CN106000370B - 一种光致Ti3+自掺杂TiO2光催化剂的制备方法 - Google Patents
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/063—Titanium; Oxides or hydroxides thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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Abstract
本发明公开了一种光致Ti3+自掺杂TiO2光催化剂的制备方法。本方法将TiO2置于硼氢化物溶液中,用紫外光辐照一定时间后,进行固液分离并干燥,即得到Ti3+自掺杂TiO2。作为优选,硼氢化物为NaBH4、KBH4、LiBH4;溶剂是水(pH>5)、四氢呋喃、乙醇、甲醇,溶液温度‑30~90°C;紫外光强度>20μW/cm2,辐照时间为0.05 h~10 h;固液分离后在真空或非氧化性气体气氛下干燥,温度30~150°C,时间0.1 h~10 h。本方法工艺简单、效率高、原料廉价易得,适合工业化生产;制备的Ti3+自掺杂TiO2具有和原料TiO2一样的微观形貌,有望在光解水制氢、降解有机污染物等领域获得广泛应用。
Description
技术领域
本发明涉及改性二氧化钛光催化剂的制备,尤其涉及一种光致Ti3+自掺杂TiO2光催化剂的制备方法。
背景技术
随着全球工业化进程的不断发展,当今社会的能源短缺和环境污染问题日益严重,人们的生活与健康受到越来越严重的威胁。TiO2其无毒、成本低、光催化活性高、化学稳定性好,较强的氧化还原能力,成为最为常用的光催化剂,引起了全世界学者的广泛关注。但TiO2的带隙较宽(约3.2 eV),只有紫外光(占据<5%的总太阳能) 才能激发TiO2,产生电子-空穴对,进而光电化学过程得以发生。因此,在可见光区域(占据43%的总太阳能)增加TiO2的光吸收就显的尤为重要。其中,一个主要的途径就是掺杂(如:金属掺杂和非金属掺杂),但多数情况下,外来掺杂的离子可充当光生电子和空穴的复合中心,而且外来掺杂形成的杂质水平通常是不均匀不连续的,从而导致光生电子和空穴的迁移存在困难。此外,掺杂元素同时会造成一定的热不稳定性。
除了外来离子掺杂以外,自掺杂也是一种调控能带结构和提高量子效率的有效手段。Ti3+自掺杂TiO2是一种富有潜力可见光光催化剂。然而,目前国内外合成Ti3+自掺杂TiO2的主要使用氧化还原法,将钛的前躯体与还原剂混合、还原,最后经过煅烧得到自掺杂TiO2,或者将TiO2在高温及高压还原性气氛(如H2)下还原较长时间。有人用NaBH4作为还原剂,在180°C下用钛酸正丁酯前驱体水热法10 h,合成了Ti3+自掺杂TiO2。也有人用TiO2在200°C及2 MPa的H2气氛下还原5天时间得到自掺杂的TiO2。但是这些方法需要高温或者高压条件,所需时间较长,成本较高,生产效率较低,使其在实际应用中受到了一定的限制。
发明内容
本发明的目的是克服现有技术的不足,提供一种光致Ti3+自掺杂TiO2光催化剂的制备方法。该方法具有工艺简单,可在较低温度和常压下快速的制备出Ti3+自掺杂TiO2,同时自掺杂TiO2的形貌尺寸均取决于原始TiO2。
具体技术方案如下:
一种光致Ti3+自掺杂TiO2光催化剂的制备方法,包括以下步骤:
A. 将TiO2与硼氢化物溶液混合,搅拌均匀,并置于紫外光辐照下一定时间;
B. 将辐照后的混合液进行固液分离,得到沉淀物;
C. 将沉淀物干燥,既可以得到Ti3+自掺杂TiO2。
作为优选,所述步骤A中TiO2是颗粒状TiO2、线状TiO2、管状TiO2、带状TiO2或其混合物。
作为优选,所述步骤A中的中的硼氢化物为NaBH4、KBH4、LiBH4或其混合物。
作为优选,所述步骤A中的硼氢化物溶液的溶剂是水、四氢呋喃、乙醇、甲醇或其混合物,硼氢化物溶液温度为-30~90°C;
作为最优选,所述步骤A中的硼氢化物的溶剂是水,硼氢化物溶液是pH>5的弱酸性或碱性溶液。
作为优选,所述步骤A中的紫外光的强度>20 μW/cm2,波长范围100~380 nm,紫外光辐照时间为0.05 h~10 h。
作为优选,所述步骤B中的固液分离操作为离心,抽滤,洗涤或其混合步骤,操作在空气或非氧化性气体气氛下进行。
作为优选,所述步骤C中,在真空条件或者在非氧化性气体气氛下干燥,干燥温度为30~150°C,干燥时间0.1 h~10 h。
本发明与现有技术相比具有如下的优点:
(1) 适合工业化生产。本发明的制备方法可以在常温常压下进行,避免了加热/冷却设备和高压/低压设备的使用;本发明的制备方法所需时间短,制备效率高;本发明的制备方法所需原料廉价易得。
(2) 保留了原料TiO2的微观形貌。本发明的制备方法中,Ti3+的自掺杂温和、均匀地发生在紫外光辐照下的原料TiO2表面,不会破坏原料TiO2的微观形貌,能够以特殊形貌的TiO2为原料制备相同形貌的Ti3+自掺杂TiO2,有利于光催化性能的提升。
附图说明
图1 原始P25 TiO2与本发明实施例1得到的Ti3+自掺杂的TiO2粉末的照片对比图。
图2 原始P25 TiO2与本发明实施例1得到的Ti3+自掺杂的TiO2粉末的X射线衍射(XRD)图。
图3 原始P25 TiO2 (a)与本发明实施例1得到的Ti3+自掺杂的TiO2粉末(b)的X射线光电子能谱(XPS)图。
图4 原始P25 TiO2与本发明实施例2得到的Ti3+自掺杂的TiO2粉末的紫外可见漫反射谱(UV-Vis DRS)图。
图5 原始TiO2纳米线与本发明实施例3得到的Ti3+自掺杂的TiO2纳米线在125 W高压汞灯下的甲基橙溶液(100 mg/L)降解对比。
具体实施方式
下面结合实施例对本发明进行详细说明,但实施例并不对本发明做任何形式的限定。
实施例1
将150 mL pH=10的NaOH水溶液和聚四氟磁子加入反应瓶中,并将反应瓶置于30°C的水浴锅中,开启并控制磁力搅拌速度为40 r/min。称取0.5 g NaBH4 (Alfa Aesar,97%)和0.45 g Degussa P25 TiO2(颗粒状),加入到反应瓶中,迅速开启高压汞灯(功率125 W,主波长365 nm,强度10 mW/cm2,使用石英冷阱和30°C循环水冷却),开始紫外光辐射。紫外光辐照5 h后,将反应瓶中的混合液在空气中进行离心,去除上层清液后,将离心后的沉淀物在真空条件和40°C的温度下干燥2 h,得到灰蓝色TiO2粉末,如图1所示。得到的灰蓝色TiO2粉末的X射线衍射谱(XRD)及X射线光电子能谱(XPS)分别如图2和图3b所示。从图2的XRD图谱,相比于Degussa P25 TiO2,我们发现得到的灰蓝色TiO2粉末的晶型和尺寸未发生变化。对比灰蓝色TiO2粉末(图3b)和P25 TiO2 (图3a)的Ti元素XPS图,我们可以看到灰蓝色TiO2粉末中出现了Ti3+离子的463.4 eV和457.2 eV峰,分别属于Ti3+离子的2p1/2和2p3/2轨道产生的,这表明了Ti3+离子的存在,成功得到Ti3+自掺杂TiO2。根据XPS图谱中相应峰面积的估算,我们估计Ti3+离子的掺杂量约为35.22%。
实施例2
将150 mL pH=13的LiOH水溶液和聚四氟磁子加入反应瓶中,并将反应瓶置于40°C的水浴锅中,开启并控制磁力搅拌速度为40 r/min。称取0.327 g LiBH4 (Alfa Aesar,95%)和0.45 g Degussa P25 TiO2(颗粒状),加入到反应瓶中,迅速开启高压汞灯(功率250W,主波长365 nm,强度30 mW/cm2,使用石英冷阱和40°C循环水冷却),开始紫外光辐射。紫外光辐照1 h后,将反应瓶中的混合液在Ar气气氛进行抽滤,并用无水乙醇洗涤3次。得到的沉淀物在Ar气气氛下干燥0.1 h,干燥温度为100°C,也得到灰蓝色的Ti3+自掺杂TiO2粉末。图4为得到的Ti3+自掺杂TiO2的UV-Vis DRS谱。我们可以看到,相对于原始的P25 TiO2,实施例2制备的Ti3+自掺杂TiO2的吸收带边红移了约30 nm,且在可见光区域有一定强度的吸收,说明我们实施例2得到的Ti3+自掺杂TiO2具有可见光活性。
实施例3
将150 mL无水乙醇和聚四氟磁子加入反应瓶中,并将反应瓶置于15°C的水浴锅中,开启并控制磁力搅拌速度为40 r/min。称取0.2 g NaBH4 (Alfa Aesar,97%)和0.3 gTiO2纳米线,加入到反应瓶中,迅速开启高压汞灯(功率125 W,主波长365 nm,强度10 mW/cm2,使用石英冷阱和15°C循环水冷却),开始紫外光辐射。紫外光辐照2 h后,将反应瓶中的混合液在N2气气氛下进行抽滤,将抽滤后的沉淀物在真空条件和65°C的温度下干燥0.2 h,也得到灰蓝色的Ti3+自掺杂TiO2纳米线。实施例3与原始的TiO2纳米线对在相同条件下甲基橙溶液的降解对比(图5)发现,实施例3合成的Ti3+自掺杂TiO2纳米线的光降解效率较原始TiO2纳米线有所提升。
Claims (3)
1.一种光致Ti3+自掺杂TiO2光催化剂的制备方法,其特征是包括以下步骤:
A.将TiO2与硼氢化物溶液混合,搅拌均匀,并置于紫外光辐照下一定时间,步骤A中TiO2是颗粒状TiO2、线状TiO2、管状TiO2、带状TiO2或其混合物,步骤A中的硼氢化物溶液的溶剂是水、四氢呋喃、乙醇、甲醇或其混合物,硼氢化物溶液温度为-30~90℃,步骤A中的紫外光的强度>20μW/cm2,波长范围100~380nm,紫外光辐照时间为0.05h~10h;
B.将辐照后的混合液进行固液分离,得到沉淀物,步骤B中的固液分离操作为离心,抽滤,洗涤或其混合步骤,操作在空气或非氧化性气体气氛下进行;
C.将沉淀物干燥,得到Ti3+自掺杂TiO2,步骤C中,在真空条件或者在非氧化性气体气氛下干燥,干燥温度为30~150℃,干燥时间0.1h~10h。
2.根据权利要求1所述的制备方法,其特征在于:步骤A中的中的硼氢化物为NaBH4、KBH4、LiBH4或其混合物。
3.根据权利要求1所述的制备方法,其特征在于:步骤A中的硼氢化物的溶剂是水,硼氢化物溶液是pH>5的弱酸性或碱性溶液。
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