CN109320757A - 一种氢键共价有机凝胶材料hcog-1的合成方法 - Google Patents

一种氢键共价有机凝胶材料hcog-1的合成方法 Download PDF

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CN109320757A
CN109320757A CN201811353180.6A CN201811353180A CN109320757A CN 109320757 A CN109320757 A CN 109320757A CN 201811353180 A CN201811353180 A CN 201811353180A CN 109320757 A CN109320757 A CN 109320757A
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covalent organic
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hydrogen bond
terephthalaldehyde
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李阳雪
董军
徐非凡
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Jilin University
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    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/28—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum
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    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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    • B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
    • B01J20/28047—Gels
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    • C08G12/00—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
    • C08G12/02—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes
    • C08G12/04—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with acyclic or carbocyclic compounds
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    • C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
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    • C08J2361/00—Characterised by the use of condensation polymers of aldehydes or ketones; Derivatives of such polymers
    • C08J2361/20—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
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Abstract

一种氢键共价有机凝胶材料HCOG‑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0.02mol/L，命名为A溶液；将对苯二甲醛溶于A溶液中，保持其浓度为0.03mol/L，命名为B溶液，B溶液中各物质的摩尔比为：苯‑1,3,5‑三酰肼：对苯二甲醛＝2：3。将B溶液放置在恒温油浴锅内，100℃加热反应10分钟，得到黄色凝胶；将黄色凝胶置于透析袋中，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，得到氢键共价有机凝胶材料HCOG‑1。HCOG‑1具有非晶态无定型结构，具有优良的热稳定性以及较大的比表面积。

Description

一种氢键共价有机凝胶材料HCOG-1的合成方法
技术领域
本发明属于纳米材料与环境材料制备领域，涉及氢键共价有机凝胶材料HCOG-1的合成方法，其中的HCOG是氢键共价有机凝胶的英文缩写，其中的杠1是编号。
背景技术
多孔有机聚合物(Porous Organic Polymers，POPs),包括结晶态和无定型形态，由于它们在储气，催化，传感和许多其他领域取得了相当大的进步，因此在许多研究人员中一直备受关注。共价有机凝胶(Covalent Organic Gels,COGs)，作为一类多孔有机聚合物，是由中间聚集体诱导的多孔共价有机材料。与以前众所周知的POPs相比，共价有机凝胶的优点包括两个主要方面：①反应时间短和合成产率高；②从微孔到大孔的较广的孔径分布。然而，COG的合理设计仍然是一个很大的挑战。
通常，凝胶机制包括三个步骤，包括：①胺-醛缩合形成COF链；②COF链聚集以符合COF颗粒(COFP)；③COFP的聚集以构建分层的COG结构。在COG形成期间，COFP通过各种非共价相互作用连接在一起，例如弱范德华力、氢键、π-π堆积等，其中，由酰胺，羧酸，羰基产生的氢键在COG的合成中起着重要作用。据我们所知，还没有报道关注由氢键诱导形成的COG。
发明内容
本发明的目的在于提供一种氢键共价有机凝胶材料HCOG-1的合成方法，所制得的HCOG-1材料具有大的比表面积，并具有很好的热稳定性和水溶液稳定性。
一种氢键共价有机凝胶材料HCOG-1的合成方法，包括以下步骤：
步骤一：将苯-1,3,5-三酰肼(BTCH)溶于有机溶剂二甲基亚砜(DMSO)中，保持其浓度为0.02mol/L，命名为A溶液。
步骤二：将对苯二甲醛(TPA)溶于A溶液中，保持其浓度为0.03mol/L，命名为B溶液。
此时，上述B溶液中摩尔比为：苯-1,3,5-三酰肼：对苯二甲醛＝2：3。
步骤三：将上述B溶液放置在恒温油浴锅内，100℃加热反应10分钟，得到黄色凝胶；
步骤四：将步骤三得到的黄色凝胶置于透析袋中，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。
步骤五：将步骤四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，得到氢键共价有机凝胶材料HCOG-1。
本发明的有益效果在于：
本发明合成方法得到的共价有机凝胶材料HCOG-1具有非晶态无定型结构，具有优良的热稳定性以及较大的比表面积。
附图说明
图1是本发明合成的HCOG-1的合成示意图。
图2是本发明合成的HCOG-1的粉末X-射线衍射谱图。
图3是本发明合成的HCOG-1的扫描电子显微镜照片。
图4是本发明合成的HCOG-1的傅里叶变换-红外光谱图。
图5是本发明合成的HCOG-1的固体核磁共振13C CP/MAS谱图。
图6是本发明合成的HCOG-1在氮气气氛下的热重曲线。
图7是本发明合成的HCOG-1的氮气吸脱附曲线。
图8是本发明合成的HCOG-1的流变学测试。
具体实施方式
合成HCOG-1所使用的原料均为商业可得产品。
如图1所示，一种氢键共价有机凝胶材料HCOG-1的合成方法。包括以下步骤：
步骤一：称取50mg苯-1,3,5-三酰肼(BTCH)溶于5mL有机溶剂二甲基亚砜(DMSO)中，保持其浓度为0.02mol/L，命名为A溶液。
步骤二：称取40mg对苯二甲醛(TPA)溶于A溶液中，保持其浓度为0.03mol/L，命名为B溶液。
此时，上述B溶液中摩尔比为：苯-1,3,5-三酰肼：对苯二甲醛＝2：3。
步骤三：将上述B溶液放置在恒温油浴锅内，100℃加热反应10分钟，得到黄色凝胶。
步骤四：将步骤三得到的黄色凝胶置于透析袋中，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。
步骤五：将步骤四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，得到氢键共价有机凝胶材料HCOG-1。
本发明合成的HCOG-1的粉末X-射线衍射谱图如图2所示。
本发明合成的HCOG-1的扫描电子显微镜照片如图3所示。
本发明合成的HCOG-1的傅里叶变换-红外光谱如图4所示。
本发明合成的HCOG-1的固体核磁共振13C CP/MAS谱如图5所示。
本发明合成的HCOG-1在氮气气氛下的热重曲线如图6所示。
本发明合成的HCOG-1的氮气吸脱附曲线如图7所示。
本发明合成的HCOG-1的流变学测试如图8所示。
本发明合成的HCOG-1材料优势在于：
1、非晶态无定型结构，较大的比表面积，对污染物具有强吸附性
2、具有优良的热稳定性。

Claims (1)

1.一种氢键共价有机凝胶材料HCOG-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0.02mol/L，命名为A溶液；
步骤二：将对苯二甲醛溶于A溶液中，保持其浓度为0.03mol/L，命名为B溶液；
此时，上述B溶液中摩尔比为：苯-1,3,5-三酰肼：对苯二甲醛＝2：3；
步骤三：将上述B溶液放置在恒温油浴锅内，100℃加热反应10分钟，得到黄色凝胶；
步骤四：将步骤三得到的黄色凝胶置于透析袋中，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；
步骤五：将步骤四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，得到氢键共价有机凝胶材料HCOG-1。
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CN113058567A (zh) * 2021-02-09 2021-07-02 深圳世纪盛源环境科技有限公司 氢键诱导的高稳定性多孔共价有机凝胶材料及其制备方法
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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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CN113402730A (zh) * 2021-08-04 2021-09-17 吉林大学 一种氢键共价有机气凝胶材料hcoa-2的合成方法

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Application publication date: 20190212