CN109467714A - 一种磁性复合金属-有机骨架材料及其应用 - Google Patents
一种磁性复合金属-有机骨架材料及其应用 Download PDFInfo
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Abstract
本发明公开了一种磁性复合金属‑有机骨架材料，制备方法包括以下步骤：取九水合硝酸铁、四水合硝酸铟和咪唑‑4,5‑二羧酸溶解于N,N‑二甲基甲酰胺溶液中,在上述溶液中加入苯并咪唑，搅拌均匀，将上述混合溶液转移至圆底烧瓶中，加热至反应，通过离心分离收集产物，然后用工业酒精将产物洗涤数次，烘干得到铁‑铟基MOF前驱体；取铁‑铟基MOF前驱体于烧瓶中，加入蒸馏水，超声处理，缓慢加入聚碳酸酯，磁力搅拌，待其分散均匀后，升温至30℃水浴反应2h，反应结束后强磁分离，分离得到的固体用蒸馏水和乙醇分别洗涤3次，即得聚碳酸酯化铁‑铟基复合金属‑有机骨架材料。
Description
技术领域
本发明涉及一种磁性复合金属-有机骨架材料及其应用,属于化工合成领域。
背景技术
金属有机骨架材料（MOFs），又称金属配位聚合物，是指以无机金属或金属簇与含氮氧多齿有机配体通过配位键连接而形成的晶体材料，是一类具有高比表面积、可调变孔道尺寸，有机功能化的多孔材料。由于MOFs材料可以根据不同磁性氧化物大小从而选择不同的有机配体和金属离子搭建不同大小和结构的孔道，所以近几年选择MOFs材料作为载体负载磁性氧化物受到了越来越多关注，
金属有机骨架材料（MOFs）在催化、吸附、分离等方面有广泛的应用，MOFs作为催化剂研究较多的是一些固-液相的催化反应,但但MOFs作为催化剂时,在催化剂的分离和回收上还存在一些问题,例如催化剂与反应溶液的高速离心分离能耗比较高,并且在分离过程中难免会损失一些催化剂,这对催化反应工艺都是不利的。
如果在磁性核上原位合成一层MOFs,制备出磁性的MOFs催化剂,就可以利用磁性材料在外磁场下容易分离的特性,简化催化反应的分离过程,减少催化剂的损失。
发明内容
本发明的目的在于提供一种磁性复合金属-有机骨架材料，具有较大的比较面积和特殊的孔道，作为催化剂具有很好的效果，容易分离，
制备方法包括以下步骤：
取九水合硝酸铁、四水合硝酸铟和咪唑-4,5-二羧酸溶解于N,N-二甲基甲酰胺溶液中,在上述溶液中加入苯并咪唑，搅拌均匀，将上述混合溶液转移至圆底烧瓶中，加热至120℃，反应4h，通过离心分离收集产物，然后用工业酒精将产物洗涤数次，烘干得到铁-铟基MOF前驱体；
取铁-铟基MOF前驱体于烧瓶中，加入蒸馏水，超声处理，缓慢加入聚碳酸酯，在50rmp转速下磁力搅拌1h，待其分散均匀后，升温至30℃水浴反应2h，反应结束后强磁分离，分离得到的固体用蒸馏水和乙醇分别洗涤3次，即得聚碳酸酯化铁-铟基复合金属-有机骨架材料。
有益效果：本发明为聚碳酸酯化铁-铟基复合金属-有机骨架材料具有无定形的、孔道杂乱的状态转化成为高度结晶、孔道有序的共价有机框架,获得具有优异多孔性质的共价有机框架复合微球，该复合微球具有尺寸均一、高分散性以及高度有序多孔性等特点,从而使纳米催化剂形成多孔高比表面积的形态，饱和磁性好，能达到50以上的emug-1，
在液相催化反应,中与反应产物可以很容易地用外加磁场进行分离，这可以提高液相催化反应的催化剂重复使用效率，减少液相催化反应的分离成本,特别是用于乙烯与苯液相烷基化反应具有很好的催化效果。
具体实施方式
实施例1
一种磁性复合金属-有机骨架材料，其特征在于该方法,包括以下步骤：
取九水合硝酸铁3g、四水合硝酸铟（2g）和咪唑-4,5-二羧酸（5g）溶解于N,N-二甲基甲酰胺（600ml）溶液中,在上述溶液中加入苯并咪唑，搅拌均匀，将上述混合溶液转移至圆底烧瓶中，加热至120℃，反应4h，通过离心分离收集产物，然后用工业酒精将产物洗涤数次，烘干得到铁-铟基MOF前驱体；
取1g铁-铟基MOF前驱体于烧瓶中，加入10ml蒸馏水，超声处理15min，缓慢加入5g聚碳酸酯，在50rmp转速下磁力搅拌1h，待其分散均匀后，升温至30℃水浴反应2h，反应结束后强磁分离，分离得到的固体用蒸馏水和乙醇分别洗涤3次，即得聚碳酸酯化铁-铟基复合金属-有机骨架材料。饱和磁化强度为92emug-1，
使用该实施例为催化剂，反应温度220℃下，乙烯转化率为99.9％乙苯选择性为97.1％，催化剂重复循环使用3次，对乙烯转化率没有明显下降，催化剂基本没有损失。
实施例2
取九水合硝酸铁1g、四水合硝酸铟2g和咪唑-4,5-二羧酸5g溶解于N,N-二甲基甲酰胺（600ml）溶液中,在上述溶液中加入苯并咪唑，搅拌均匀，将上述混合溶液转移至圆底烧瓶中，加热至120℃，反应4h，通过离心分离收集产物，然后用工业酒精将产物洗涤数次，烘干得到铁-铟基MOF前驱体；
取1g铁-铟基MOF前驱体于烧瓶中，加入10ml蒸馏水，超声处理15min，缓慢加入5g聚碳酸酯，在50rmp转速下磁力搅拌1h，待其分散均匀后，升温至30℃水浴反应2h，反应结束后强磁分离，分离得到的固体用蒸馏水和乙醇分别洗涤3次，即得聚碳酸酯化铁-铟基复合金属-有机骨架材料。饱和磁化强度为65emug-1
使用该实施例为催化剂，反应温度220℃下，乙烯转化率为94.1％， 乙苯选择性为92.1％，催化剂重复循环使用3次，对乙烯转化率没有明显下降，催化剂基本没有损失。
实施例3
取九水合硝酸铁2g、四水合硝酸铟（2g）和咪唑-4,5-二羧酸（5g）溶解于N,N-二甲基甲酰胺（600ml）溶液中,在上述溶液中加入苯并咪唑，搅拌均匀，将上述混合溶液转移至圆底烧瓶中，加热至120℃，反应4h，通过离心分离收集产物，然后用工业酒精将产物洗涤数次，烘干得到铁-铟基MOF前驱体；
取1g铁-铟基MOF前驱体于烧瓶中，加入10ml蒸馏水，超声处理15min，缓慢加入5g聚碳酸酯，在50rmp转速下磁力搅拌1h，待其分散均匀后，升温至30℃水浴反应2h，反应结束后强磁分离，分离得到的固体用蒸馏水和乙醇分别洗涤3次，即得聚碳酸酯化铁-铟基复合金属-有机骨架材料。饱和磁化强度为58emug-1
使用该实施例为催化剂，在乙烯与苯液相烷基化反应中，反应温度220℃下，乙烯转化率为96.8％， 乙苯选择性为95.3％，催化剂重复循环使用3次，对乙烯转化率没有明显下降，催化剂基本没有损失。。
对照例1
取九水合硝酸铁3g和咪唑-4,5-二羧酸（5g）溶解于N,N-二甲基甲酰胺（600ml）溶液中,在上述溶液中加入苯并咪唑，搅拌均匀，将上述混合溶液转移至圆底烧瓶中，加热至120℃，反应4h，通过离心分离收集产物，然后用工业酒精将产物洗涤数次，烘干得到铁基MOF前驱体。饱和磁化强度为54emug-1，
使用该实施例为催化剂，在乙烯与苯液相烷基化反应中，反应温度220℃下，乙烯转化率为72.8％， 乙苯选择性为65.3％，催化剂重复循环使用3次，对乙烯转化率明显下降，催化剂略损失。
对照例2
取九水合硝酸铁3g、四水合硝酸铟（2g）和咪唑-4,5-二羧酸（5g）溶解于N,N-二甲基甲酰胺（600ml）溶液中,在上述溶液中加入苯并咪唑，搅拌均匀，将上述混合溶液转移至圆底烧瓶中，加热至120℃，反应4h，通过离心分离收集产物，然后用工业酒精将产物洗涤数次，烘干得到铁-铟基MOF前驱体；
取1g铁-铟基MOF前驱体于烧瓶中，加入10ml蒸馏水，超声处理15min在50rmp转速下磁力搅拌1h，待其分散均匀后，升温至30℃水浴反应2h，反应结束后强磁分离，分离得到的固体用蒸馏水和乙醇分别洗涤3次，即得铁-铟基复合金属-有机骨架材料。饱和磁化强度为62emug-1，
使用该实施例为催化剂，反应温度220℃下，乙烯转化率为90.9％， 乙苯选择性为89.1％，催化剂重复循环使用3次，对乙烯转化率下降，催化剂略有损失。
Claims (3)
1.一种磁性复合金属-有机骨架材料，其特征在于该材料制备方法包括以下步骤：
取九水合硝酸铁、四水合硝酸铟和咪唑-4,5-二羧酸溶解于N,N-二甲基甲酰胺溶液中,在上述溶液中加入苯并咪唑，搅拌均匀，将上述混合溶液转移至圆底烧瓶中，加热至120℃，反应4h，通过离心分离收集产物，然后用工业酒精将产物洗涤数次，烘干得到铁-铟基MOF前驱体；
取铁-铟基MOF前驱体于烧瓶中，加入蒸馏水，超声处理，缓慢加入聚碳酸酯，在50rmp转速下磁力搅拌1h，待其分散均匀后，升温至30℃水浴反应2h，反应结束后强磁分离，分离得到的固体用蒸馏水和乙醇分别洗涤3次，即得聚碳酸酯化铁-铟基复合金属-有机骨架材料。
2.根据权利要求1所述一种磁性复合金属-有机骨架材料，其特征在于, 所述的九水合硝酸铁、四水合硝酸铟质量比为1:5-5:1。
3.权利要求1所述的磁性复合金属-有机骨架材料用于乙烯与苯液相烷基化反应的催化剂。
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