CN107308986A - 一种具有光催化活性气凝胶微球的制备方法 - Google Patents
一种具有光催化活性气凝胶微球的制备方法 Download PDFInfo
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Abstract
本发明公开了一种具有光催化活性的气凝胶微球的制备方法,属于气凝胶光催化剂制备、化学化工领域,其目的在于制备具有光催化活性的气凝胶微球,以提高粉末催化剂的光催化活性、稳定性及循环使用性,拓宽催化剂种类。本文以氧化银为光催化剂和交联剂,选用黏土和海藻酸钠为载体,制备了具有光催化活性的气凝胶微球。所制备的气凝胶微球可以循环光催化降解废水中的染料。本发明的优点在于所选用的海藻酸钠和黏土分别为天然聚合物和矿物,既廉价又环保,制备条件低、设备简单,所得的产品具有生物兼容性、光催化活性,可用于废水处理,在环境保护、化学化工领域具有广泛的应用前景。
Description
技术领域
本发明公开了一种新型气凝胶微球光催化剂,具体涉及一种具有光催化活性的气凝胶微球的制备方法,属于高分子气凝胶微球制备、光催化、化学化工领域。
背景技术
气凝胶是指凝胶的网状结构中充满气体的多孔性非晶固体材料。气凝胶中的孔结构具有开孔性和相互连通性,气体或者液体可以在气凝胶的孔洞中自由进出,甚至可以进入具有催化活性的凝胶内部,且能贯穿整个凝胶网络。基于以上这些特性,气凝胶的吸附效率高于常用的吸附剂,其在吸附废水中的污染物方面有很大的潜力。另外气凝胶具有高孔隙率和高比表面积可作为催化剂的载体。气凝胶一般是由纳米级的骨架和微米级的穿透孔构成大尺寸的块体材料,结合它的低密度使得催化剂会漂浮于废水表面易于回收、利于循环使用。因此气凝胶可以作为催化剂或者催化剂的载体用于去除废水中的污染物。
黏土是一种资源丰富、价格低廉且具有许多优良物性的重要矿物原料。由多种水合硅酸盐和一定量的氧化铝、碱金属氧化物和碱土金属氧化物组成,并含有石英、长石、云母及硫酸盐、硫化物、碳酸盐等杂质。以黏土矿物作为纳米氧化物的载体,一方面可以实现纳米氧化物光催化材料的固载,另一方面可以利用矿物的离子交换和吸附性能将废水中的有机物污染物有效地吸附至纳米氧化物的晶粒表面,增加催化剂与污染物的接触几率,提高光催化降解效率。
目前,已报道的气凝胶光催化剂制备方法多种,但是本发明所用的制备方法的优点在于:此方法具有反应条件温和、简单易行。所得的气凝胶微球明显改善氧化银的团聚现象,提高了光催化降解染料性能,且益于回收再循环利用,便于实际应用。
发明内容
现有催化剂材料一般以粉末状形式存在,光催化降解染料废水中易分散,但很难回收,这会导致催化剂的流失,降低回收率同时会造成二次污染。本发明的目的在于将催化剂原位固载到水凝胶膜或气凝胶微球网络中。
本发明所述具有光催化活性的气凝胶微球的制备,其特征在于:利用黏土、海藻酸钠和银盐,通过注射法和离子交换法制备尺寸可调、网络结构可控和具有光催化活性的气凝胶微球,它可用于光催化降解废水中的染料,可作为一种新型的水处理剂。
本发明所述具有光催化活性的气凝胶微球的制备方法,具体步骤包括。
步骤一,通过搅拌的方法将黏土均匀分散于海藻酸钠溶液中。
步骤二,通过注射法将黏土-海藻酸钠混合溶液逐滴加入到银盐溶液中,形成水凝胶微球,然后蒸馏水反复冲洗数次,将未反应的银离子洗去。
步骤三,通过光还原和干燥将银基水凝胶转为氧化银基气凝胶微球。
所用干燥方法可选用超临界二氧化碳、真空干燥和冷冻干燥等方法。
本发明所选用黏土、海藻酸钠作为气凝胶微球的载体,用于固载氧化银光催化剂,具有以下优点。
1. 黏土和海藻酸钠分别属于天然矿物和聚合物,制备的气凝胶微球光催化剂无毒、无污染,非常适合用于水处理。
2. 海藻酸钠最大的特点是与阳离子交联形成宏观尺寸上的水凝胶微球。
3. 黏土作为光催化剂的载体,不仅可以实现光催化材料的固载,而且可以吸附废水中的有机物污染物,增加催化剂与污染物的接触几率,提高光催化降解效率。
4. 黏土有离子交换作用,可以调控气凝胶的孔结构。
(四)附图说明
图1为本发明第1实施例制备的氧化银/海藻酸钠-黏土气凝胶微球的扫描电镜图。
图2为本发明第1实施例制备的氧化银/海藻酸钠-黏土气凝胶微球光催化降解橙黄II染料的动力学曲线图。
图3为本发明第1实施例制备的氧化银/海藻酸钠-黏土气凝胶微球光催化降解染料的循环使用图。
(四)具体实施方式
通过具体的实施例对本发明进行进一步详细描述:实施例1:1 mg的锂藻土加入10 mL1%(W/V)的海藻酸钠水溶液中,分别形成1:0、50:1、40:1和30:1(ALG:锂藻土的不同质量比)的混合溶液。该溶液在室温下搅拌使其完全混匀。然后,用1 mL的注射器逐滴地将该混合溶液慢慢地加入10 mL 1%(W/V)AgNO3溶液中。水凝胶微球迅速生成。取出水凝胶微球,用去离子水冲洗除去微球表面过量的Ag+。最后经光还原60 min和冷冻干燥形成气凝胶微球。
实施例2:10 mg的膨润土加入10 mL 3%(W/V)的海藻酸钠水溶液中,分别形成1:0、50:1、40:1和30:1(ALG: 膨润土的不同质量比)的混合溶液。该溶液在室温下搅拌使其完全混匀。然后,用1 mL的注射器逐滴地将该混合溶液慢慢地加入10 mL 4%(W/V)AgClO4溶液中。水凝胶微球迅速生成。取出水凝胶微球,用去离子水冲洗除去微球表面过量的Ag+。最后经光还原60 min和冷冻干燥形成气凝胶微球。
实施例3:20 mg的锂藻土加入10 mL 5%(W/V)的海藻酸钠水溶液中,分别形成1:0、50:1、40:1和30:1(ALG: 锂藻土的不同质量比)的混合溶液。该溶液在室温下搅拌使其完全混匀。然后,用1 mL的注射器逐滴地将该混合溶液慢慢地加入10 mL 7%(W/V)AgF溶液中。水凝胶微球迅速生成。取出水凝胶微球,用去离子水冲洗除去微球表面过量的Ag+。最后经光还原60 min和冷冻干燥形成气凝胶微球。
实施例4:30 mg的硅藻土加入10 mL 7%(W/V)的海藻酸钠水溶液中,分别形成1:0、50:1、40:1和30:1(ALG: 硅藻土的不同质量比)的混合溶液。该溶液在室温下搅拌使其完全混匀。然后,用1 mL的注射器逐滴地将该混合溶液慢慢地加入10 mL 10%(W/V)AgF溶液中。水凝胶微球迅速生成。取出水凝胶微球,用去离子水冲洗除去微球表面过量的Ag+。最后经光还原60 min和冷冻干燥形成气凝胶微球。
实施例5:40 mg的硅藻土加入10 mL 9%(W/V)的海藻酸钠水溶液中,分别形成1:0、50:1、40:1和30:1(ALG: 硅藻土的不同质量比)的混合溶液。该溶液在室温下搅拌使其完全混匀。然后,用1 mL的注射器逐滴地将该混合溶液慢慢地加入10 mL 13%(W/V)AgF溶液中。水凝胶微球迅速生成。取出水凝胶微球,用去离子水冲洗除去微球表面过量的Ag+。最后经光还原60 min和冷冻干燥形成气凝胶微球。
实施例6:50 mg的锂藻土加入10 mL 11%(W/V)的海藻酸钠水溶液中,分别形成1:0、50:1、40:1和30:1(ALG:锂藻土的不同质量比)的混合溶液。该溶液在室温下搅拌使其完全混匀。然后,用1 mL的注射器逐滴地将该混合溶液慢慢地加入10 mL 16%(W/V)AgF溶液中。水凝胶微球迅速生成。取出水凝胶微球,用去离子水冲洗除去微球表面过量的Ag+。最后经光还原30 min和冷冻干燥形成气凝胶微球。
实施例7:60 mg的锂藻土加入10 mL 13%(W/V)的海藻酸钠水溶液中,分别形成1:0、50:1、40:1和30:1(ALG:锂藻土的不同质量比)的混合溶液。该溶液在室温下搅拌使其完全混匀。然后,用1 mL的注射器逐滴地将该混合溶液慢慢地加入10 mL 19%(W/V)AgF溶液中。水凝胶微球迅速生成。取出水凝胶微球,用去离子水冲洗除去微球表面过量的Ag+。最后经光还原60 min和冷冻干燥形成气凝胶微球。
实施例8:70 mg的锂藻土加入10 mL 15%(W/V)的海藻酸钠水溶液中,分别形成1:0、50:1、40:1和30:1(ALG:锂藻土的不同质量比)的混合溶液。该溶液在室温下搅拌使其完全混匀。然后,用1 mL的注射器逐滴地将该混合溶液慢慢地加入10 mL 21%(W/V)AgF溶液中。水凝胶微球迅速生成。取出水凝胶微球,用去离子水冲洗除去微球表面过量的Ag+。最后经光还原60 min和冷冻干燥形成气凝胶微球。
实施例9:80 mg的锂藻土加入10 mL 15%(W/V)的海藻酸钠水溶液中,分别形成1:0、50:1、40:1和30:1(ALG:锂藻土的不同质量比)的混合溶液。该溶液在室温下搅拌使其完全混匀。然后,用1 mL的注射器逐滴地将该混合溶液慢慢地加入10 mL 24%(W/V)AgF溶液中。水凝胶微球迅速生成。取出水凝胶微球,用去离子水冲洗除去微球表面过量的Ag+。最后经光还原60 min和冷冻干燥形成气凝胶微球。
实施例10:100 mg的锂藻土加入10 mL 15%(W/V)的海藻酸钠水溶液中,分别形成1:0、50:1、40:1和30:1(ALG:锂藻土的不同质量比)的混合溶液。该溶液在室温下搅拌使其完全混匀。然后,用1 mL的注射器逐滴地将该混合溶液慢慢地加入10 mL 30%(W/V)AgF溶液中。水凝胶微球迅速生成。取出水凝胶微球,用去离子水冲洗除去微球表面过量的Ag+。最后经光还原60 min和冷冻干燥形成气凝胶微球。
Claims (4)
1.一种具有光催化活性气凝胶微球的制备方法,其特征在于,所述气凝胶微球利用简单方法制备:将黏土加入海藻酸钠(ALG)溶液中,搅拌均匀,逐滴滴加到银盐(1%~30%)溶液中,制得银基水凝胶微球,最后将银基水凝胶微球经光照和干燥后制得氧化银基气凝胶微球。
2.根据权利要求1 所述,其特征在于:ALG的质量百分含量范围为1%~15%。
3.黏土有高岭土、膨润土、锂藻土和硅藻土等,其加入量范围为1~100 mg。
4.根据权利要求1所述,其特征在于:硝酸银、高氯酸银和氟化银作为凝胶的交联点,其质量百分含量为1%~30%。
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