CN107243339A - 一种二氧化铈纳米棒光催化剂的制备方法 - Google Patents
一种二氧化铈纳米棒光催化剂的制备方法 Download PDFInfo
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- VYLVYHXQOHJDJL-UHFFFAOYSA-K cerium trichloride Chemical compound Cl[Ce](Cl)Cl VYLVYHXQOHJDJL-UHFFFAOYSA-K 0.000 claims description 10
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Abstract
本发明涉及一种二氧化铈纳米棒光催化剂的制备方法,通过控制变量制备了三种形貌的纳米棒单体,并且从中选择出了光催化性能最好的纳米棒单体。利用七水三氯化铈,氢氧化钠,去离子水为原料,通过水热法反应制得二氧化铈纳米棒光催化剂单体。本实验通过制备三种不同形貌的二氧化铈纳米棒单体,研究其光催化性能,填补了研究二氧化铈纳米棒单体光催化性能的空白。
Description
技术领域
本发明涉及一种二氧化铈纳米棒光催化剂的制备方法,属于光催化剂技术领域。
背景技术
随着科学技术的发展,人类的生活水平也是逐渐的提升。自两次工业革命以来,社会的生产力得到极大的提高,但是人类的生活环境却是每况愈下,各种污染随之而来。雾霾,水污染等等接踵而至。许多大城市屡屡被雾霾所困扰,pm2.5指数只增不减,有时百米之外灰蒙蒙的一片,这不仅影响交通安全,更是会对人类的身体产生极大的伤害。众所周知,水孕育了生命,水对人类的作用极大。可现在水污染极其严重,河流漂浮着众多的污染物,不仅仅是表面上的塑料袋,它更是含有难以分解的有机化合物,这些几乎都是致癌物。但如今的污水处理技术很单一,不仅效果不太好,而且容易造成二次污染,这就限制了污水处理技术的发展,利用活性炭吸附就是一个例子。
而光催化技术与普通的吸附以及其他污水处理相比,有着很大的优势,它具备以下几个优点,(1)反应条件非常温和,常温常压,太阳光照射下即可催化污染物较为完全分解。(2)无二次污染,光催化反应的产物,一般是H2O﹑CO2﹑N2等无污染物质,对环境友好。(3)反应原理简单,制备方便,操作也很简单,可以大规模的生产。(4)光催化剂可以重复利用,不会出现用一次就失活的情况。正是因为光催化技术具备平常技术无法企及的优点,因此它成为近几年来科学工作者的研究热点,它也在水污染,环保等方面体现了非常高的经济价值。
二氧化铈具备独特的物理和化学性质,例如在催化剂,紫外光吸收剂,抛光材料,燃料电池等方面得到了广泛的应用。二氧化铈作为稀土元素铈的一种氧化物,具有立方萤石型结构和很好的储氢能力,因此具有较多的氧空位和较低的氧化还原电势,正是因为有这些特点,其具备较强的催化氢化的能力。首先,二氧化铈具备的萤石型结构,晶胞中的每个Ce4+按面心立方点阵排列 ,O2-占据所有的四面体位置 ,每个Ce4+周围被个8个O2-包围,,而每个O2-则与最近的4个Ce4+配位。当二氧化铈颗粒尺寸降到纳米级别时,它外层与次外层电子会变得不稳定,会使得铈的价态在三价与四价间转化,并且其表面及体相的晶格氧原子能够直接参与反应并被消耗,所以同时会形成氧空位,而二氧化铈纳米棒中氧空位的产生与消除直接伴随着氧的放出和存储过程,使其具备独特的氧化还原性能,同时CeO2也有着良好的化学稳定性和高温快速氧空位扩散能力,因此它可以很好地将有机污染物快速地降解为H2O﹑CO2﹑N2等无污染物质。相比于其他氧化物, CeO2表面氧空位的形成能较低。例如, CeO2表面的氧空位形成能(2.0 eV 左右)要远低于 TiO2表面的氧空位形成能(4.8eV),形成能越低,氧空位形成越容易,催化降解的效果越好,由此可见,二氧化铈作为光催化剂具有较大的优势。
目前对于二氧化铈纳米棒的制备已经有了一些方法,但是很多制备方法存在制备麻烦,原料浪费的问题。例如专利(CN104445339A)写到的方法中,采用乙酸铈与氨水混合,用微波加热,高温灼烧后得到成品,这种方法对环境的要求高,并且原料会存在浪费的问题。再如专利(CN104891550A)中提到,通过利用混合沉淀剂制备二氧化铈,该方法步骤很多,各类反应物所需量要很精确,这就存在制备麻烦,并且历经如此多的步骤,会导致产率的降低。再如专利(CN105502468A)中说到,通过将硝酸铈与四乙基氢氧化铵经过一系列步骤制得二氧化铈纳米棒,这种方法制得的纳米棒过大,氧空位的比表面积小,会使催化性能减弱。
发明内容
本发明的目的提供一种二氧化铈纳米棒光催化剂的制备方法,通过控制变量制备了三种形貌的纳米棒单体,并且从中选择出了光催化性能最好的纳米棒单体。利用七水三氯化铈,氢氧化钠,去离子水为原料,通过水热法反应制得二氧化铈纳米棒光催化剂单体。本发明通过制备三种不同形貌的二氧化铈纳米棒单体,研究其光催化性能,填补了研究二氧化铈纳米棒单体光催化性能的空白。
一种二氧化铈纳米棒光催化剂的制备方法,步骤如下:
制备A型二氧化铈纳米棒单体
1.5g CeCl3•7H2O加入5ml去离子水中溶解,制成A液,2.4gNaOH加入15ml去离子水中溶解,制成B液,把A液和B液混合,搅拌10min之后,将混合溶液加入到反应釜中,130℃下反应18h,得到的产物用去离子水洗涤,然后在室温下反应干燥20h,继续在300℃下焙烧4h,即得A型二氧化铈纳米棒单体,A型二氧化铈纳米棒单体简称为3M CeO2。
一种二氧化铈纳米棒光催化剂的制备方法,步骤如下:
制备B型二氧化铈纳米棒单体
1.5g CeCl3•7H2O加入5ml去离子水中溶解,制成A液,4gNaOH加入15ml去离子水中溶解,制成B液,把A液和B液混合,搅拌10min之后,将混合溶液加入到反应釜中,130℃下反应18h,得到的产物用去离子水洗涤,然后在室温下反应干燥20h,继续在300℃下焙烧4h,即得B型二氧化铈纳米棒单体,B型二氧化铈纳米棒单体简称为5M CeO2。
一种二氧化铈纳米棒光催化剂的制备方法,步骤如下:
制备C型二氧化铈纳米棒单体
1.5g CeCl3•7H2O加入5ml去离子水中溶解,制成A液,6.4gNaOH加入15ml去离子水中溶解,制成B液,把A液和B液混合,搅拌10min之后,将混合溶液加入到反应釜中,130℃下反应18h,得到的产物用去离子水洗涤,然后在室温下反应干燥20h,继续在300℃下焙烧4h,即得C型二氧化铈纳米棒单体,C型二氧化铈纳米棒单体简称为8M CeO2。
本发明的原理是利用了二氧化铈独特的立方萤石型结构,以及很好的储氢能力。立方萤石结构中,铈离子与氧离子与1:8的比例进行匹配,当我们把二氧化铈的尺寸降至纳米级别时,铈离子的价态发生转变,晶格氧原子参与反应,因此形成了氧空位,这伴随着氧的放出和储存,让二氧化铈纳米棒具备了很强的催化氧化性能。此外,二氧化铈纳米棒的氧空位形成能比其他常见的催化剂要低,故催化性能也比较好,利用变量制备三种形貌的二氧化铈纳米棒单体,通过测试其光催化性能,得到拥有最好催化性能的催化剂。
本发明的优点为:
1、本发明通过控制一种变量制备了三种不同形貌的二氧化铈纳米棒单体,并且通过催化实验从里面选择出了光催化性能最好的一种纳米棒单体,填补了二氧化铈纳米棒单体方面研究的空白。
2、本发明的产物二氧化铈纳米棒单体纯度高 ,分散性好 ,且制备过程中污染小,能量消耗也少。成本低,可量产。
3、二氧化铈纳米棒单体对人体及其他生物无毒,不会产生二次污染。
4、使用方法非常简单,只需要将催化剂放入污水,在太阳光照射下就能成功分解有机污染物。
5、二氧化铈纳米棒单体具有良好的活性,不会存在使用一次就失活的现象,它可以重复利用。
附图说明
图1:本发明二氧化铈纳米棒单体拉曼图。
图2:本发明二氧化铈纳米棒单体光催化性能图。
图3:本发明二氧化铈纳米棒单体氮吸收曲线。
图4:本发明二氧化铈纳米棒单体光电流密度。
图5:本发明二氧化铈纳米棒单体粒径分布图。
图6:本发明二氧化铈纳米棒单体扫描电镜照片。
具体实施方式
实施例1
一种二氧化铈纳米棒光催化剂的制备方法,步骤如下:
制备A型二氧化铈纳米棒单体
1.5g CeCl3•7H2O加入5ml去离子水中溶解,制成A液,2.4gNaOH加入15ml去离子水中溶解,制成B液,把A液和B液混合,搅拌10min之后,将混合溶液加入到反应釜中,130℃下反应18h,得到的产物用去离子水洗涤,然后在室温下反应干燥20h,继续在300℃下焙烧4h,即得A型二氧化铈纳米棒单体,A型二氧化铈纳米棒单体简称为3M CeO2。
实施例2
制备B型二氧化铈纳米棒单体
1.5g CeCl3•7H2O加入5ml去离子水中溶解,制成A液,4gNaOH加入15ml去离子水中溶解,制成B液,把A液和B液混合,搅拌10min之后,将混合溶液加入到反应釜中,130℃下反应18h,得到的产物用去离子水洗涤,然后在室温下反应干燥20h,继续在300℃下焙烧4h,即得B型二氧化铈纳米棒单体,B型二氧化铈纳米棒单体简称为5M CeO2。
实施例3
一种二氧化铈纳米棒光催化剂的制备方法,步骤如下:
制备C型二氧化铈纳米棒单体
1.5g CeCl3•7H2O加入5ml去离子水中溶解,制成A液,6.4gNaOH加入15ml去离子水中溶解,制成B液,把A液和B液混合,搅拌10min之后,将混合溶液加入到反应釜中,130℃下反应18h,得到的产物用去离子水洗涤,然后在室温下反应干燥20h,继续在300℃下焙烧4h,即得C型二氧化铈纳米棒单体,C型二氧化铈纳米棒单体简称为8M CeO2。
通过说明书附图可知,三种不同二氧化铈纳米棒吸光能力不尽相同,5M CeO2纳米棒吸光范围最强,达到436nm (通过切线法做切线得到此结果,一般测算吸光范围都是利用切线法得出).在光催化试验中,其中5M CeO2纳米棒光催化性能优异,在两个小时的时间内,可以降解70%的有机污染物。粒径分布图可知,其中5M CeO2纳米棒的粒径最小,总体在15nm范围,较低的粒径提高了催化剂比表面积,使得其反应位点增加。
Claims (3)
1.一种二氧化铈纳米棒光催化剂的制备方法,其特征为:步骤如下:
制备A型二氧化铈纳米棒单体
1.5g CeCl3•7H2O加入5ml去离子水中溶解,制成A液,2.4gNaOH加入15ml去离子水中溶解,制成B液,把A液和B液混合,搅拌10min之后,将混合溶液加入到反应釜中,130℃下反应18h,得到的产物用去离子水洗涤,然后在室温下反应干燥20h,继续在300℃下焙烧4h,即得A型二氧化铈纳米棒单体,A型二氧化铈纳米棒单体简称为3M CeO2。
2.一种二氧化铈纳米棒光催化剂的制备方法,其特征为:步骤如下:
制备B型二氧化铈纳米棒单体
1.5g CeCl3•7H2O加入5ml去离子水中溶解,制成A液,4gNaOH加入15ml去离子水中溶解,制成B液,把A液和B液混合,搅拌10min之后,将混合溶液加入到反应釜中,130℃下反应18h,得到的产物用去离子水洗涤,然后在室温下反应干燥20h,继续在300℃下焙烧4h,即得B型二氧化铈纳米棒单体,B型二氧化铈纳米棒单体简称为5M CeO2。
3.一种二氧化铈纳米棒光催化剂的制备方法,其特征为:步骤如下:
制备C型二氧化铈纳米棒单体
1.5g CeCl3•7H2O加入5ml去离子水中溶解,制成A液,6.4gNaOH加入15ml去离子水中溶解,制成B液,把A液和B液混合,搅拌10min之后,将混合溶液加入到反应釜中,130℃下反应18h,得到的产物用去离子水洗涤,然后在室温下反应干燥20h,继续在300℃下焙烧4h,即得C型二氧化铈纳米棒单体,C型二氧化铈纳米棒单体简称为8M CeO2。
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