CN113563597A - 一种氢键共价有机气凝胶材料hcoa-1的合成方法 - Google Patents

一种氢键共价有机气凝胶材料hcoa-1的合成方法 Download PDF

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CN113563597A
CN113563597A CN202110888090.2A CN202110888090A CN113563597A CN 113563597 A CN113563597 A CN 113563597A CN 202110888090 A CN202110888090 A CN 202110888090A CN 113563597 A CN113563597 A CN 113563597A
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洪梅
张芳园
李阳雪
贾艾媛
石灿
谭鑫
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Jilin University
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Abstract

一种氢键共价有机气凝胶材料HCOA‑1的合成方法,该方法是:将苯‑1,3,5‑三酰肼溶于有机溶剂二甲基亚砜中,保持其浓度为0.04mol/L,命名为A溶液。将4,4‑联苯二磺酸溶于A溶液中,保持其浓度为0.12mol/L,命名为B溶液。将对苯二甲醛溶于B溶液中,保持其浓度为0.06mol/L,命名为C溶液。将C溶液放置在恒温油浴锅内,100℃加热反应30分钟,得到浅黄色聚合物。将得到的浅黄色聚合物置于透析袋中,以蒸馏水作为透析液,除去有机溶剂,2‑3天后,透析袋内出现明显分层后取出,得到获取物。将得到的获取物倒入烧杯中,随后进行冷冻干燥,得到氢键共价有机气凝胶材料HCOA‑1。HCOA‑1化学稳定性高,合成方法简单,具有多级次孔道,官能团丰富,具有形状可塑性。

Description

一种氢键共价有机气凝胶材料HCOA-1的合成方法
技术领域
本发明属于环境材料与纳米材料制备领域,涉及氢键共价有机气凝胶材料HCOA-1的合成方法。
背景技术
共价有机聚合物(COPs)作为一种新兴的多孔共价有机材料,通过稳定的共价键相连接。由于其具有稳定的结构、高比表面积、大孔隙率、可修饰的结构和易于功能化的特点而受到了关注并被广泛应用于能源、医药和环境领域。COPs通常是由两类单体通过一种共价键构建而成,严重限制了其结构的复杂性和功能的多样性,而制备出具有多功能结构的新型COPs是亟待解决的问题。
本发明通过简单的溶剂热法制备了一种三组分氢键共价有机气凝胶HCOA-1。优势在于:(1)引入带磺酸基团的芳烃,使合成的HCOA-1在具有共价键优点的同时具有氢键作用的活性位点,氢键的存在有利于提高HCOA-1的吸附性能;(2)氧和硫原子的极化作用引起的偶极-偶极相互作用可以使所制备的HCOA-1具有较高的吸附亲和力;(3)氢键和共价键的共同作用,打破了单纯共价键的限制,为构建具有多级次孔道的COPs材料提供了更多的可能性。
发明内容
本发明的目的在于提供一种氢键共价有机气凝胶HCOA-1的合成方法,包括以下步骤:
步骤一:将苯-1,3,5-三酰肼溶于有机溶剂二甲基亚砜中,保持其浓度为0.04mol/L,命名为A溶液;
步骤二:将4,4-联苯二磺酸溶于A溶液中,保持其浓度为0.12mol/L,命名为B溶液;
步骤三:将对苯二甲醛溶于B溶液中,保持其浓度为0.06mol/L,命名为C溶液;
所述C溶液中摩尔比为:苯-1,3,5-三酰肼:4,4-联苯二磺酸:对苯二甲醛=2:6:3;
步骤四:将上述C溶液放置在恒温油浴锅内,100℃加热反应30分钟,得到浅黄色聚合物;
步骤五:将步骤四得到的浅黄色聚合物置于透析袋中,以蒸馏水作为透析液,除去有机溶剂,2-3天后,透析袋内出现明显分层后取出,得到获取物;
步骤六:将步骤五得到的获取物倒入烧杯中,在低温条件下冷冻,随后进行冷冻干燥,得到氢键共价有机气凝胶材料HCOA-1。
氢键共价有机气凝胶材料HCOA-1的结构式如下:
本发明的有益效果在于:
本发明合成方法得到的氢键共价有机聚合物材料HCOA-1化学稳定性高,合成方法简单,具有多级次孔道,官能团丰富,形状可塑性。
附图说明
图1是本发明的氢键共价有机气凝胶材料HCOA-1的合成示意图。
图2是本发明合成的HCOA-1的粉末X-射线衍射谱图;
图3是本发明合成的HCOA-1的扫描电子显微镜照片;
图4是本发明合成的HCOA-1的傅里叶变换-红外光谱图;
图5是本发明合成的HCOA-1在氮气气氛下的热重曲线;
图6是本发明合成的HCOA-1的氮气吸脱附曲线;
图7是本发明合成的HCOA-1的X射线光电子能谱测量光谱分析图。
具体实施方式
合成HCOA-2所使用的原料均为商业可得产品。
如图1所示,一种氢键共价有机聚合物材料HCOA-1的合成方法,包括以下步骤:
步骤一:将苯-1,3,5-三酰肼溶于有机溶剂二甲基亚砜中,保持其浓度为0.04mol/L,命名为A溶液;
步骤二:将4,4-联苯二磺酸溶于A溶液中,保持其浓度为0.12mol/L,命名为B溶液;
步骤三:将对苯二甲醛溶于B溶液中,保持其浓度为0.06mol/L,命名为C溶液;
此时,上述C溶液中摩尔比为:苯-1,3,5-三酰肼:4,4-联苯二磺酸:对苯二甲醛=2:6:3;
步骤四:将上述C溶液放置在恒温油浴锅内,100℃加热反应30分钟,得到浅黄色聚合物;
步骤五:将步骤四得到的浅黄色聚合物置于透析袋中,以蒸馏水作为透析液,除去有机溶剂,2-3天后,透析袋内出现明显分层后取出,得到获取物;
步骤六:将步骤五得到的获取物倒入烧杯中,在低温条件下冷冻,随后进行冷冻干燥,得到氢键共价有机气凝胶材料HCOA-1。
本发明合成的HCOA-1的粉末X-射线衍射谱图如图2所示。
本发明合成的HCOA-1的扫描电子显微镜照片如图3所示。
本发明合成的HCOA-1的傅里叶变换-红外光谱图如图4所示。
本发明合成的HCOA-1在氮气气氛下的热重曲线如图5所示。
本发明合成的HCOA-1的氮气吸脱附曲线如图6所示。
本发明合成的HCOA-1的X射线光电子能谱测量光谱分析如图7所示。

Claims (1)

1.一种氢键共价有机气凝胶材料HCOA-1的合成方法,其特征在于:包括以下步骤:
步骤一:将苯-1,3,5-三酰肼溶于有机溶剂二甲基亚砜中,保持其浓度为0.04mol/L,命名为A溶液;
步骤二:将4,4-联苯二磺酸溶于A溶液中,保持其浓度为0.12mol/L,命名为B溶液;
步骤三:将对苯二甲醛溶于B溶液中,保持其浓度为0.06mol/L,命名为C溶液;
所述C溶液中摩尔比为:苯-1,3,5-三酰肼:4,4-联苯二磺酸:对苯二甲醛=2:6:3;
步骤四:将上述C溶液放置在恒温油浴锅内,100℃加热反应30分钟,得到浅黄色聚合物;
步骤五:将步骤四得到的浅黄色聚合物置于透析袋中,以蒸馏水作为透析液,除去有机溶剂,2-3天后,透析袋内出现明显分层后取出,得到获取物;
步骤六:将步骤五得到的获取物倒入烧杯中,在低温条件下冷冻,随后进行冷冻干燥,得到氢键共价有机气凝胶材料HCOA-1。
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Cited By (1)

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CN115646463A (zh) * 2022-11-01 2023-01-31 吉林大学 基于竞争吸附的多组分共价有机聚合物修复左氧氟沙星污染地下水的原位注入方法

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CN110951075A (zh) * 2019-12-13 2020-04-03 吉林大学 一种氢键共价有机聚合物材料hcop-6的合成方法
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CN110951075A (zh) * 2019-12-13 2020-04-03 吉林大学 一种氢键共价有机聚合物材料hcop-6的合成方法
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Application publication date: 20211029