CN106582461A - 一种氮化碳水凝胶及其制备方法 - Google Patents
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Abstract
本发明公开了一种氮化碳水凝胶及其制备方法。所述凝胶由高分散的氮化碳、聚合物单体N,N‑二甲基丙烯酰胺和交联剂N,N’‑亚甲基双丙烯酰胺共同组成,在光引发条件下,半导体氮化碳材料产生光生电子和空穴,并与丰富的水反应生成大量的羟基自由基,再与高分子单体和交联剂发生聚合反应,形成氮化碳水凝胶。该氮化碳水凝胶具有良好的机械强度和形变恢复的能力,并拥有独特的亲水性和紫外光响应。充分利用水凝胶的溶胀特性,将其应用在水污染治理可以发现:氮化碳水凝胶对阳离子染料,如亚甲基蓝(MB)具有突出的吸附和降解作用。
Description
技术领域
本发明涉及一种氮化碳水凝胶材料的设计制备及应用,属于纳米材料应用领域。
背景技术
近年来,水凝胶是研究最为广泛的软材料之一,并且普遍存在于自然界中。它是以水为分散介质的凝胶,具有网状交联结构的水溶性高分子中引入一部分疏水基团和亲水残基,亲水残基与水分子结合,将水分子连接在网状内部,而疏水残基遇水膨胀的交联聚合物。是一种高分子网络体系,性质柔软,能保持一定的形状,能吸收大量的水。作为一种高吸水高保水材料,水凝胶被广泛用于各个领域,如干旱地区的抗旱、化妆品中的面膜、农用薄膜、调湿剂、原油或成品油的脱水、矿业中的抑尘剂、食品中的保鲜剂和增稠剂、医疗中的药物载体等等。2013年美国约翰·霍普金斯大学医学院报告称:一种新型水凝胶生物材料可以用于软骨修复手术中,它能够帮助刺激病人骨髓产生干细胞,长出新的软骨;加拿大最新的研究显示,水凝胶不仅有利于干细胞移植,也可加速眼睛与神经损伤的修复。除此之外,它还可以作为隐形眼镜的主要材料普遍存在于我们的生活当中。
石墨相氮化碳(g-C3N4)以其特有的层状类石墨烯结构而引起了广泛关注。作为一种新型有机聚合物半导体材料,其带隙为2.7 eV,可以吸收可见光,其层与层之间以范德华力相连,具有较好的化学与热力学稳定性,同时价格低廉,制备简单,被公认为是一种非常具有发展潜力的环境友好,可持续使用的新型可见光催化材料。
最近, Zhang等人采用二氧化碳作为引发剂成功制备了氮化碳水凝胶。但其做采用的氮化碳原料均来自于难分散的块状传统氮化碳(由三聚氰胺直接煅烧制得),十分不利于水凝胶的均匀生长 [Zhang Y, Zhou Z, Shen Y, Zhou Q, Wang J, Liu A, Liu S,Zhang Y. Reversible assembly of graphitic carbon nitride 3D network forhighly selective dyes absorption and regeneration. ACS Nano, 2016, 10, 9036-9043]。为解决上述问题,该课题组采用了氢氧化钠对其表面进行修饰,提高溶解性的同时,却因强碱的引入使其难以降解碱性染料(如亚甲基蓝等)。因此,对碱性染料有突出吸附和降解作用的氮化碳水凝胶还没有被报道。
发明内容
本发明的目的在于提供一种氮化碳水凝胶材料及其制备方法。
实现本发明目的的技术解决方案为:一种氮化碳水凝胶材料,并对碱性染料有突出的吸附和降解作用。
上述氮化碳水凝胶采用以下步骤制备而得:
第一步,将氮化碳均匀地分散在水溶液中;
第二步,将第一步所制得的氮化碳水溶液与聚合物单体(N,N-二甲基丙烯酰胺)和交联剂(N,N’-亚甲基双丙烯酰胺)混合,超声并搅拌均匀得到混合溶液;
第三步,向第二步的混合溶液中通入氮气,对溶解氧进行置换,再用注射器吸取;
第四步,将注射器垂直放置到白色LED灯(功率为50-200W)下,并与光源保持一定距离(5-10 cm),照射直至溶液变成凝胶。
本发明氮化碳水凝胶的制备方法,第一步中所述的氮化碳采用超分子预组装的方法制备,具有良好的分散性,其水溶液浓度为0.001-0.01 wt%。
本发明氮化碳水凝胶的制备方法中,第二步混合溶液中,聚合物单体(N,N-二甲基丙烯酰胺)的质量浓度为1-10 wt%,交联剂(N,N’-亚甲基双丙烯酰胺)的质量为0.01-0.1wt%,氮化碳水溶液、N,N-二甲基丙烯酰胺和N,N’-亚甲基双丙烯酰胺三者之间的质量比为1100:100:1;超声时间为5-10 min。
本发明氮化碳水凝胶的制备方法中,第三步中氮气通入时间为1-5 min,一共置换3次,抽取溶液时尽量避免气泡的产生。
本发明氮化碳水凝胶的制备方法种,第四步中白色LED灯功率为50-200W,注射器与光源的距离为5-10 cm。
本发明与现有技术相比,其优点在于:(1)超分子预组装的方法制备的氮化碳具有良好的分散性,有利于形成均匀的氮化碳水凝胶;(2)制备过程中采用光引发的技术以水为溶剂,具有绿色无污染的特点;(3)采用注射器为反应容器可以大幅度降低反应成本,简单易操作;(4)微量氮化碳也可以得到有效应用,对碱性染料有突出的吸附和降解作用;(5)氮化碳水凝胶具有很好生物相容性,并且对人体无毒无害,有希望应用于仿生材料的研究;(6)氮化碳水凝胶具有突出的荧光效应,可以用于生物标记。
附图说明
图1是本发明实例1所制备的氮化碳水凝胶的制备方法示意图。
图2是本发明超分子预组装法制得的氮化碳的场发射扫描电镜(a为低倍数,b为高倍数)。
图3是本发明实例1所制备的氮化碳水凝胶的冷冻场发射扫描电镜(a为低倍数,b为高倍数)。
图4是本发明实例1所制备的氮化碳水凝胶的机械性能研究。
图5 a是氮化碳水凝胶对不同染料的吸附性能研究;b是氮化碳水凝胶的光催化性能研究。
具体实施方式
本发明的氮化碳水凝胶通过以下步骤制备:
第一步,将氮化碳均匀地分散在水溶液中;
第二步,将第一步所制得的氮化碳水溶液(氮化碳含量为0.001-0.01 wt%)与聚合物单体(N,N-二甲基丙烯酰胺,1-8 wt%)和交联剂(N,N’-亚甲基双丙烯酰胺,0.01-0.08 wt%)混合,超声并搅拌;
第三步,向第二步的混合溶液中通入氮气,对溶解氧进行置换,再用注射器吸取一定量的混合溶液;
第四步,将注射器垂直放置到白色LED灯(功率为50-200W)下,并与光源保持一定距离(5-10 cm),照射直至溶液变成凝胶。
实施实例1:
第一步:将1 mg氮化碳在100 mL去离子水中进行超声分散24 h,得到氮化碳水溶液;
第二步,将400 mg N,N-二甲基丙烯酰胺和4 mg N,N’-亚甲基双丙烯酰胺溶解在4.6 g的氮化碳水溶液中,超声5-10分钟;
第三步,向上述混合溶液中通入氮气,对溶解氧进行置换,再用5 ml的圆柱形注射器吸取一定量的混合溶液;
第四步,将注射器垂直放置到白色LED灯(功率为50-200W)下,并与光源保持一定距离(5-10 cm),照射直至溶液变成凝胶。
本发明所采用的制备过程如图1所示。
实施实例2:
第一步:将2 mg氮化碳在100 mL去离子水中进行超声分散24 h,得到氮化碳水溶液;
第二步,将400 mg N,N-二甲基丙烯酰胺和4 mg N,N’-亚甲基双丙烯酰胺溶解在 4.6g的氮化碳水溶液中,超声5-10分钟;
第三步,向上述混合溶液中通入氮气,对溶解氧进行置换,再用5 ml的圆柱形注射器吸取一定量的混合溶液;
第四步,将注射器垂直放置到白色LED灯(功率为50-200W)下,并与光源保持一定距离(5-10 cm),照射直至溶液变成凝胶。
实施实例3:
第一步:将3 mg氮化碳在100 mL去离子水中进行超声分散24 h,得到氮化碳水溶液;
第二步,将400 mg N,N-二甲基丙烯酰胺和4 mg N,N’-亚甲基双丙烯酰胺溶解在 4.6g的氮化碳水溶液中,超声5-10分钟;
第三步,向上述混合溶液中通入氮气,对溶解氧进行置换,再用5 ml的圆柱形注射器吸取一定量的混合溶液;
第四步,将注射器垂直放置到白色LED灯(功率为50-200W)下,并与光源保持一定距离(5-10 cm),照射直至溶液变成凝胶。
第五步,将上述凝胶应用染料的光降解研究,具体步骤如下:将制得的水凝胶切成0.5 mL的圆柱体,再分别加入5 mL亚甲基蓝(MB)、甲基橙(MO)或者罗丹名B(RhB)(浓度均为10 mg/L),暗室条件下进行吸附,5 h后达到吸附平衡,通过紫外-可见分光光度计确定吸附量,再将溶液置于可见光下,对凝胶的光催化性能进行研究。结果表明本发明所制备的氮化碳水凝胶具有良好的吸附和光催化活性,尤其是对碱性染料亚甲基蓝的降解。
本发明所采用超分子预组装法制备的氮化碳如图2所示;本发明制得的氮化碳水凝胶的冷冻扫描电镜如图3;图4是氮化碳水凝胶的机械性能研究;图5a是氮化碳水凝胶对不同染料的吸附性能研究,图5b是氮化碳水凝胶的光催化性能研究。
Claims (7)
1.一种氮化碳水凝胶的制备方法,其特征在于,包括如下步骤:
第一步,将氮化碳均匀地分散在水溶液中;
第二步,将第一步所制得的氮化碳水溶液与聚合物单体和交联剂混合,超声并搅拌均匀得到混合溶液;
第三步,向第二步的混合溶液中通入氮气,对溶解氧进行置换,再用注射器吸取;
第四步,将注射器垂直放置到白色LED灯下,并与光源保持一定距离,照射直至溶液变成凝胶。
2.根据权利要求1所述的制备方法,其特征在于,第一步中,所述的氮化碳采用超分子预组装的方法制备,氮化碳水溶液浓度为0.001-0.01 wt%。
3.根据权利要求1所述的制备方法,其特征在于,第二步中,聚合物单体采用N,N-二甲基丙烯酰胺,交联剂采用N,N’-亚甲基双丙烯酰胺。
4.根据权利要求1所述的制备方法,其特征在于,第二步中,聚合物单体的质量浓度为1-10 wt%,交联剂的质量浓度为0.01-0.1 wt%,氮化碳水溶液、聚合物单体和交联剂三者之间的质量比为1100:100:1;超声时间为5-10 min。
5.根据权利要求1所述的制备方法,其特征在于,第三步中,氮气通入时间为1-5 min。
6.根据权利要求1所述的制备方法,其特征在于,第四步中,白色LED灯功率为50-200W,注射器与光源的距离为5-10 cm。
7.如权利要求1-6任一所述的制备方法制备的氮化碳水凝胶。
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