CN109201008B - 一种高效吸附有机染料的金属卤化物材料及其制备方法 - Google Patents
一种高效吸附有机染料的金属卤化物材料及其制备方法 Download PDFInfo
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Abstract
本发明属于无机化学技术领域,涉及一种高效吸附有机染料的金属卤化物材料及其制备方法,先将银盐、铁盐、二甲亚砜、水、氢碘酸混合均匀得到混合物;再将混合物装入带盖子的玻璃瓶中,在80℃下晶化2天得到结晶性良好的块状红色晶体;然后块状红色晶体用乙醇洗涤,并在室温下干燥,即制备得到金属卤化物材料,合成的具有染料吸附功能的一维链状金属卤化物材料对亚甲基蓝有着快速且优异的吸附特性,而且吸附了亚甲基蓝的金属卤化物材料在硝酸钠溶液中,可以逐渐释放出亚甲基蓝染料,具备优异的可逆及循环性能;其原料简单易得,制备方法简单,操作方便,重复性好,环境友好。
Description
技术领域:
本发明属于无机化学技术领域,具体涉及一种高效吸附有机染料的金属卤化物材料及其制备方法。
背景技术:
近年来,有机染料在不同工业领域中已成为不可或缺的重要加工材料,并且随着染料的不断更新发展,其种类也越来越多。然而,这些染料在印染、纺织、造纸、油漆以及皮革等工业生产中,会高质量高浓度地排放到工业废水中,从而对环境造成较为严重的影响。据统计,全世界约有15%的染料在生产过程中被排放出来,由于其浓度高、毒性大并且通常带有极性基团,从而严重危害生态环境。此外,一些染料污染物在自然环境中又进一步通过氧化水解等作用形成其他有毒副产物,进而导致环境加剧恶化,处理难度也进一步加大。目前,治理染料污染物的主要方法有物理吸附、化学反应、生物降解等方法,其中吸附技术由于其对环境友好且较为便捷等优点,在处理有机染料废水方面被广泛地应用,但传统的吸附剂如活性炭,存在价格高昂,重复性低等不利因素,限制了其应用范围。因此寻求一种能够高效、稳定、简便地处理染料污染物的吸附材料十分必要。
金属卤化物材料,作为一种新型的晶态杂化材料,目前备受人们关注。这类化合物是由具有灵活配位模式的金属离子与不同的卤素离子桥连形成的一类新兴材料,其主体框架通常带有负电荷,抗衡离子多数为质子化的有机胺或金属-有机配合物。最近,溶剂化的无机金属离子被逐渐地当做模板剂和抗衡离子,来构筑新颖的金属卤化物材料。相对灵活的无机阳离子,以及主体框架的负电性赋予了该类化合物良好的离子交换性能,进而引起了科学家们极大的兴趣,与其他吸附剂相比,这类材料由于其可重复性好、价格相对低廉、环境友好等优点,使其在对有机染料所造成的环境污染等问题上具有较大的应用前景。因此,迫切需要提供一种具有吸附性能的新型金属卤化物材料及其制备方法。
发明内容:
本发明的目的在于克服现有技术存在的缺点,提供一种高效吸附有机染料的金属卤化物材料的及其制备方法,以对染料污染物的吸附为导向,运用自组装和晶体工程学原理,通过对结构的深入探究和对性能的不断挖掘,开发出能高效吸附有机染料污染物的新颖材料。
为了实现上述目的,本发明所述高效吸附有机染料的金属卤化物材料的分子式为[Fe(DMSO)6][Ag6I9]·DMSO,分子量为2392.07,晶体学数据为 α=90°,β=96.271(9)°,γ=90°, Z=2,空间群为P21/m,其中DMSO为二甲亚砜;该材料具有一维链状结构,利用溶剂化的三价铁离子做抗衡离子和结构导向剂,诱导出由银离子和碘离子无限连接构筑的带有负电荷的一维链状结构。
本发明制备所述高效吸附有机染料的金属卤化物材料的具体过程为:
(1)、将0.1-0.2mmol银盐、0.1mmol铁盐、5mL二甲亚砜、2-5mL水、0.05-0.1mL氢碘酸混合均匀得到混合物;
(2)、将步骤(1)制成的混合物装入带盖子的玻璃瓶中,在80℃下晶化2天得到结晶性良好的块状红色晶体;
(3)、将步骤(2)所得块状红色晶体用乙醇洗涤,并在室温下干燥,即制备得到金属卤化物材料。
本发明所述的银盐为碘化银;铁盐为硫酸铁;有机染料为亚甲基蓝、酸性品红、罗丹明B或甲基紫;玻璃瓶的容积为25mL。
本发明将制备的金属卤化物材料浸于含浓度为10-5M有机染料的乙醇溶液中,用紫外可见分光光度计测试其在不同时间的吸光度,有机染料为亚甲基蓝时,在浸泡3小时后对亚甲基蓝的吸附量可达50%,10小时后可以达到90%。
本发明与现有技术相比,合成的具有染料吸附功能的一维链状金属卤化物材料在浸于不同有机染料的乙醇溶液中时,呈现出不同的吸附效果,尤其对特定的阳离子染料有着良好的离子交换性能,且对于尺寸大小较为合适的亚甲基蓝有着快速且优异的吸附特性,紫外-可见吸收光谱表明该吸附材料在3小时后对亚甲基蓝的吸附量可达50%,10小时后可达到90%,而且吸附了亚甲基蓝的金属卤化物材料在硝酸钠溶液中,可以逐渐释放出亚甲基蓝染料,证明了其具备优异的可逆及循环性能;其原料简单易得,制备方法简单,操作方便,重复性好,环境友好。
附图说明:
图1为本发明所述金属卤化物材料中金属的配位环境示意图。
图2为本发明所述金属卤化物材料的一维结构图。
图3为本发明所述金属卤化物材料在吸附前后的粉末X-射线衍射谱图和单晶拟合谱图。
图4为本发明所述金属卤化物材料吸附亚甲基蓝溶液的紫外-可见吸收光谱。
图5为本发明所述金属卤化物材料物释放亚甲基蓝溶液的紫外-可见吸收光谱。
具体实施方式:
下面通过实施例并结合附图对本发明作进一步说明。
本实施例所述高效吸附有机染料的金属卤化物材料的分子式为[Fe(DMSO)6][Ag6I9]·DMSO,分子量为2392.07,晶体学数据为 α=90°,β=96.271(9)°,γ=90°, Z=2,空间群为P21/m,其中DMSO为二甲亚砜;该材料具有一维链状结构,利用溶剂化的三价铁离子做抗衡离子和结构导向剂,诱导出由银离子和碘离子无限连接构筑的带有负电荷的一维链状结构(如图2所示)。
本实施例制备所述高效吸附有机染料的金属卤化物材料的具体过程为:
(1)、将0.1-0.2mmol银盐、0.1mmol铁盐、5mL二甲亚砜、2-5mL水、0.05-0.1mL氢碘酸混合均匀得到混合物;
(2)、将步骤(1)制成的混合物装入带盖子的玻璃瓶中,在80℃下晶化2天得到结晶性良好的块状红色晶体;
(3)、将步骤(2)所得块状红色晶体用乙醇洗涤,并在室温下干燥,即制备得到金属卤化物材料。
本实施例所述的银盐为碘化银;铁盐为硫酸铁;有机染料为亚甲基蓝、酸性品红、罗丹明B、甲基紫;玻璃瓶的容积为25mL。
本实施例对亚甲基蓝有着快速且优异的吸附特性,紫外-可见吸收光谱(如图4所述)表明该吸附材料在3小时后对亚甲基蓝的吸附量可达50%,10小时后可达到90%,而且从图5所示紫外-可见吸收光谱可以看出,吸附了亚甲基蓝的金属卤化物材料在硝酸钠溶液中,可以逐渐释放出亚甲基蓝染料,证明了其具备优异的可逆及循环性能。
实施例1:
本实施例将0.0235g碘化银、0.04g硫酸铁、5mL二甲亚砜、2mL水以及0.05mL氢碘酸的混合物加入到25mL带盖子的玻璃瓶中,在80℃的烘箱中晶化2天,待反应完成后将玻璃瓶取出在室温下自然冷却,将生成的晶体移出并用乙醇反复清洗3次,室温下烘干得到块状红色晶体,对晶体结构解析表明所得化合物具有一维链状结构,银离子与碘离子的键合构筑了无限延伸的一维链,游离的溶剂合铁离子填充在链与链间,用来维持体系的电荷平衡。紫外-可见吸收光谱实验测试表明,该晶态化合物对尺寸合适的阳离子染料亚甲基蓝有着高效、快速和优异的吸附效果。
实施例2:
本实施例将0.0235g碘化银、0.04g硫酸铁、5mL二甲亚砜、2mL水以及0.1mL的氢碘酸混合物加入到25mL带盖子的玻璃瓶中,在80℃的烘箱中晶化2天,经过如实施例1中冷却、洗涤和干燥的方法,得到的目标产物各项表征及结果与实施例1相同。
实施例3:
本实施例将0.047g碘化银、0.04g硫酸铁、5mL二甲亚砜、2mL水以及0.05mL的氢碘酸混合物加入到25mL带盖子的玻璃瓶中,在80℃的烘箱中晶化2天,经过如实施例1中冷却、洗涤和干燥的方法,得到的目标产物各项表征及结果与实施例1相同。
实施例4:
本实施例将0.0235g碘化银、0.04g硫酸铁、5mL二甲亚砜、5mL水以及0.05mL的氢碘酸混合物加入到25mL带盖子的玻璃瓶中,在80℃的烘箱中晶化2天,经过如实施例1中冷却、洗涤和干燥的方法,得到的目标产物各项表征及结果与实施例1相同。
Claims (2)
1.一种高效吸附有机染料的金属卤化物材料的制备方法,其特征在于具体制备过程为:
(1)、将0.1-0.2mmol银盐、0.1mmol铁盐、5mL二甲亚砜、2-5mL水、0.05-0.1mL氢碘酸混合均匀得到混合物;
(2)、将步骤(1)制成的混合物装入带盖子的玻璃瓶中,在80℃下晶化2天得到结晶性良好的块状红色晶体;
2.根据权利要求1所述金属卤化物材料的制备方法,其特征在于所述银盐为碘化银;铁盐为硫酸铁;有机染料为亚甲基蓝、酸性品红、罗丹明B或甲基紫;玻璃瓶的容积为25mL。
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