CN106423280A - 一种阳离子有机聚合物的制备及催化二氧化碳固定的方法 - Google Patents
一种阳离子有机聚合物的制备及催化二氧化碳固定的方法 Download PDFInfo
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Abstract
本发明涉及一种Salen‑Al为基础的双功能阳离子多孔有机聚合物的制备及催化二氧化碳固定为环状碳酸酯的方法。这类双功能阳离子多孔有机聚合物催化剂由Salen‑Al配体和2,4,6‑三(咪唑‑1‑基)‑1,3,5‑三嗪组成，通过偶联反应制备而成，该催化剂制备简单，并具有较高活性、较高选择性的催化二氧化碳与烯烃环氧化物反应，催化剂与产物分离简单，能多次循环使用。
Description
技术领域
本发明属于二氧化碳固定催化剂技术领域，具体涉及一种由Salen-Al合成双功能阳离子多孔有机聚合物催化剂Al-CPOP的制备方法，和催化二氧化碳固定位环状碳酸酯反应的应用。
背景技术
环状碳酸酯是一种非常重要的合成中间体，性能优良的有机溶剂，可溶解多种聚合物；另可作为有机中间体，可替代环氧乙烷用于二氧基化反应，并是酯交换法生产碳酸二甲酯的主要原料；还可用作合成呋喃唑酮的原料、水玻璃系浆料、纤维整理剂等；此外，还应用于锂电池电解液中。但是传统的环状碳酸酯生产的过程中，会产生多种副产物，同时传统的均相催化剂有难分离、易分解和无法循环使用等缺点，会极大的增加产物后处理的难度和时间资金投入。因此人们努力通过催化剂的固定来实现均相催化剂异相化来解决以上问题。目前，一般是将Salen类催化剂负载到分子筛等硅类无机材料或者将Salen-Al做成配体制备成金属有机框架(MOF)。但这两类方法中，前者需要大量载体，负载量不高，循环性能不好，后者由于是配位作用形成的框架，而且MOF里面的溶剂分子一旦失去有可能造成框架坍塌，所以不稳定。而多孔有机聚合物由于其易于合成，具有大的比表面积，在催化等领域具有潜在的应用价值，成为近年来研究的热点。
发明内容
本发明的目的是提出了通过偶联反应制备一种双功能阳离子多孔有机聚合物催化剂及其应用。
本发明提出的双功能阳离子多孔有机聚合物催化剂制备方法，其制备过程如下：
配备有蛇形冷凝管的三颈烧瓶中加入Salen-Al配体和2,4,6-三(咪唑-1-基)-1,3,5-三嗪，反应全程氮气氛围中，以N,N-二甲基甲酰胺和乙醇为溶剂，110℃回流反应48小时。反应完成后，离心，真空干燥箱干燥，甲醇索氏提取24小时，真空干燥箱干燥，得到双功能阳离子多孔有机聚合物催化剂Al-CPOP。
本发明提出的Al-CPOP催化剂催化二氧化碳固定为环状碳酸酯反应步骤如下：向反应体系中分别加入烯烃环氧化物和催化剂Al-CPOP，两者的物质的量(其中Al-CPOP以聚合物中的金属的含量作为物质的量计算标准)之比为1:0.01，二氧化碳压力维持为0.1MPa，反应温度120℃，反应24小时后，离心，催化剂用丙酮洗涤，真空干燥箱中烘干12小时，循环使用；液相部分用无水硫酸钠干燥，柱层析分离得到相应的产物环状碳酸酯。
附图说明
图1为所得催化剂透射电镜图。
图2为所得催化剂扫描电镜图。
图3为所得催化剂的结构图。
具体实施方式
实施例1：Al-CPOP催化剂
配备有蛇形冷凝管的三颈烧瓶中加入Salen-Al配体和2,4,6-三(咪唑-1-基)-1,3,5-三嗪，反应全程氮气氛围中，以N,N-二甲基甲酰胺和乙醇为溶剂，110℃回流反应48小时。反应完成后，离心，真空干燥箱干燥，甲醇索氏提取24小时，真空干燥箱干燥，得到双功能阳离子多孔有机聚合物催化剂Al-CPOP。
实施例2：Al-CPOP催化剂催化二氧化碳固定为环状碳酸酯反应
向反应体系中分别加入环氧氯丙烷和催化剂Al-CPOP，两者的物质的量(其中Al-CPOP以聚合物中的金属的含量作为物质的量计算标准)之比为1:0.01，二氧化碳压力维持为0.1MPa，反应温度120℃，反应24小时后，离心，催化剂用丙酮洗涤，真空干燥箱中烘干12小时，循环使用；液相部分用无水硫酸钠干燥，柱层析分离得到相应的产物环状碳酸酯。
实施例3：Al-CPOP催化剂催化二氧化碳固定为环状碳酸酯反应
向反应体系中分别加入环氧丙烷和催化剂Al-CPOP，两者的物质的量(其中Al-CPOP以聚合物中的金属的含量作为物质的量计算标准)之比为1:0.01，二氧化碳压力维持为0.1MPa，反应温度120℃，反应24小时后，离心，催化剂用丙酮洗涤，真空干燥箱中烘干12小时，循环使用；液相部分用无水硫酸钠干燥，柱层析分离得到相应的烯烃环氧化反应产物。
实施例4：Al-CPOP催化剂催化烯烃环氧化反应
向反应体系中分别加入环氧苯乙烯和催化剂Al-CPOP，两者的物质的量(其中Al-CPOP以聚合物中的金属的含量作为物质的量计算标准)之比为1:0.01，二氧化碳压力维持为0.1MPa，反应温度120℃，反应24小时后，离心，催化剂用丙酮洗涤，真空干燥箱中烘干12小时，循环使用；液相部分用无水硫酸钠干燥，柱层析分离得到相应的烯烃环氧化反应产物。
表1Al-CPOP对多种底物的催化活性
Claims (5)
1.一种双功能阳离子多孔有机聚合物类催化剂，命名为Al-CPOP，以Salen-Al配体和2,4,6-三(咪唑-1-基)-1,3,5-三嗪偶联得到以双催化活性中心Salen-Al和咪唑鎓盐为基础的聚合物类催化剂。
2.一种如权利要求1所述的催化剂的制备方法，包括以下步骤：
(1)Salen单体和结晶氯化铝按照一定量和比例，以乙醇和氯仿为溶剂，在80℃氮气氛围中回流反应一天，其后水洗并于真空干燥箱中70℃烘24小时得到Salen-Al配体；
(2)Salen-Al配体和2,4,6-三(咪唑-1-基)-1,3,5-三嗪在氮气氛围中，以N,N-二甲基甲酰胺和乙醇为溶剂，110℃反应48小时，离心，真空干燥箱烘干，用甲醇索氏提取24小时，真空干燥箱干燥，得到Al-CPOP。
3.如权利要求2所述的方法，其特征在于：所述步骤(1)中，Salen单体和结晶氯化铝用量比为1:1.2，溶剂乙醇和氯仿比例为1:1。
4.如权利要求2所述的方法，其特征在于：所述步骤(2)中，Salen-Al配体和2,4,6-三(咪唑-1-基)-1,3,5-三嗪用量比为1:1.2，溶剂N,N-二甲基甲酰胺和乙醇用量比为1:1。
5.一种如权利要求1所述的催化剂催化二氧化碳固定为环状碳酸酯反应中的应用，其特征在于具体步骤如下：向反应体系中分别加入烯烃环氧化物和催化剂Al-CPOP，两者的物质的量之比为1:0.01，其中Al-CPOP以聚合物中的金属的含量作为物质的量计算标准；二氧化碳的压力维持0.1MPa，反应温度120℃，反应24小时后，离心，催化剂用丙酮洗涤，真空干燥箱中烘干12小时，循环使用；液相部分用无水硫酸钠干燥，柱层析分离得到相应的反应产物环状碳酸酯。
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