CN105561918A - 负载碘的纳米孔材料和负载碘的方法 - Google Patents

负载碘的纳米孔材料和负载碘的方法 Download PDF

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CN105561918A
CN105561918A CN201510980768.4A CN201510980768A CN105561918A CN 105561918 A CN105561918 A CN 105561918A CN 201510980768 A CN201510980768 A CN 201510980768A CN 105561918 A CN105561918 A CN 105561918A
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龙英才
林德昌
蔡国君
毕宏达
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Qidong Fuyu New Material Technology Co Ltd
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Abstract

本发明属于纳米材料技术领域，具体为一种负载碘的纳米孔材料及负载碘的方法。本发明负载碘的纳米孔材料，其载体材料为高硅沸石分子筛、微孔磷酸铝或微孔硅磷酸铝分子筛；纳米孔的孔径大于0.3纳米。负载碘的方法包括：从碘蒸汽相吸附的方法，从溶有碘的KI水溶液中吸附的方法，从溶有碘的有机溶剂中吸附的方法。本发明所用的负载材料结构稳定，可以反复使用，非常适合用作为符合第二类碘应用要求的负载材料。负载了碘的这类材料可广泛应用于药用消毒剂、杀菌剂、杀虫剂、医用放射性碘源、以及有机反应催化剂。

Description

负载碘的纳米孔材料和负载碘的方法
技术领域
本发明属于纳米材料技术领域，具体涉及一种负载碘的纳米孔材料及负载碘的方法。
背景技术
碘是一种用途广泛的元素，在医药、照相、橡胶、染料、气象等许多领域都具有广泛的用途。其中，与人民日常生活关系最密切的有加碘盐，医药、卫生的消毒剂、杀菌剂、杀虫剂和脱臭剂，感光材料等。在许多重要的有机合成反应中碘是不可缺少的催化剂和稳定剂，在合成纤维、染料、合成橡胶、人造革等生产过程中起重要作用。碘也是人体的必需微量元素之一，参与新陈代谢的许多方面。
碘是以一种高分散元素，大量的碘存在于海洋中，但浓度低至每升海水平均仅含碘0.06mg。碘主要从海藻灰和某些地区的深井卤水中提取。原子能反应堆中核燃料铀元素的裂变产生大量的放射性碘129，与放射性锶、钡等重元素共存于废水废气中，严重污染环境。但同位素碘又是医疗中有用的元素。在反应堆的废弃核燃料处理工厂中要设法富集和回收。废水废气中无法回收的放射性碘与其它放射性重金属要设法用吸附方法除去、固封后深埋在地底。
元素碘的上述用途、提取、危害、去除等涉及到二种不同类型的负载（即吸附）碘的材料。第一类是用于反应堆废水废气的放射性污染元素的去除。它要求碘的负载量大，且不易解吸脱附，以便进一步固化处理永久封存于地底。中国专利CN201310326820.5报道用13X,5A,Y,BEA等沸石载银脱除反应堆的放射性碘；材料导报2012年11月第26卷专辑20报道Ag、Cd、Cu、Pb、K、Hg、Zn、Mn、Co、Ni等金属改性的NaX、NaA沸石、丝光沸石等含金属及改性的沸石对空气或水蒸气中的放射性碘有很好的吸附作用、去污系数达到103～104，特别是含银量为15.2％的丝光沸石对元素碘的饱和吸附容量可达196．6mg／g。这种用于去除污染的载银沸石，成本很高。
第二类要求负载的碘易于释放，用于药用消毒剂、杀菌剂、杀虫剂、医用放射性碘源、以及催化剂。负载的碘缓慢释放可以提高使用功效、延长使用寿命、并降低其对人体或催化反应的不良作用；提取和富集碘过程所用的该类材料，也要求被吸附的碘易于解吸脱附以便回收。中国专利CN102167390A报道负载碘的水滑石可缓释碘、缓慢生成单质碘释放到溶液体系中，为有机化学反应源源不断提供催化剂所需的单质碘。CN104447588A报道一种有效催化苯甲醛硅氰化反应新型负载碘催化剂Ni-MOF-3。MOF是一种有机-无机杂化骨架型类沸石材料。
显然，上述这二类负载碘的材料都是微孔材料，但应用目的和发挥的功能不尽相同。本发明提出一种符合第二类应用要求的碘负载材料及其负载碘的方法。该材料是高硅沸石分子筛、微孔磷酸铝（ALPO）或微孔硅磷酸铝（SAPO）分子筛，其结构孔径大于0.3纳米。负载碘的方法可以是从碘蒸汽相吸附，或是从含碘的KI水溶液中吸附，也可以从含碘的有机溶剂溶液中吸附。
单质碘I2分子的尺寸约0.27X0.68nm，可以被吸附进入上述发明所涉及的高硅沸石分子筛以及ALPO或SAPO分子筛的孔道中被负载。因高硅沸石分子筛以及ALPO或SAPO分子筛的结构中缺少强电性的阳离子，骨架呈现一定的疏水性质。被负载在孔道中的碘与骨架的作用较弱，仍然保持单分子或分子簇状态，在一定条件下容易脱附或缓慢释放。该类负载材料结构稳定，可以反复使用，非常适合用作为符合第二类碘应用要求的负载材料。负载了碘的这类材料可广泛应用于药用消毒剂、杀菌剂、杀虫剂、医用放射性碘源、以及有机反应催化剂。
发明内容
本发明的目的在于提供一种性能优异、结构稳定的负载碘的纳米孔材料及负载碘的方法。
本发明提供的负载碘的纳米孔材料，其载体材料为高硅沸石分子筛、微孔磷酸铝（ALPO）或微孔硅磷酸铝（SAPO）分子筛；纳米孔的孔径大于0.3纳米。每克载体材料碘的负载量为30-450毫克。
本发明中，所述的高硅沸石分子筛，其骨架结构硅铝摩尔比（SAR）大于6，其结构类型包括：人工合成的FAU（Y）型，MOR（丝光沸石）型，MFI（ZSM-5）型，BEA（Beta）型，FER（镁碱沸石、ZSM-35）型，TON（ZSM-22）型，MRE（ZSM-48）型，CHA(SSZ-13)型，DDR(Decadodecasil3R)型等；还包括矿物沸石分子筛中的丝光沸石（MOR型），斜发沸石（HEU型），辉沸石（STI型），菱沸石（CHA型）等。
本发明中，所述的微孔磷酸铝（ALPO）或微孔硅磷酸铝（SAPO）分子筛，其结构类型包括：CHA(SAPO-34)型，RHO（SAPO-RHO,DNL-6）型，AEI（ALPO-18）型,AFI（ALPO-5和SAPO-5）型，AEL（ALPO-11或SAPO-11）型等。
本发明提出的负载碘的方法，可以是从碘蒸汽相吸附的方法，或是从溶有碘的KI水溶液中吸附的方法，也可以从溶有碘的有机溶剂中吸附的方法。
本发明中，所述的从碘蒸汽相吸附的方法，是将载体材料通过对蒸汽相碘的吸附实现负载，蒸汽相的碘可以是纯碘蒸汽，也可以是空气包括潮湿空气中所含的碘蒸汽。吸附的温度范围是15-100oC，时间1-48h。
本发明中，所述的从溶有碘的KI水溶液中吸附的方法，是将载体材料浸入溶有碘的KI水溶液中，该溶液中KI浓度0.1-2摩尔，碘的含量是1-5%。吸附的温度范围是25-35oC，时间1-10h；载体与溶液的液体/固体重量比是5-15。
本发明中，所述的从溶有碘的有机溶剂中吸附的方法，是将载体材料浸入溶有碘的有机溶剂中，所用有机溶剂可以是甲醇、酒精、二硫化碳或四氯化碳等。碘在有机溶剂中的含量为2-15%，吸附的温度范围为25-30oC，时间为0.5-2h。载体与溶液的液体/固体重量比是5-10。
本发明所用的负载材料结构稳定，可以反复使用，非常适合用作为符合第二类碘应用要求的负载材料。负载了碘的这类材料可广泛应用于药用消毒剂、杀菌剂、杀虫剂、医用放射性碘源、以及有机反应催化剂。
具体实施方式
下面通过具体实施例进一步描述本发明。
实施例1从碘蒸汽相吸附负载碘
在一个形三叉玻璃管的下方一侧底部封闭的支管中放置固体纯碘晶体，另一侧底部封闭的支管中放入粉状纳米微孔负载材料，向上开口的支管用于联通控制气氛的管路。该三叉形管被放置在恒温水浴中，保持一定的负载温度。碘晶体升华产生的碘蒸汽扩散至相联通的另一侧支管中、被纳米微孔负载材料所吸附。在一定的温度下吸附一定时间后的负载了碘的样品，用X光荧光光谱仪（XRF）测定其碘负载量。
吸附气氛控制：空气-常压、相对湿度小于50%；潮湿空气-常压、相对湿度大于90%；
真空-压力0.1托。试验结果见表1。
表1
。
实施例2从溶有碘的KI水溶液中吸附负载碘
在玻璃容器中倒入含一定量碘的KI溶液的，随后称取一定量的粉状纳米微孔负载材料放进该容器。容器置于可加热控温的电磁搅拌器的加热板上。在强烈地搅拌条件下，悬浮于溶液中的纳米微孔负载材料可迅速吸附溶液中所溶解的单质碘。负载试验结束后，经过滤、去离子水洗涤后用丙酮冲洗、空气中室温晾干1小时后用XRF方法测定其碘的负载量。试验结果见表2。
表2
。
实施例3从溶有碘的有机溶剂中吸附负载碘
在有磨口盖的玻璃容器中倒入含一定量含碘有机溶液，随后称取一定量的粉状纳米微孔负载材料放进该容器。容器置于电磁搅拌器板上。在强烈地搅拌条件下，悬浮于溶液中的纳米微孔负载材料可迅速从含碘的有机溶剂中吸附所含的单质碘。负载试验结束后，滤去有机溶剂后的样品，置于空气中0.5-1小时，待表面吸附的有机溶剂挥发后、用XRF方法测定其碘的负载量。试验结果见表3。
表3
。
上述改性辉沸石、丝光沸石、斜发沸石、斜发沸石均为天然。

Claims (7)

1.一种负载碘的纳米孔材料，其特征在于，载体材料为高硅沸石分子筛、微孔磷酸铝或微孔硅磷酸铝分子筛；纳米孔的孔径大于0.3纳米；每克载体材料碘的负载量为30-450毫克。
2.根据权利要求1所述的负载碘的纳米孔材料，其特征在于，所述的高硅沸石分子筛其骨架结构硅铝摩尔比大于6，其结构类型包括：人工合成的FAU（Y）型，MOR（丝光沸石）型，MFI（ZSM-5）型，BEA（Beta）型，FER（镁碱沸石、ZSM-35）型，TON（ZSM-22）型，MRE（ZSM-48）型，CHA(SSZ-13)型，DDR(Decadodecasil3R)型；还包括矿物沸石分子筛中的丝光沸石（MOR型），斜发沸石（HEU型），辉沸石（STI型），菱沸石（CHA型）。
3.根据权利要求1所述的负载碘的纳米孔材料，其特征在于，所述的微孔磷酸铝或微孔硅磷酸铝分子筛，其结构类型包括：CHA(SAPO-34)型，RHO（SAPO-RHO,DNL-6）型，AEI（ALPO-18）型,AFI（ALPO-5或SAPO-5）型，AEL（ALPO-11或SAPO-11）型。
4.如权利要求1-3之一所述的纳米孔材料的负载碘的方法，其特征在于采用下述方法之一种：从碘蒸汽相吸附的方法，从溶有碘的KI水溶液中吸附的方法，从溶有碘的有机溶剂中吸附的方法。
5.根据权利要求4所述的方法，其特征在于，所述的从碘蒸汽相吸附负载碘的方法，是将载体材料通过对蒸汽相碘的吸附实现负载，蒸汽相的碘是纯碘蒸汽，或者是空气包括潮湿空气中所含的碘蒸汽；吸附的温度为15-100oC，时间为1-48h。
6.根据权利要求4所述的方法，其特征在于，所述的从溶有碘的KI水溶液中吸附的方法，是将载体材料浸入溶有碘的KI水溶液中，该溶液中KI浓度为0.1-2摩尔，碘的含量是1-5%；吸附的温度为25-35oC，时间为1-10h；载体与溶液的液/固体重量比是5-15。
7.根据权利要求4所述的方法，其特征在于，所述的从溶有碘的有机溶剂中吸附的方法，是将载体材料浸入溶有碘的有机溶剂中，所用有机溶剂是甲醇、酒精、二硫化碳或四氯化碳；碘在有机溶剂中的含量为2-15%，吸附的温度为25-30oC，时间为0.5-2h；载体与溶液的液体/固体重量比是5-10。
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CN109994239A (zh) * 2019-04-18 2019-07-09 中国科学院长春应用化学研究所 一种用多孔三聚氰胺树脂吸附碘的方法
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