CN108906092A - 一种选择性去除阳离子染料的Ag3PO4@Ag/碳球三元异质结复合材料的制备方法 - Google Patents
一种选择性去除阳离子染料的Ag3PO4@Ag/碳球三元异质结复合材料的制备方法 Download PDFInfo
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Abstract
本发明公开了一种选择性去除阳离子染料的Ag3PO4@Ag/碳球三元异质结复合材料的制备方法，将摩尔浓度为0.5mol/L的葡萄糖溶液置于水热反应釜中于180℃水热反应5‑8h得到平均直径为0.3‑0.7μm的碳球；将10wt%‑25wt%的氨水溶液滴加至0.05‑0.2mol/L的AgNO3溶液中配制成透明的银氨溶液；将碳球加入到银氨溶液中，其中碳球与AgNO3的质量比为0.01‑0.1:1，搅拌2‑10h；将Na2HPO4溶液滴加到上述混合溶液中，其中Ag+与PO4 3‑的摩尔比为3:1‑10，反应1‑3h，随后离心、过滤、洗涤，真空干燥箱中50℃干燥制得Ag3PO4@Ag/碳球三元异质结复合材料。本发明能够实现快速高效去除阳离子染料的目的，合成的Ag3PO4@Ag/碳球三元异质结复合材料具有很好的稳定性。
Description
技术领域
本发明属于复合光催化材料的合成技术领域，具体涉及一种选择性去除阳离子染料的 Ag3PO4@Ag/碳球三元异质结复合材料的制备方法。
背景技术
新型光催化剂Ag3PO4具有良好的可见光催化性能，在可见光下(λ>420nm)光解水制O2时量子效率可达90％且可有效降解有机染料，是一种很有发展前景的光催化剂。但是由于Ag3PO4的导带位置比H2O/H2的氧化还原电位更正，导致光催化过程中H2O分子无法捕获光生电子，这些光生电子将与Ag3PO4中的Ag+发生反应生成金属Ag分布在Ag3PO4的表面，出现光腐蚀现象，影响Ag3PO4的光稳定性及光催化性能。
碳材料具有良好的导电性能，与Ag3PO4复合以后可以快速转移光生电子，增加Ag3PO4光催化性能的同时减少光腐蚀。金属Ag纳米颗粒也可以增加Ag3PO4中光生电子的转移及对可见光的吸收。将碳材料、Ag纳米颗粒同时与Ag3PO4复合可以进一步提高其光催化性能和光稳定性，已有文献报道Ag3PO4与碳材料(石墨烯、碳纳米管等)、Ag纳米颗粒共同复合可进一步提高其光催化性能，但是Ag纳米颗粒一般分布在Ag3PO4表面上，过多的 Ag纳米颗粒会占据Ag3PO4表面上的活性位点影响其光催化性能，因此Ag纳米颗粒的负载位置对其光催化性能有一定的影响。本申请采用化学沉淀法合成一种Ag3PO4@Ag/碳球三元异质结，其中Ag纳米颗粒分布在碳球上，碳球镶嵌在Ag3PO4中，这样既可以加速光生电荷的分离又不影响Ag3PO4光催化性能的发挥。
另外，利用异质结材料的吸附和光催化协同效应可以更有效的去除有机染料。在去除过程中，染料可以先从液相转移到固相催化剂，然后在光催化过程中染料被催化降解实现吸附位点的原位再生，提高了染料的去除效率。目前虽有一些异质结材料利用吸附光催化去除有机染料的报道，但是尚未见关于Ag3PO4@Ag/碳球三元异质结复合材料选择性去除阳离子染料的报道。
发明内容
本发明解决的技术问题是提供了一种选择性去除阳离子染料的Ag3PO4@Ag/碳球三元异质结复合材料的制备方法，含有Ag纳米颗粒的碳球不仅能够选择性地吸附阳离子染料，而且能够增加Ag3PO4对可见光的吸收以及加快光生电子的快速转移，最终实现快速高效去除阳离子染料的目的，合成的Ag3PO4@Ag/碳球三元异质结复合材料具有很好的稳定性。
本发明为解决上述技术问题采用如下技术方案，一种选择性去除阳离子染料的Ag3PO4@Ag/碳球三元异质结复合材料的制备方法，其特征在于具体步骤为：将摩尔浓度为0.5mol/L的葡萄糖溶液置于水热反应釜中于180℃水热反应5-8h得到平均直径为 0.3-0.7μm的碳球；将10wt％-25wt％的氨水溶液滴加至0.05-0.2mol/L的AgNO3溶液中配制成透明的银氨溶液；将碳球加入到银氨溶液中，其中碳球与AgNO3的质量比为 0.01-0.1:1，搅拌2-10h；将Na2HPO4溶液滴加到上述混合溶液中，其中Ag+与PO4 3-的摩尔比为3:1-10，反应1-3h，随后离心、过滤、洗涤，真空干燥箱中50℃干燥制得Ag3PO4@Ag/ 碳球三元异质结复合材料。
本发明制得的Ag3PO4@Ag/碳球三元异质结复合材料中Ag纳米颗粒分布在碳球上，碳球镶嵌在Ag3PO4中，减少对Ag3PO4活性位点的覆盖，加速光生电子的转移，能够实现对阳离子染料亚甲基蓝的选择性去除。
本发明与现有技术相比具有以下优点：
1、Ag纳米颗粒直接生长在碳球上，碳球镶嵌在Ag3PO4中，减少对Ag3PO4活性位点的覆盖，加速光生电子的转移；2、室温下通过一步化学反应就可同时得到Ag纳米颗粒和Ag3PO4，不需要额外的光照和强还原剂还原得到Ag纳米颗粒；3、Ag3PO4@Ag/碳球三元异质结复合材料兼具吸附和光催化的性能，能够选择性去除阳离子染料亚甲基蓝，具有很好的稳定性。
附图说明
图1是实施例3制得的Ag3PO4@Ag/碳球三元异质结复合材料的SEM图，由图可以看出碳球镶嵌在Ag3PO4中；
图2是实施例2制得的Ag3PO4@Ag/碳球三元异质结复合材料的XRD图，由图可知样品中含有Ag3PO4和金属Ag；
图3是实施例2制得的Ag3PO4@Ag/碳球三元异质结复合材料的TEM图，由图可以看出Ag纳米颗粒分布在碳球上，碳球镶嵌在Ag3PO4中；
图4是Ag3PO4及实施例1和2制得的Ag3PO4@Ag/碳球三元异质结复合材料去除阳离子染料亚甲基蓝的效果图，由图可知制得的Ag3PO4@Ag/碳球三元异质结复合材料对亚甲基蓝具有很强的吸附和光催化降解效果；
图5是Ag3PO4及实施例1制得的Ag3PO4@Ag/碳球三元异质结复合材料去除阴离子染料甲基橙的效果图，由图可知制得的Ag3PO4@Ag/碳球三元异质结复合材料对甲基橙没有吸附效果，仅有光催化降解能力，进而表明本发明制得的制得的Ag3PO4@Ag/碳球三元异质结复合材料主要对阳离子染料具有良好的去除效果。
具体实施方式
以下通过实施例对本发明的上述内容做进一步详细说明，但不应该将此理解为本发明上述主题的范围仅限于以下的实施例，凡基于本发明上述内容实现的技术均属于本发明的范围。
实施例1
将摩尔浓度为0.5mol/L的葡萄糖溶液置于水热反应釜中于180℃水热反应5h得到平均直径为0.3μm的碳球；将25wt％的氨水溶液滴加至0.05mol/L的AgNO3溶液中配制成透明的银氨溶液；将碳球加入到银氨溶液中，其中碳球与AgNO3的质量比为0.01:1，搅拌 6h；将Na2HPO4溶液滴加到上述混合溶液中，其中Ag+与PO4 3-的摩尔比为3:2，反应3h，随后离心、过滤、洗涤，真空干燥箱中50℃干燥制得Ag3PO4@Ag/碳球三元异质结复合材料，标记为Ag3PO4@Ag/碳球-1。
实施例2
将摩尔浓度为0.5mol/L的葡萄糖溶液置于水热反应釜中于180℃水热反应8h得到平均直径为0.7μm的碳球；将15wt％的氨水溶液滴加至0.1mol/L的AgNO3溶液中配制成透明的银氨溶液；将碳球加入到银氨溶液中，其中碳球与AgNO3的质量比为0.03:1，搅拌 2h；将Na2HPO4溶液滴加到上述混合溶液中，其中Ag+与PO4 3-的摩尔比为3:10，反应1h，随后离心、过滤、洗涤，真空干燥箱中50℃干燥制得Ag3PO4@Ag/碳球三元异质结复合材料，标记为Ag3PO4@Ag/碳球-2。
实施例3
将摩尔浓度为0.5mol/L的葡萄糖溶液置于水热反应釜中于180℃水热反应8h得到平均直径为0.7μm的碳球；将10wt％的氨水溶液滴加至0.1mol/L的AgNO3溶液中配制成透明的银氨溶液；将碳球加入到银氨溶液中，其中碳球与AgNO3的质量比为0.1:1，搅拌10h；将Na2HPO4溶液滴加到上述混合溶液中，其中Ag+与PO4 3-的摩尔比为3:1，反应2h，随后离心、过滤、洗涤，真空干燥箱中50℃干燥制得Ag3PO4@Ag/碳球三元异质结复合材料，标记为Ag3PO4@Ag/碳球-3。
以上实施例描述了本发明的基本原理、主要特征及优点，本行业的技术人员应该了解，本发明不受上述实施例的限制，上述实施例和说明书中描述的只是说明本发明的原理，在不脱离本发明原理的范围下，本发明还会有各种变化和改进，这些变化和改进均落入本发明保护的范围内。
Claims (2)
1.一种选择性去除阳离子染料的Ag3PO4@Ag/碳球三元异质结复合材料的制备方法，其特征在于具体步骤为：将摩尔浓度为0.5mol/L的葡萄糖溶液置于水热反应釜中于180℃水热反应5-8h得到平均直径为0.3-0.7μm的碳球；将10wt%-25wt%的氨水溶液滴加至0.05-0.2mol/L的AgNO3溶液中配制成透明的银氨溶液；将碳球加入到银氨溶液中，其中碳球与AgNO3的质量比为0.01-0.1:1，搅拌2-10h；将Na2HPO4溶液滴加到上述混合溶液中，其中Ag+与PO4 3-的摩尔比为3:1-10，反应1-3h，随后离心、过滤、洗涤，真空干燥箱中50℃干燥制得Ag3PO4@Ag/碳球三元异质结复合材料。
2.根据权利要求1所述的选择性去除阳离子染料的Ag3PO4@Ag/碳球三元异质结复合材料的制备方法，其特征在于：制得的Ag3PO4@Ag/碳球三元异质结复合材料中Ag纳米颗粒分布在碳球上，碳球镶嵌在Ag3PO4中，减少对Ag3PO4活性位点的覆盖，加速光生电子的转移，能够实现对阳离子染料亚甲基蓝的选择性去除。
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