CN108976262B - 一种铋碘杂化材料的室温制备与罗丹明b降解应用 - Google Patents
一种铋碘杂化材料的室温制备与罗丹明b降解应用 Download PDFInfo
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- 229940043267 rhodamine b Drugs 0.000 title claims abstract description 21
- CBIXFXPGRXJEAJ-UHFFFAOYSA-N [I].[Bi] Chemical compound [I].[Bi] CBIXFXPGRXJEAJ-UHFFFAOYSA-N 0.000 title claims abstract description 18
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- RAIPHJJURHTUIC-UHFFFAOYSA-N 1,3-thiazol-2-amine Chemical compound NC1=NC=CS1 RAIPHJJURHTUIC-UHFFFAOYSA-N 0.000 claims abstract description 8
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- KOECRLKKXSXCPB-UHFFFAOYSA-K triiodobismuthane Chemical compound I[Bi](I)I KOECRLKKXSXCPB-UHFFFAOYSA-K 0.000 claims abstract description 3
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Abstract
一种可水解产生BiOI纳米片的铋碘基无机‑有机杂化材料的室温制备及其对罗丹明B的选择性褪色应用。本发明的目的在于提供一种低能耗、操作简便、环境友好的无机‑有机杂化材料(Hatz)BiI4的室温制备方法,其中atz=2‑氨基噻唑;并将其用于方便、快速、高效的选择性降解罗丹明B染料废弃物领域。这种材料置于蒸馏水中可直接水解产生新型半导体催化剂BiOI纳米片。可选择碘化铋,2‑氨基噻唑,乙醇和氢碘酸为反应原料,在室温下经过溶液挥发法获得化合物(Hatz)BiI4的单晶,其优异性能可用于化学法选择性处理染料废液中的罗丹明B,且无需外界提供任何能量。
Description
技术领域
本发明涉及无机-有机杂化材料领域,尤其涉及一种铋碘杂化材料(Hatz)BiI4的室温制备方法及其对罗丹明B染料的选择性褪色的应用,其中atz = 2-氨基噻唑。
背景技术
现代工业技术的飞速发展,导致各种污染物排放至水中,不仅严重威胁人类健康,还带来了不容忽视的经济损失。在各种工业废水中印染废水,罗丹明B对水资源的污染越来越重,引起了人们的广泛关注。在染料废水中,罗丹明B常与其它染料或有机组分混在一起;传统物理吸附方法对罗丹明B染料无选择性的降解或褪色效果,不利于其它混合组分的富集和回收。因此,开发合成简便、能快速并高选择性地使罗丹明B褪色的材料成为一个刻不容缓的问题。然而,现有的此类材料的合成方法如溶剂热法,因具有能耗高,耗时长,过程可控性差的缺点,而显得不尽如人意。此外,目前报道的可使罗丹明B选择性褪色的材料多基于一些无机半导体催化剂,需在外界提供能量(如光能)的情况下进行,此类材料的使用极易受到外界自然条件制约。化学处理方法,如化学氧化法,因无需外界提供能量,不受外界光照条件的制约,即可实现有机染料分子的脱色,具有独特的优势,逐渐受到更多的研究关注。基于此,开发合成步骤简单、低能耗,无需外界提供能量即可选择性地使罗丹明B褪色的新型材料具有重要的实际意义。
另一方面,BiOI纳米片作为一种新型半导体材料,具有良好的紫外和可见光吸收性能,因在催化等领域具有潜在的应用前景,引起了人们的广泛关注。然而,这种材料的合成过程仍有一些不足。传统BiOI制备方法如水解法、沉淀法、高温固相法、水热法、溶剂热法等,大多数合成方法需要封端剂(如表面活性剂)或者苛刻的反应条件。这些传统的方法起始原料都不止一种,如采用含铋无机盐与KI或HI混合,具有操作条件相对复杂,过程相对繁琐,反应条件不易控制,重现性不好等缺点,因此探索一种更高效且更便捷的方式制备BiOI成为材料制备领域一个亟待解决的问题。
发明内容
本发明的目的在于,针对已报道的可使罗丹明B选择性褪色材料的制备过程繁琐、能耗高、工作时需要外界提供能量且选择性不高等问题,提供一种可室温制备、简单易控的铋基杂化材料的合成方法;该材料可用于高效、高选择性、无需外界能量地使罗丹明B选择性褪色,同时亦可直接水解可产生BiOI纳米片,提供一种新型的BiOI制备方法。
本发明的技术方案包括以下内容:
1. 一种可以有效使罗丹明B选择性褪色的铋碘基无机-有机杂化材料(Hatz)BiI4,其中atz = 2-氨基噻唑,其特征在于该铋碘基无机-有机杂化材料为正交晶系,结晶于空间群Pbcn,单胞参数为a = 11.99埃,b = 15.02埃,c = 7.71埃,α = 90度,β = 90度,γ = 90度。
2. 如项1所述的铋碘基无机-有机杂化材料(Hatz)BiI4的晶体结构,BiI6八面体通过共边连接形成一维[BiI4]–阴离子链,N-质子化的2-氨基噻唑阳离子填充在由[BiI4]–阴离子链围成的四边形孔道中。
3. 如项1所述的铋碘基无机-有机杂化材料(Hatz)BiI4的制备方法,将摩尔比为1:1的BiI3与2-氨基噻唑分别用HI和乙醇溶解,再混合两种溶液,室温搅拌4小时后在通风橱下自然挥发,收集固体产物,即可得到黑紫色条状的(Hatz)BiI4晶体。
4. 如项1所述的铋碘基无机-有机杂化材料(Hatz)BiI4的用途,其特征在于:该铋碘基无机-有机杂化材料可作为一种无需外界能量即可选择性降解染料废弃物的褪色材料;也可在pH为5.5的蒸馏水中水解产生形貌良好的BiOI纳米片。
本发明的有益效果:1)铋碘基无机-有机杂化材料的室温合成方法,具有条件简单、能耗低、易控且环境友好的特点;制备的材料可直接在水溶液中使用,无需外界提供能量即可使染料废水中的罗丹明B选择性褪色,脱色条件温和、简便、不易受外界干扰;2)可由该材料通过简单的水解反应制备BiOI纳米片,过程简单易控,无需其它反应物和表面活性剂,无额外能量消耗
附图说明
图1为(Hatz)BiI4对橙黄G和罗丹明B混合染料选择性褪色过程中的紫外-可见吸收光谱。反应1分钟后,两种染料都有较明显的褪色,但褪色程度完全不同。
图2为褪色过程中染料浓度随时间变化曲线。当反应12分钟后,罗丹明B的C/C0值为0.09,说明溶液中罗丹明B已基本脱色完全,而橙黄G的C/C0为0.58左右,大部分仍未降解。
图3为(Hatz)BiI4在pH为5.5的蒸馏水中水解产物的粉末衍射花样,说明水解得到固体为BiOI,无明显其它杂相。
图4为水解产物BiOI的TEM图像,为不规则的片状。
具体实施方式
(1)铋碘基无机-有机杂化材料(Hatz)BiI4的合成
反应物碘化铋和2-氨基噻唑的摩尔比例为1:1,称取相应质量的固体反应物分别用HI和乙醇溶解,再混合两种溶液,室温下将反应溶液搅拌均匀,自然挥发,得到黑紫色(Hatz)4BiI4的晶体产物。
(2)铋碘基无机-有机杂化材料(Hatz)BiI4选择性褪色罗丹明B和橙黄G的混合溶液黑暗条件下,将20毫升9.46毫克/升的橙黄G和20毫升5.4毫克/升的罗丹明B在烧杯中混合均匀,用0.5摩尔/升的HCl调节pH至3.0(记为0分钟)。取20毫克(Hatz)BiI4加入至上述混合染料溶液中,间隔一定的时间后对染料溶液进行紫外-可见分光光度分析(1分钟、3分钟、5分钟、8分钟、12分钟)。
(3)铋碘基无机-有机杂化材料(Hatz)BiI4的水解
将样品研磨,分散在超纯水中,用1摩尔/升的KOH溶液调节溶液pH为5.5,置于室温下水解24小时,将得到的粉末用水洗涤,干燥后测粉末衍射。
Claims (2)
1.一种使罗丹明B选择性褪色的铋碘基无机-有机杂化材料(Hatz)BiI4,其中atz = 2-氨基噻唑,其特征在于该铋碘基无机-有机杂化材料结晶于正交晶系Pbcn空间群,单胞参数为a = 11.99埃,b = 15.02埃,c = 7.71埃,α = 90度,β = 90度,γ = 90度;
由以下方法制备而成:反应物碘化铋和2-氨基噻唑的摩尔比例为1:1,称取相应质量的固体反应物分别用HI和乙醇溶解,再混合两种溶液,室温下将反应溶液搅拌均匀,晾干。
2.一种权利要求1所述的铋碘基无机-有机杂化材料(Hatz)BiI4的用途,其特征在于:该铋碘基无机-有机杂化材料用于混合染料水溶液中罗丹明B的选择性降解。
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