CN112142650A - 一种新型碘化铋酸盐及其制备方法和在荧光、光降解中的应用 - Google Patents

一种新型碘化铋酸盐及其制备方法和在荧光、光降解中的应用 Download PDF

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CN112142650A
CN112142650A CN202011082292.XA CN202011082292A CN112142650A CN 112142650 A CN112142650 A CN 112142650A CN 202011082292 A CN202011082292 A CN 202011082292A CN 112142650 A CN112142650 A CN 112142650A
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倪春林
张静
刘维
陈锶寒
陈丛丛
陈克来
徐奕琳
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Abstract

本发明属于环保功能材料技术领域,具体涉及一种新型卤化铋酸盐,为六碘合铋阴离子和苄基吡啶阳离子组成的化合物,其制备方法包括以下步骤:取一定量溴化苄和吡啶,加入适量溶剂混合溶解,搅拌回流,然后蒸发浓缩,再用乙醚洗涤,得到溴化苄基吡啶盐;取BiI3溶于适量浓碘酸,取一定量溴化苄基吡啶盐溶于适量溶剂,将两溶液混合搅拌回流,得到澄清滤液,于冷冻析晶,即得新型碘化铋酸盐。本发明新型卤化铋酸盐在365nm紫外光照射下发出强烈的橘红色光,在可见光下对罗丹明B和甲基橙进行快速降解,具有很好的循环降解效率。本发明还提供了该新型碘化铋酸盐的制备方法,该方法产率高,节约成本,易于操作,利于工业化生产。

Description

一种新型碘化铋酸盐及其制备方法和在荧光、光降解中的 应用
技术领域
本发明属于环保功能材料技术领域,具体涉及一种新型卤化铋酸盐,即六碘合铋酸·苄基吡啶盐,及其制备方法与在荧光、光降解中的应用。
背景技术
随着工业化和城市化进程的不断推进,由废气、有机物、聚合物和生物质等引起的污染问题变得日益严峻。其中,部分人工合成的有机污染物,尽管在环境中浓度很低,但仍具有较高的毒性,因此有机污染物的去除也得到了广泛的关注。近几十年来,从废水中去除有机染料的技术也在不断开发,如吸附、光降解、生物降解和臭氧氧化等。其中,光催化技术能将多种有机污染物彻底矿化去除,特别是一些生物难以有效降解的有毒有害物质,且反应速度快,工艺成本低,运行条件温和且环境友好,成为了去除有机污染最有效最“绿色”的方法之一。光催化技术以太阳能为驱动力,利用光催化剂将光能转化为化学能,可以直接利用太阳光降解和矿化水体与空气中的各类污染物,具有良好的应用前景。
铋系半导体光催化材料由于其独特的价带结构(即Bi的6s轨道和O 的2p轨道发生杂化从而形成较窄的能带隙)成为处理环境污染的一种新型材料。近年来,卤代铋酸盐(III)作为光催化剂和光学材料的潜在应用在有机-无机杂化化合物领域引起了广泛地关注,但现有卤代铋酸盐仍存在能带隙较宽,可见光利用率低,紫外光下不可见等,亟待解决以提高应用价值。
发明内容
为解决上述问题,本发明提供一种新型碘化铋酸盐,即六碘合铋酸·苄基吡啶盐[BzPy]3[BiI6],其在365nm紫外光照射下发出强烈的橘红色光,在可见光(λ> 400nm)下对罗丹明B(RHB)和甲基橙(MO)进行快速降解,具有很好的循环降解效率。本发明还提供了该新型碘化铋酸盐的制备方法,该方法产率高,节约成本,易于操作,利于工业化生产。
为实现上述目的,本发明通过以下技术方案实现:
设计一种新型碘化铋酸盐,即六碘合铋酸·苄基吡啶盐[BzPy]3[BiI6],为六碘合铋阴离子和苄基吡啶阳离子组成的化合物,其化学结构如式所示:
Figure DEST_PATH_IMAGE001
优选的,所述新型碘化铋酸盐为晶体形态,属于单斜晶系,P2(1)/c空间群。
优选的,所述新型碘化铋酸盐的晶胞参数为a=10.8354(7) Å,b=31.387(2) Å,c=12.8582(10) Å,β=98.914(2)°,晶胞体积为4320.1(5) Å3
本发明新型碘化铋酸盐的制备方法,包括以下步骤:
(1)取一定量溴化苄和吡啶,加入适量溶剂(优选甲醇)混合溶解,于65-70℃搅拌回流(优选16-24小时),然后蒸发浓缩,再用乙醚洗涤,得到黄色油状物,为目标产物[BzPy]Br;所用苄溴和吡啶盐之间的摩尔比为1:(0.8-1.2);
(2)取BiI3溶于适量HI(优选0.1-0.3 mol/L,HI为浓度40%以上的浓碘酸),取一定量[BzPy]Br溶于适量溶剂(优选乙腈),将两溶液混合于80-90℃搅拌回流(优选1.5-3小时),得到澄清滤液,于-15℃到-20℃冷冻析晶,得到红色晶体,即为新型碘化铋酸盐;所用BiI3和[BzPy]Br之间的摩尔比为1:2.5-4。
本发明具有以下积极有益效果:
(1)本发明新型碘化铋酸盐在365nm紫外光照射下展示出良好的橘红色荧光效果,是性能优异的光学材料。其带隙较窄,约为1.56eV,能很好的利用可见光,在可见光下对罗丹明B(RhB)阳离子型染料和甲基橙(MO)阴离子型染料均有着良好的光降解效果。
(2)本发明新型碘化铋酸盐的制备方法操作简便、产率高;所需仪器设备简单,易于操作;所需溶剂耗量少,节约成本,应用范围广,利于工业化推广。
附图说明
图1为本发明实施例1的晶体结构图(氢原子省略);
图2为本发明实施例1单位晶胞堆积图(氢原子省略);
图3为对比例1材料的单位晶胞堆积图(氢原子省略);
图4为本发明实施例1和对比例1的固体紫外可见吸收光谱;
图5为本发明实施例1和对比例1的禁带宽度图;
图6为本发明实施例 1 和对比例1的荧光发射光谱图;
图7为本发明实施例 1 在特定时间间隔处理RHB的紫外光谱;插入物是五次循环光降解率;
图8为本发明实施例 1 和对比例1对RhB降解效果随时间变化图;
图9为本发明实施例 1 和对比例1在催化剂用量不同的情况下对MO光降解率。
具体实施方式
为了更好的了解本发明,下面通过具体的实施例来说明本发明的技术方案。
实施例1:
一种新型碘化铋酸盐,制备方法包括以下步骤:
(1)称取0.02mol溴化苄和0.02mol吡啶于100 mL磨口锥形瓶中,加入30mL甲醇溶解,65-70℃搅拌回流20小时,旋转蒸发后再用乙醚洗涤,得到黄色油状物为目标产物[BzPy]Br,产率为87.1%。
(2)取3mmol所得[BzPy]Br于锥形瓶中,加20mL乙腈溶解;取1mmol BiI3,于烧杯中,加入5mL 45%浓碘酸溶解;将烧杯中溶液缓慢倒入锥形瓶中,85℃加热搅拌回流2 h,置于冰箱里(-18℃左右)冷冻析晶,12小时后得到红色晶体,即为六碘合铋酸·苄基吡啶盐[BzPy]3[BiI6],其产率为82.4%。
对比例1
专利CN109761887实施例1公开的[BzPy]4[Bi2Cl10]。
将实施例1所得材料进行红外光谱检测,IR(cm-1):ν(C-H):3114、3043,ν(C=C):1625、1577、1490、1482,ν(CH2):1452,ν(C-N):1282、1203、1154。
将材料进行固体紫外吸收光谱检测,图谱见图4,实施例1和对比例1吸收截止波长分别为700和390 nm,对应的光学带隙分别为1.56 和3.08 eV,表明实施例1有着比对比例1更好的可见光吸收能力,是一种优异的光催化剂和光学材料。
将实施例1所得材料进行X-射线单晶衍射,晶体学数据见表1,晶体结构见图1,单位晶胞堆积见图2,其阴离子基团以孤立的形式存在,而对比例1的阴离子基团则以二聚体的形式存在,见图3。
将实施例1所得材料进行荧光分析,光致发光光谱见图6,在245nm激发波长下,本实施例碘化铋酸盐在580nm左右出现一个橙黄色发射峰,将所得材料于365nm紫外光照射下进行发光性能检测,能发出明显的橘红色光,见图7插入物。580nm左右的峰是由阴离子结构引起的;多聚体的阴离子相邻的阴离子由于距离太近指致使激发态和基态的势能存在交叉,这将导致非辐射跃迁的能量损失,以至于发生荧光效率较低和淬灭的现象,而以孤立的形式存在的阴离子基团则可以避免这一现象。
在室温下,将所得晶体在300w氙灯下对罗丹明B(RHB)和甲基橙(MO)进行光催化活性评价(λ > 400nm)。
Figure 270833DEST_PATH_IMAGE002
光降解RhB具体实施方法为:将10mg样品悬浮在100mL RhB染料溶液(10.0mg/L)中超声一分钟混匀,然后悬浮液在黑暗中搅拌60分钟,达到染料分子在催化剂表面的吸附脱附平衡。然后把反应液置于可见光下照射,每间隔10分钟,用注射器吸取3.0mL反应液,用紫外-可见分光度计检测。为了评估所得催化化合物的稳定性,进行多次循环重复试验,结果见图7。实施例1和对比例1降解效果见图8。
图7所示,实施例1在50min后,RhB光降解率达到99.02%,五次循环后降解率仍高达97.84%。图8所示,两种材料光降解RhB差异无明显区别,表明两种材料对RhB均有很好的光降解活性。
光降解MO具体实施方法为:分别取10mg、20mg、50mg、100mg样品悬浮在100mL MO染料溶液(10.0mg/L)中超声一分钟混匀,后悬浮液在黑暗中搅拌60分钟,达到染料分子在催化剂表面的吸附脱附平衡。然后把反应液置于可见光下照射,每间隔20分钟,用注射器吸取3.0mL反应液,用紫外-可见分光度计检测,结果见图9。
图9所示,实施例1在不同催化剂量投加下表现出比对比例1显著优异的降解MO效果。结果表明,本发明实施例1材料对阳离子型和阴离子型染料均有着较优异的降解效果,这一点弥补了对比例1光降解MO的不足。
以上所述,仅是本发明的几个具体实施例,并不局限于上述具体实施方式,本领域技术人员还可据此做出多种变化,但任何与本发明等同或者类似的变化都应涵盖在本发明权利要求的范围内。

Claims (10)

1.一种新型碘化铋酸盐,其特征在于:所述碘化铋酸盐为六碘合铋酸·苄基吡啶盐,为六碘合铋阴离子和苄基吡啶阳离子组成的化合物,其化学结构如式所示:
Figure 165264DEST_PATH_IMAGE002
2.根据权利要求1所述的新型碘化铋酸盐,其特征在于:所述新型碘化铋酸盐为晶体形态,属于单斜晶系,P2(1)/c空间群。
3.根据权利要求2所述的新型碘化铋酸盐,其特征在于:所述新型碘化铋酸盐的晶胞参数为a=10.8354(7) Å,b=31.387(2) Å,c=12.8582(10) Å,β=98.914(2)°,晶胞体积为4320.1(5) Å3
4.权利要求1-3任一项所述新型碘化铋酸盐的制备方法,其特征在于,包括以下步骤:
(1)取一定量溴化苄和吡啶,加入适量溶剂混合溶解,于65-70℃搅拌回流,然后蒸发浓缩,再用乙醚洗涤,得到目标产物溴化苄基吡啶盐;
(2)取BiI3溶于适量浓碘酸,取一定量溴化苄基吡啶盐溶于适量溶剂,将两溶液混合于80-90℃搅拌回流,得到澄清滤液,于-15℃到-20℃冷冻析晶,即得新型碘化铋酸盐。
5.根据权利要求4所述的制备方法,其特征在于:步骤(1)所述溶剂为甲醇,搅拌回流时间为16-24 小时。
6.根据权利要求4所述的制备方法,其特征在于:步骤(1)所用苄溴和吡啶盐之间的摩尔比为1:(0.8-1.2)。
7.根据权利要求4所述的制备方法,其特征在于:步骤(2)所用BiI3和溴化苄基吡啶盐之间的摩尔比为1:(2.5-4)。
8.根据权利要求4所述的制备方法,其特征在于:步骤(2)所用BiI3溶于浓碘酸的浓度为0.1-0.3 mol/L,浓碘酸中HI含量为40wt%以上。
9.根据权利要求4所述的制备方法,其特征在于:步骤(2)所述溶剂为乙腈,搅拌回流时间为1.5-3小时。
10.权利要求1-3任一项所述新型碘化铋酸盐在荧光材料或光降解中的应用。
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