CN101378993B - 制备TiO2纳米颗粒水性分散液的方法以及由此所得分散液 - Google Patents
制备TiO2纳米颗粒水性分散液的方法以及由此所得分散液 Download PDFInfo
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Abstract
本发明涉及制备锐钛矿型TiO2水性分散液的方法,以及这样所得的分散液,制备表面光催化涂层的用途以及气体和液体光催化净化中的用途。
Description
技术领域:
本发明设计制备纳米颗粒化合物的方法,特别是制备TiO2纳米颗粒分散液。
背景技术:
二氧化钛是一种白色颜料,其具有很强的遮盖力,被用于颜料以及造纸和合成橡胶。现在二氧化钛主要应用是突出利用其光催化性能,换句话说,通过紫外光作用,利用这一特性来形成可以催化氧化降解有害或有毒物质(例如苯、二噁英和其他有机污染物)以及令人厌恶和致病的物质(例如霉菌、细菌)的自由基。这样的应用因而广泛用于环境领域,例如防污染,清洁剂以及卫生制品。
对于这些应用,二氧化钛被用作将被处理的表面的涂层材料以最大化光催化效果。最广泛用于这种用途的二氧化钛的晶型称之为“锐钛矿型”,这是因为其化学稳定且易得,以及其光催化能力高于另外两种晶型(金红石型和板钛矿型)。
另一方面,二氧化钛吸收光谱重叠(即使是锐钛矿型)对于太阳光谱不是很大,这使得低光催化效率。基于这个原因,不同的尝试试图改性TiO2,例如,将其掺杂其它金属或者制备纳米颗粒化合物;事实上,这显著增加表面面积以及光催化效果。
一些已知的制备锐钛矿型TiO2(包括纳米颗粒型)的方法提供粉末状TiO2。为了适于制备光催化涂层,这个粉末必须分散在适当的溶剂中并与其它可能的添加剂复配以改善涂层粘性,但是这导致二氧化钛颗粒凝聚而无法保持光催化效果和能力。此外,经过一段时间,在这些分散液中的TiO2颗粒会沉在容置该分散液的容器底部,导致储存中的稳定性问题。
另外,本申请人的专利申请No.FI2004A252描述了一种方法可以制备稳定的锐钛矿型二氧化钛纳米分散液,其中水和适当的络合溶剂被用作溶剂。
发明内容:
申请人发明一种方法用于获得已经仅分散在水中的锐钛矿型二氧化钛纳米颗粒,直接用于制备光催化涂层。基于本发明方法所得分散液不会引起颗粒凝聚,即使经过长期储存,基于分散液的同源性可以制备保持颗粒材料光催化活性的涂层。
因而本发明的目的在于制备锐钛矿型二氧化钛纳米颗粒水分散液,其中钛醇盐被用于在加热下在水中以及无机酸和非离子表面活性剂存在下反应,如果需要时溶液最终被缩减到很小体积。本发明进一步目的在于使用本方法获得的锐钛矿型二氧化钛纳米颗粒水分散液的用途,及其用于制备光催化表面涂层,用于光催化净化气体和液体,用于制备具有防太阳光的人肌肤用化妆品。
本发明的特点和优点将在随后的描述中展示。
附图说明:
图1显示干燥产物粉末的衍射图,其中Y轴显示辐射密度,X轴显示入射角振幅。这份分析显示本发明所得锐钛矿型二氧化钛的晶型。
具体实施方式:
本发明的方法可以直接在水中制备锐钛矿型TiO2,进而在工艺终端获得尺寸为30-50nm的TiO2颗粒。颗粒的测量方法是现有技术已知的,例如XRD(X-射线衍射)、FEG-SEM(场发射枪-扫描电子显微镜)、TEM(透射电子显微镜)以及DLS(动态光散射)。不同于将纳米粉末分散在溶剂混合物或水中所制备的,这些分散液显示出没有明显的聚集或凝聚以及固体沉淀,即使长期储存分散液。
这种分散液的优点是明显的相应的光催化性以及均匀涂层可以由这种分散液制得。基于本发明所得的分散指数低于0.3(DLS法测得),因而基于本发明的分散液不同于现有技术通过纳米颗粒粉末分散于溶剂中所得的分散液。
在这个方法中用作初始产物的钛醇盐可以选自甲醇钛、乙醇钛、正丙醇钛、异丙醇钛、正丁醇钛和异丁醇钛。
特别优选为异丙醇钛,这是因为其便宜并且在本发明方法条件下反应最好。
非离子表面活性剂选自由非极性部分和极性官能团、非离子化醚、酯、醚-酯组成的表面活性剂;特别优选为曲拉通X-100(TX-100)。
基于本发明的无机酸是指例如盐酸、硝酸、硫酸、高氯酸、氢溴酸和碘化氢;优选卤素酸,特别优选盐酸。
钛醇盐/无机酸的醇化物摩尔比为0.005-15,优选为5-6。
反应温度为15℃-95℃,优选45℃-55℃。
反应时间为12-72小时,优选24小时。
在必要时,当用于制备涂层,本分散液可以与表面涂层领域常用添加剂和稀释剂复配(例如粘性改进剂或溶剂例如水或乙醇)以获得所需的稀释水平。
另一方面,当用于净化液体或气体产物,本分散液被吸附在硅胶上或其它适宜的具有吸附特性的无机载体上,然后浸没在液体中,或(以当前状态或稀释)置于将要净化的气体的容器中通过冲洗起泡。
表面有本分散液制成涂层的载体应用很广泛,从纺织纤维产物到成衣或陶瓷以及在玻璃、金属、镜子等类似材料中的载体。
基于本发明的表面涂层的光催化活性是指将涂层暴露于适当波长(典型为388nm)光线的结果,当暴露于紫外线后形成具有抗菌、抑菌和超亲水特性的表面。事实上涂有TiO2的载体显示出缺少斥水性,称为超亲水性,使得TiO2处理的表面可以自我清洁。
此外,由于TiO2颗粒的尺寸极小,本分散液是透明的,使得其所施用的表面可见,而无改变。这个透明性也使得产品适用于化妆品领域已制备具有高防紫外线水平的防晒品。
本分散液的另一优点是其高温性能。事实上,将表面涂层施用于陶瓷载体需要高温处理载体,而本分散液保持相同的外观、锐钛矿型晶型以及纳米颗粒特性,如同加热前一样。
基于本方法的特定实施例,通过添加金属盐到初始溶液中,Ti可以被掺杂有过渡金属,特别是Ag、Cu和Ce。在这个情况下,本方法形成的掺杂有Ag、Cu或Ce的TiO2分散液可以在没有紫外线的情况下表现出催化活性。
下面是本发明的一些特定实施例,用于示范而非限定。
例如5克浓HCl,7.5克TX-100,加水到总重750克,被置于2L反应器中,通过外套油循环热透加热。温度提升到50℃。在这一点迅速加入50g Ti[OCH(CH3)2]4(TIP),可以立即看到白色絮状沉淀。
7小时后得到非常稳定的透明溶胶。
表征
通过确定溶液中二氧化钛浓度(ICP技术)以及颗粒尺寸(DLS技术)进行表征。
浓度:1.5%TiO2(重量比)
尺寸:36.67nm,多分散性指数=0.282
例2
5g浓HCl,7.5g TX-100,加水至总重750g,置于2L反应器中,通过外套油循环热透加热。温度提升到50℃。在这一点迅速加入50gTIP,可以立即看到白色絮状沉淀。
24小时后得到非常稳定的透明溶胶。
表征
浓度:1.45%TiO2(重量比)
尺寸:30.26nm,多分散性指数=0.216
例3
500cc通过水解02合成所得产物被置于旋转蒸发仪中浓缩。浴被加热到40℃。油动力真空泵为浴制造真空。
得到110cc溶液。
表征
浓度:6.69%TiO2(重量比)
尺寸:26.72nm with a,多分散性指数=0.269
例4
5g浓HCl,1.0g TX-100,加水至总重936g,置于2L反应器中,通过外套油循环热透加热。温度提升到50℃。
在这一点迅速加入64g TIP,立即可见白色絮状沉淀。
24小时后得到非常稳定的透明溶胶。
表征
浓度:1.8%TiO2(重量比)
尺寸:49.62nm,多分散性指数=0.246
例5
5g浓HCl,加水至总重936g,置于2L反应器中,通过外套油循环热透加热。温度提升到50℃。在这一点迅速加入64g TIP,立即看到白色絮状沉淀。
24小时后得到非常稳定的透明溶胶。
表征
浓度:1.8%TiO2(重量比)
尺寸:52.71nm,多分散性指数=0.286
例6
将TiO
2
纳米颗粒水分散液应用于纤维上
例1-5所得悬浮液可用于处理纤维并使得他们吸收对皮肤有害的紫外线,降低皮肤癌的风险。
15Kg的0.5M乙酸钠溶液和0.5Kg的Pimasil(硅氧烷树脂)被添加到13Kg水中制备并浓缩到6%的产品。所得混合物通过填料技术施用到纤维上然后进行在热定型和染色过程中机器在有横向张力的状态下加工织物干燥。这样所得的纤维的UPF值是同样类型当未被处理的纤维的20倍。
例7
将TiO
2
纳米颗粒水分散液应用于陶瓷或玻璃表面
例1-5所得悬浮液被施用于陶瓷或玻璃表面(使用喷雾或浸渍涂布技术),以初始浓度或被稀释(用水或醇)。所得表面保持其初始特性,这是因为施用的这一层是完全透明的。表面具有完全的光催化功能:自清洁、抗菌、降解有机污染物。
Claims (26)
1.制备锐钛矿型TiO2纳米颗粒分散液的方法,其中钛醇盐在加热条件下以及存在无机酸和非离子表面活性剂情况下在水中反应,所得溶液可按需缩减到较小体积,所述无机酸选自盐酸、硝酸、硫酸、高氯酸、氢溴酸和碘化氢,所述非离子表面活性剂具有酯或醚类极性官能团。
2.如权利要求1所述的方法,其中所述钛醇盐选自甲醇钛、乙醇钛、正丙醇钛、异丙醇钛、正丁醇钛、异丁醇钛。
3.如权利要求2所述的方法,其中所述钛醇盐是异丙醇钛。
4.如权利要求1-3任一所述的方法,其中所述无机酸是卤素酸。
5.如权利要求4所述的方法,其中所述卤素酸是HCl。
6.如权利要求1所述的方法,其中所述非离子表面活性剂是曲拉通X-100(TX-100)。
7.如权利要求4所述的方法,其中钛醇盐/卤素酸摩尔比是0.005-15。
8.如权利要求7所述的方法,其中钛醇盐/卤素酸摩尔比是5-6。
9.如权利要求1所述的方法,其中反应温度为15℃-95℃,反应时间为12-72小时。
10.如权利要求9所述的方法,其中反应温度为45℃-55℃,反应时间为24小时。
11.如权利要求1所述的方法,其中Ag或Cu或Ce金属盐被添加到含有钛醇盐、无机酸和表面活性剂的溶液中。
12.锐钛矿型TiO2纳米颗粒水分散液,由权利要求1-11任一所述方法所得。
13.TiO2纳米颗粒水分散液,其中Ti掺杂有选自过渡金属的金属,由权利要求11所述方法而得。
14.如权利要求13所述的分散液,其中所述过渡金属选自Ag、Cu和Ce。
15.基于权利要求12所述的TiO2纳米颗粒分散液的用途,用于制备在所需表面上的光催化涂层。
16.基于权利要求13所述的TiO2纳米颗粒分散液的用途,用于制备在所需表面上的光催化涂层。
17.基于权利要求14所述的TiO2纳米颗粒分散液的用途,用于制备在所需表面上的光催化涂层。
18.如权利要求15所述的用途,其中所述表面选自纺织纤维表面、金属表面、陶瓷表面和搪瓷制品表面。
19.如权利要求16所述的用途,其中所述表面选自纺织纤维表面、金属表面、陶瓷表面和搪瓷制品表面。
20.如权利要求17所述的用途,其中所述表面选自纺织纤维表面、金属表面、陶瓷表面和搪瓷制品表面。
21.基于权利要求12所述TiO2的纳米颗粒分散液的用途,用于光催化净化气体和液体。
22.基于权利要求13所述TiO2的纳米颗粒分散液的用途,用于光催化净化气体和液体。
23.基于权利要求14所述TiO2的纳米颗粒分散液的用途,用于光催化净化气体和液体。
24.基于权利要求12所述TiO2的纳米颗粒分散液的用途,用于制备具有人肌肤防太阳光功能的化妆品。
25.基于权利要求13所述TiO2的纳米颗粒分散液的用途,用于制备具有人肌肤防太阳光功能的化妆品。
26.基于权利要求14所述TiO2的纳米颗粒分散液的用途,用于制备具有人肌肤防太阳光功能的化妆品。
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JP4382607B2 (ja) * | 2004-03-15 | 2009-12-16 | 住友大阪セメント株式会社 | 酸化チタン粒子 |
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ITFI20040252A1 (it) * | 2004-12-06 | 2005-03-06 | Colorobbia Italiana Spa | Processo per la preparazione di dispersioni di ti02 in forma di nanoparticelle, e dispersioni ottenibili con questo processo |
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2006
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2007
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Also Published As
Publication number | Publication date |
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JP2009525246A (ja) | 2009-07-09 |
EP1996515A1 (en) | 2008-12-03 |
ATE490220T1 (de) | 2010-12-15 |
PT1996515E (pt) | 2011-03-09 |
PL1996515T3 (pl) | 2011-05-31 |
ZA200806991B (en) | 2009-06-24 |
JP5281415B2 (ja) | 2013-09-04 |
BRPI0707256B1 (pt) | 2018-06-19 |
US20080317959A1 (en) | 2008-12-25 |
CA2640938C (en) | 2014-10-28 |
ES2357369T3 (es) | 2011-04-25 |
CN101378993A (zh) | 2009-03-04 |
KR20080094675A (ko) | 2008-10-23 |
DE602007010908D1 (de) | 2011-01-13 |
BRPI0707256A2 (pt) | 2011-04-26 |
EP1996515B1 (en) | 2010-12-01 |
RU2008135345A (ru) | 2010-03-10 |
NZ570356A (en) | 2010-09-30 |
RU2431604C2 (ru) | 2011-10-20 |
AU2007211536B2 (en) | 2012-10-04 |
DK1996515T3 (da) | 2011-03-14 |
US8431621B2 (en) | 2013-04-30 |
KR101353850B1 (ko) | 2014-01-20 |
AU2007211536A1 (en) | 2007-08-09 |
WO2007088151A1 (en) | 2007-08-09 |
BRPI0707256A8 (pt) | 2018-01-09 |
ITFI20060030A1 (it) | 2007-08-02 |
CA2640938A1 (en) | 2007-08-09 |
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