法
技术领域
本发明的目标是一种生产具有光催化和杀生物性质的含有经金属、尤其贵金属改性的空间定向二氧化钛纳米管的材料的方法，所述材料可适用于降解气相中的污染物，尤其存在于空气调节系统中，包括汽车系统，例如用于生产空气净化装置。
背景技术
形成具有光催化性质的薄层的已知方法在于使用电泳方法将二氧化钛固定在聚合物基质上、一层导电玻璃、钢瓦、浸渍有二氧化硅的玻璃或钛膜上。
申请案说明书EP2233614描绘了所述电化学法获得二氧化钛纳米管的方法。将上面固定有一层细微的钛的不导电或导电衬底的表面浸没于电解质溶液中。导电衬底充当阴极，而不导电衬底充当阳极。以下物质可以用作衬底：钨、硅、锆、铌、铪、铂、金、钴、钯、镍、玻璃、陶瓷、塑料或聚合物。生产纳米管的方法中所用的电解质可以是氟化铵、乙二醇、水。电解质的温度在5℃与60℃之间变化，而电压在5V与40V之间变化。所获得的纳米管的长度是400nm并且内径是50nm。
专利说明书US008158034B2描绘了生产掺杂有氮的二氧化钛纳米管的方法。TiO2纳米管是在使钛箔在由含氟化铵的乙二醇组成的电解质溶液中阳极氧化的方法中获得。将使用的无源电极是由铂或镍制成并且进行阳极氧化方法5小时。所获得的无定形纳米管在由空气组成的氛围中在400℃的温度中煅烧3小时。然后，二氧化钛纳米管在用等离子体负载的气相物理沉积方法中掺杂有氮。
专利申请案US20120175266(A1)描绘了通过使用电化学法利用离子液体作为电解质生产纳米管的方法。纳米管是通过阳极氧化与含有离子液体(优选地，1-丁基-3-甲基咪唑离子液体)的电解质接触的钛来制成。电解质也可以由多种物质的溶液组成，如水、醇、二醇、质子化胺、腈、砜、酰胺、有机氯化物、碳酸二烷基酯、有机醚、液体烃。强酸和其盐，如HF、KF、LiF、NH4F、HCl、来自KC1、NaCl、NH4Cl的群组的盐、HBr(……)NH4Br、LiNOO3、NaNO3、KNO3、磷酸盐、磷化氢、氯酸盐、溴酸盐，也可以用作电解质。电解质可以含有表面活性剂。纳米管是使用光伏器件或在氢气生成设备中制成并且进行煅烧工艺以增加结晶度。纳米管是在当场阳极氧化过程中和/或在纳米管形成工艺后经掺杂，并且掺合物尤其包括锂离子、钠离子和钾离子以及稀土金属和过渡金属。
发明内容
生产具有光催化和杀生物性质的含有经金属、尤其贵金属改性的空间定向二氧化钛纳米管的材料的方法在于使放置在含有氟化铵和乙二醇的电解质中的含有钛(优选地钛箔)的基底产生感应电流，用超声波清洁所获得的材料并且接着干燥和煅烧，根据本发明其特征在于以下事实：所获得的材料是放置在多组分溶液中，优选地在惰性气体氛围中。多组分溶液必须含有30-50重量％的醇(优选地，异丙醇)，以及一种或数种(优选地，两种或三种)各0.05-5重量％的量的选自包括以下各物的群组的金属的离子和/或纳米分子：银、金、铂、钯、钌、铜、锌、镍、铑、钨、钴、铁，以及水。金属的相互重量比确定在1:1与1:10之间。优选地，多组分溶液在暗室条件中混合3-180分钟，优选地120分钟。然后，其用UV发射灯照射0.5-6小时，在60-100℃的温度下干燥0.5-24小时，有利地6-12小时。
附图说明
无
具体实施方式
在根据本发明的方法的一个实施方案选项中，多组分溶液与如聚乙烯醇和/或乙烯吡咯烷酮的多元醇混合，而所获得的材料在干燥工艺后在250-750℃的温度下进行煅烧。优选地，其在400-450℃的温度下煅烧0.5-6小时，有利地2小时。
在根据本发明的方法的其它实施方案变化形式中，将使用的多组分溶液是由含有选自包括以下各物的群组的一种金属的离子和/或纳米分子的溶液制成：银、金、铂、钯、钌、铜、锌、镍、铑、钨、钴、铁，并且随后混合、曝露和固结工艺是以相同方式进行。然后，将所获得的材料放置在含有选自所述群组的不同金属的离子和/或纳米分子的多组分溶液中。重复混合、曝露和干燥工艺。
本发明版本的特征在于以下事实：所获得的材料是用含有液体烃、表面活性剂、一种或数种(优选地，两种或三种)选自包括以下各物的群组的金属的离子和/或纳米分子的油包水型微乳液覆盖：银、金、铂、钯、钌、铜、锌、镍、铑、钨、钴、铁。金属的相互重量比设定成在1:1到1:10之间，并且随后用含有液体烃、表面活性剂和还原性试剂的油包水型微乳液覆盖，接着在60-100℃的温度下干燥0.5-24小时，有利地6-12小时，并且随后优选在250-750℃、更优选地400-450℃的温度下煅烧0.5-6小时，有利地2小时。
优选地，将使用的液体烃是由环己烷和/或十二烷和/或庚烷和/或癸烷和/或辛烷制成，将使用的表面活性剂是由如对1,1,3,3-四甲基-丁基-苯基-聚乙-二醇醚和/或脱水山梨糖醇单油酸酯、(双-(2-乙基己基)磺基丁二酸钠和/或聚氧基乙基二醇壬基苯基-(9)醚的非离子型或离子型表面活性剂制成，以及将使用的还原性试剂是硼氢化钠和/或肼和/或抗坏血酸。
放置在反应器内部的材料用发射UVA和/或UVB/或UVC射线的灯，优选地利用组合直接激发TiO2粒子的UV发射LED以及可见光的系统照射，其由于LSPR表面等离子体激元的存在直接活化如Ag、Au、Pt的贵金属并且接着所述贵金属将电子传递到上面已经放置所述贵金属的二氧化钛粒子的传导带。
以核-壳型和/或合金结构固定在纳米管表面上的贵金属、双金属、三金属增加材料的光催化活性并且同时使其具有杀生物性质连同除臭性质。使用纳米管自然使得传输光激发电子更有效以及与气相中的污染物接触的表面更大，显著增加污染物降解的效力。
本发明已更详细地呈现在实施实例中。
实例I
一块20cm×30cm尺寸的钢片(钛箔，纯度：99.7％并且厚度：0.127μm)是通过将其连续浸没在丙酮、异丙醇和甲醇中并用超声波处理10分钟来清洁，接着用脱矿质水冲洗并露天干燥。将经清洁的表面放置在乙二醇(98体积％)、水(2体积％)以及氟化铵(0.09M)的溶液中。将溶液放置在由塑料制成的容器中。将基底材料以使其量仅2/3浸没的方式竖直放置在溶液中。将呈铂网形式的电极远离基底材料放置在溶液中。铂网具有在垂直方向上伸长并且围绕基底材料的圆环形式。将两个浸没的电极(铂网和基底材料)连接到供电单元并且接着施加40V电压，同时使铂网以阴极方式而基底材料以阳极方式极化。进行电化学过程60分钟。在所述过程期间，不断地混合溶液。在电化学过程期间，在基底材料的表面上形成直径200nm长度6μm的TiO2纳米管。从溶液中取出基底材料连同在表面上形成的TiO2纳米管的基质，用脱矿质水冲洗并接着放置在脱矿质水中进行超声波5分钟。将所获得的材料在80℃中干燥24小时，并且在450℃的温度下煅烧6小时(使用2℃/min的温度增量)。
然后，将具有纳米管的基底浸没在含有0.2MAgNO3以及0.05MHAuCl4的水和异丙醇(1:1)溶液中；通过通入氩气30分钟去除空气并且接着混合溶液30分钟，随后用发射UV-Vis范围的射线的500W汞灯照射2小时。在80℃的温度下干燥样品2小时。
将含有经双金属纳米粒子(具有合金结构的Au/Ag并且尺寸是10到20nm)改性的TiO2纳米管的材料放入反应器中以便在气相期间降解污染物，并且用组合的直接激发TiO2粒子的UV发射LED以及由于表面等离子体激元的存在激发贵金属粒子的Vis发射LED的系统照射，并使其通过二氧化钛粒子以降解有机污染物。反应器中的最小湿度是40％。在材料曝露1小时后，气相中99％的甲苯(初始浓度：200ppm)降解。在60分钟后针对酿酒酵母(S.cerevisiae)真菌的杀生物活性是80％。
第1项.用直径200nm的纳米管覆盖的钛钢片的SEM图像
实例II
将如实例I中所说明而获得的覆盖有二氧化钛纳米管的基底浸没在45V施加电压下含有甘油(55％v/v)、水(45％v/v)和氟化铵(0.27M)的混合物中。将所获得的直径220nm的纳米管放置在含有0.1％molPt(IV)离子以及0.5％molAu(III)离子的水-0.2MAOT-环己烷微乳液中。将含有N2H4作为还原剂(1.2％mol的量)的第二水-0.2MAOT-环己烷微乳液引入系统。然后，将光催化层在60℃的温度下干燥12小时并且在400℃的温度下煅烧3小时。将含有经核-多孔壳型双金属Au/Pt纳米粒子改性的TiO2纳米管的材料放置在反应器中并用375nm波长的UV光照射。甲苯降解效力(初始浓度：200ppm)在四个后续曝露循环(每一曝露循环60分钟)中分别是98％、99％、99％和100％。
实例III
将如实例I中所说明而获得的覆盖有二氧化钛纳米管的基底浸没在含有氯铂酸(0.05M)、硝酸铜(II)(0.01M)以及硝酸银(I)(0.05M)的甲醇(10重量％)和异丙醇(30重量％)的水溶液中；所述溶液的pH值是5。接着通过通入氩气30分钟从溶液去除空气；将溶液混合120分钟以便使金属离子吸附在纳米管的表面上，并且用300-400nm波长的射线照射60分钟。在80℃的温度下干燥所获得的材料2小时。
将含有经三金属(Pt/Cu/Ag)纳米粒子改性的TiO2纳米管的光催化材料放置在反应器中以便在气相期间降解污染物，并且使用由LED(15个LED，直径：5mm，光照角度：30度，波长：375nm和10个LED，直径：5mm，光照角度：30度，波长：415m，通过单个LED收集的功率：约63mW，通过LED组收集的功率：约1.6W)组成的光源照射。在35分钟曝露后，降解99％甲苯以及95％大肠杆菌(E.Coli)。
实例IV
将如实例I中所说明而获得的覆盖有二氧化钛纳米管的基底浸没在含有Pt(II)离子(0.1M)的异丙醇(30重量％)的水溶液中，接着通过通入氩气30分钟去除空气；将溶液混合20分钟并用300-400nm波长范围的射线照射60分钟。将所获得的材料放置在含有Pd(II)离子(0.1M)的异丙醇(30重量％)的水溶液中，通过通入氩气30分钟从溶液去除空气；将溶液混合20分钟并用300-400nm波长的射线照射60分钟。将所获得的材料在80℃的温度下固结2小时。
将含有经铂以及5到10nm尺寸的钯纳米粒子改性的TiO2纳米管的光催化材料放置在反应器中，以便在气相期间使用由LED(15个LED，直径：5mm，光照角度：30度，波长：375nm和10个LED，直径：5mm，光照角度：30度，波长：415m，通过单个LED收集的功率：约63mW，通过LED组收集的功率：约1.6W)组成的光源降解污染物。在30分钟曝露后，降解98％甲苯以及97％降解大肠杆菌。

Claims (3)

1.一种生产具有光催化和杀生物性质的含有经金属、尤其贵金属改性的空间定向二氧化钛纳米管的材料的方法，所述方法在于使放置在含有氟化铵和乙二醇的电解质中的含有钛、优选地钛箔的基底产生感应电流，用超声波清洁所获得的材料并且接着干燥和煅烧，其特征在于以下事实：所获得的材料优选地在惰性气体氛围中，在含有30到50重量％的醇、优选地异丙醇以及一种或数种、优选地两种或三种各0.05到5重量％的量的选自包括以下各物的群组的金属的离子和/或纳米分子：银、金、铂、钯、钌、铜、锌、镍、铑、钨、钴、铁的多组分溶液中，使得所述金属的相互重量比是1:1到1:10，以及考虑到所述多组分溶液在暗室条件中混合3到180分钟、优选地120分钟，并且随后使用UV发射灯进行照射0.5到6小时，考虑到所获得的材料在60到100℃的温度下干燥0.5到24小时、有利地6到12小时。
2.根据权利要求1所述的方法，其特征在于以下事实：所述多组分溶液与如聚乙烯醇和/或乙烯吡咯烷酮的多元醇混合，而所获得的材料在干燥工艺后在250到750℃、更优选地400到450℃的温度下进行煅烧0.5到6小时、有利地2小时。
3.根据权利要求1所述的方法，其特征在于以下事实：将使用的所述多组分溶液是由含有的溶液制成
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