CN112058285B - 一种Ag/Ag3PO4/碳化树脂复合物的制备方法及应用 - Google Patents
一种Ag/Ag3PO4/碳化树脂复合物的制备方法及应用 Download PDFInfo
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Abstract
本发明公开一种Ag/Ag3PO4/碳化树脂复合物的制备方法，包括以下步骤：将阴离子交换树脂加入到0.1‑1M磷酸盐溶液中，振荡吸附交换2‑8h，过滤干燥后，将阴离子交换树脂加入到0.05‑0.5M的AgNO3溶液中反应10‑60min，过滤后烘干，然后在惰性气体保护下，或抽真空条件下在200‑250℃碳化4‑10h，即制得Ag/Ag3PO4/碳化树脂复合物。本发明还提供上述制备方法制得的Ag/Ag3PO4/碳化树脂复合物及其应用。本发明的有益效果在于：本发明制备方法简单、成本低，适用于工业化生产，制得的产物对水中的有机污染物具有一定的降解效果。
Description
技术领域
本发明涉及材料技术领域，具体涉及一种Ag/Ag3PO4/碳化树脂复合物的制备方法及应用。
背景技术
Ag和Ag3PO4由于具有催化、抗菌等性能，因此，在工业上，常用于抗菌剂和光催化剂。近年来，为提高Ag3PO4的应用范围，Ag3PO4复合物制备技术是材料学、化学等学科研究的热点之一。
公开号为CN109277106A的专利公开了一种Ag/Ag3PO4/硅藻土复合可见光光催化剂及其制备方法，Ag/Ag3PO4/硅藻土复合可见光光催化剂的制备过程是：先将制备的光催化剂Ag3PO4负载到硅藻土上，制得Ag3PO4/硅藻土光催化剂，再采用原位光还原法，在Ag3PO4/硅藻土光催化剂表面生成 Ag单质。但该种Ag/Ag3PO4/硅藻土复合物材料制备过程较为繁琐。
发明内容
本发明所要解决的技术问题之一在于现有技术中的Ag/Ag3PO4复合物制备方法较复杂，提供一种制备方法简便的Ag/Ag3PO4/碳化树脂复合物的制备方法。
本发明通过以下技术手段实现解决上述技术问题的：
一种Ag/Ag3PO4/碳化树脂复合物的制备方法，包括以下步骤：将阴离子交换树脂加入到0.1-1M磷酸盐溶液中，振荡吸附交换2-8h，过滤干燥后，将阴离子交换树脂加入到0.05-0.5M的AgNO3溶液中反应10-60min，过滤后烘干，然后在惰性气体保护下，或在抽真空条件下在200-250℃煅烧 4-10h，即制得Ag/Ag3PO4/碳化树脂复合物。
有益效果：本发明制备方法简单、成本低，适用于工业化生产，无需采用原位光还原法，直接将阴离子交换树脂先加入到磷酸盐溶液中吸附交换，再加入到Ag+离子溶液中反应，经过滤、干燥、煅烧后，即可获得本发明中的Ag/Ag3PO4/碳化树脂复合物。
在惰性气体保护或真空条件下的煅烧温度为200-250℃，可以使阴离子交换树脂碳化，同时制得的产物中含有Ag3PO4、Ag、碳化的阴离子交换树脂组分。
优选地，所述磷酸盐溶液包括磷酸氢二钠水溶液。
优选地，所述Ag/Ag3PO4/碳化树脂复合物为球形，直径在200-500μm 之间。
优选地，所述惰性气体为氮气，所述氮气流量为10-40mL/min。
优选地，所述抽真空条件为将管式炉抽真空至0.01-0.05Pa。
优选地，所述阴离子交换树脂包括强碱性阴离子交换树脂或弱碱性阴离子交换树脂。
本发明所要解决的技术问题之二在于现有技术中的Ag或Ag3PO4复合物对有机污染物吸附、降解效果较差等问题，提供一种Ag/Ag3PO4/碳化树脂复合物。
本发明通过以下技术手段实现解决上述技术问题的：
一种采用上述制备方法制得的Ag/Ag3PO4/碳化树脂复合物。
有益效果：本发明中的Ag/Ag3PO4/碳化树脂复合物在紫外光、可见光下对水中的有机污染物都具有一定的降解效果。
优选地，所述Ag/Ag3PO4/碳化树脂复合物为球形，直径在200-500μm 之间。
本发明所要解决的技术问题之三在于现有技术中的Ag或Ag3PO4复合物对水中有机污染物的吸附、降解效果较差的问题，提供一种Ag/Ag3PO4/ 碳化树脂复合物在降解有机污染物中的应用。
本发明通过以下技术手段实现解决上述技术问题的：
一种Ag/Ag3PO4/碳化树脂复合物在降解有机污染物中的应用。
有益效果：Ag/Ag3PO4/碳化树脂复合物对水中的有机污染物具有一定的降解效果。
优选地，将0.05g Ag/Ag3PO4/碳化树脂复合物置于50mL、5mg/L亚甲基蓝水溶液中，在100w紫外灯或100w日光灯照射下进行脱色。
有益效果：本发明中的Ag/Ag3PO4/碳化树脂复合物在紫外灯光照80min 亚甲基蓝水溶液脱色率最高达到98.2％。
优选地，将0.2g Ag/Ag3PO4/碳化树脂复合物置于100mL CODcr为 210mg/L的生活污水中，在100w紫外灯或100w日光灯下照射180min。
有益效果：本发明中的Ag/Ag3PO4/碳化树脂复合物在紫外灯光照射下对生活污水具有一定的降解效果，且在紫外灯光照180min生活污水CODcr 降解率最高达到43.5％，在可见光下光照180min，生活污水CODcr降解率最高达到18.4％。
本发明的优点在于：
本发明制备方法简单、成本低，适用于工业化生产，无需采用原位光还原法，直接将阴离子交换树脂先加入到磷酸盐溶液中吸附交换，再加入到Ag+离子溶液中反应，经过滤、干燥、煅烧后，即可获得本发明中的 Ag/Ag3PO4/碳化树脂复合物。
本发明中的Ag/Ag3PO4/碳化树脂复合物在紫外光、可见光下对水中的有机污染物都具有一定的降解效果，在紫外灯光照80min亚甲基蓝水溶液脱色率最高达到98.2％，在可见光下光照80min亚甲基蓝水溶液脱色率最高达到29.6％。
在紫外灯光照180min生活污水CODcr降解率最高达到43.5％，在可见光下光照180min，生活污水CODcr降解率最高达到18.4％。
本发明制得的Ag/Ag3PO4/碳化树脂复合物在紫外光下和可见光下对水中有机污染物的降解效果明显优于现有技术中的Ag3PO4/离子交换树脂复合物。
附图说明
图1为本发明实施例1中Ag/Ag3PO4/碳化树脂复合物的X射线衍射图谱；
图2为本发明实施例1中Ag/Ag3PO4/碳化树脂复合物的扫描电镜图。
具体实施方式
为使本发明实施例的目的、技术方案和优点更加清楚，下面将结合本发明实施例，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
下述实施例中所用的试验材料和试剂等，如无特殊说明，均可从商业途径获得。
下述实施例中所使用的弱碱型阴离子交换树脂、强碱阴离子交换树脂均购买自上海劲凯树脂有限公司。
实施例中未注明具体技术或条件者，均可以按照本领域内的文献所描述的技术或条件或者按照产品说明书进行。
实施例1
Ag/Ag3PO4/碳化树脂复合物的制备方法
在烧杯中将2g强碱阴离子交换树脂加入到150mL、0.1M磷酸氢二钠溶液中，并于振荡器上振荡交换8h，然后过滤、干燥后，将上述阴离子交换树脂加入到100mL、0.05M AgNO3溶液中反应60min，过滤后烘干，再将所得树脂在管式炉中于10ml/min流量的氮气保护下，200℃煅烧10h，即可制得1.9g Ag/Ag3PO4/碳化树脂复合物。
实施例2
Ag/Ag3PO4/碳化树脂复合物的制备方法
在烧杯中将2g强碱阴离子交换树脂加入到50mL、1.0M磷酸氢二钠溶液中，并于振荡器上振荡2h，然后过滤、干燥后，将上述阴离子交换树脂加入到60mL、0.5M AgNO3溶液中反应10min，过滤后烘干，再将所得树脂在管式炉中于40ml/min流量的氮气保护下，250℃煅烧4h，即可制得1.6g Ag/Ag3PO4/碳化树脂复合物。
实施例3
Ag/Ag3PO4/碳化树脂复合物的制备方法
在烧杯中将2g弱碱性阴离子交换树脂加入到80mL、0.8M磷酸氢二钠溶液中，并于振荡器上振荡4h，然后过滤、干燥后，将上述阴离子交换树脂加入到70mL、0.1M AgNO3溶液中反应40min，过滤后烘干，再将所得树脂在管式炉中抽真空到0.05Pa条件下，220℃煅烧8h，即可制得1.8g Ag/Ag3PO4/碳化树脂复合物。
实施例4
Ag/Ag3PO4/碳化树脂复合物的制备方法
在烧杯中将2g弱碱性阴离子交换树脂加入到120mL、0.4M磷酸氢二钠溶液中，并于振荡器上振荡5h，然后过滤、干燥后，将上述阴离子交换树脂加入到90mL、0.2M AgNO3溶液中反应30min，过滤后烘干，再将所得树脂在管式炉中抽真空到0.01Pa条件下，230℃煅烧6h，即可制得1.7g Ag/Ag3PO4/碳化树脂复合物。
实施例5
对实施例1-实施例4中的Ag/Ag3PO4/碳化树脂复合物性能进行测定
(1)通过德国Bruke D8 Advance X射线衍射仪分析了Ag3PO4晶型，德国蔡司SigmaHD型扫描电镜观察了微球表面形貌。
测定结果如表1所示，图1为本发明实施例1中Ag/Ag3PO4/碳化树脂复合物的X射线衍射图谱，图2为本发明实施例1中Ag/Ag3PO4/碳化树脂复合物的扫描电镜图，从图1和图2可以看出，本实施例1中Ag/Ag3PO4/ 碳化树脂复合物由Ag颗粒、Ag3PO4颗粒和碳化的阴离子交换树脂组成，直径200-500μm之间，Ag颗粒、Ag3PO4颗粒在外层，Ag3PO4颗粒较多， Ag颗粒较少，碳化的阴离子交换树脂在内层。
实施例2中制备的Ag/Ag3PO4/碳化树脂复合物由Ag、Ag3PO4颗粒和碳化的阴离子交换树脂组成，直径200-500μm之间，Ag颗粒较多，Ag3PO4颗粒较少，碳化的阴离子交换树脂在内层。
实施例3中制备的Ag/Ag3PO4/碳化树脂复合物通过德国Bruke D8 Advance X射线衍射仪分析了Ag3PO4晶型，德国蔡司Sigma HD型扫描电镜观察了微球表面形貌，结果表明：所所制备的Ag/Ag3PO4/碳化树脂复合物由Ag颗粒、Ag3PO4颗粒和碳化的阴离子交换树脂组成，直径200-500μm 之间，Ag颗粒、Ag3PO4颗粒在外层，碳化的阴离子交换树脂在内层。
实施例4中所制备的Ag/Ag3PO4/碳化树脂复合物由Ag颗粒、Ag3PO4颗粒和碳化的阴离子交换树脂组成，直径200-500μm之间，Ag颗粒、Ag3PO4颗粒在外层，碳化的阴离子交换树脂在内层。
表1为实施例1-实施例4中产物性能指标
(2)对实施例1-实施例4中的Ag/Ag3PO4/碳化树脂复合物对有机污染物亚甲基蓝的降解效果进行测定。
在50mL、5mg/L的亚甲基蓝水溶液中加入0.05g的各实施例制备的 Ag/Ag3PO4/碳化树脂复合物，分别在100W紫外灯或100W日光灯照射下，亚甲基蓝水溶液80分钟的脱色率。测定结果如表2所示。
在100mL CODcr为210mg/L的生活污水中加入0.2g的各实施例制备的Ag/Ag3PO4/碳化树脂复合物，分别在100W紫外灯或100W日光灯照射 180分钟，生活污水中有机污染物得到降解，CODcr一般代表水中耗氧的有机物多少。测定结果如表3所示。
表2为Ag/Ag3PO4/碳化树脂复合物对亚甲基蓝的催化效果表
表3为Ag/Ag3PO4/碳化树脂复合物对生活污水的催化效果表
从表2可以看出，Ag/Ag3PO4/碳化树脂复合物在紫外光下、可见光下对水中有机污染物都具有一定的降解效果，且在紫外灯光照80min亚甲基蓝水溶液脱色率最高达到98.2％，在可见光下光照80min亚甲基蓝水溶液脱色率最高达到29.6％。
从表3可以看出，Ag/Ag3PO4/碳化树脂复合物在紫外光下、可见光下对生活污水有机污染物都具有一定的降解效果，且在紫外灯光照180min生活污水CODcr降解率最高达到43.5％；在可见光下光照180min，生活污水CODcr降解率最高达到18.4％。
对比例
在50mL、5mg/L的亚甲基蓝水溶液中加入0.05g的按专利(发明专利号：201210188768.7)方法制备的Ag3PO4/离子交换树脂复合物，分别在100W 紫外灯、100W日光灯照射下，亚甲基蓝水溶液80分钟的脱色率分别为 75.6％和6.8％。
在100mL CODcr为210mg/L的生活污水中加入0.2g的按专利(发明专利号：201210188768.7)方法制备的Ag3PO4/离子交换树脂复合物，在紫外灯光照180min生活污水CODcr降解率为23.6％，在可见光下光照180min，生活污水CODcr降解率为9.6％。
可以明显看出，本发明制得的Ag/Ag3PO4/碳化树脂复合物在紫外光下和可见光下对水中有机污染物的降解效果明显优于现有技术中的Ag3PO4/ 离子交换树脂复合物。
以上实施例仅用以说明本发明的技术方案，而非对其限制；尽管参照前述实施例对本发明进行了详细的说明，本领域的普通技术人员应当理解：其依然可以对前述各实施例所记载的技术方案进行修改，或者对其中部分技术特征进行等同替换；而这些修改或者替换，并不使相应技术方案的本质脱离本发明各实施例技术方案的精神和范围。
Claims (10)
1.一种Ag/Ag3PO4/碳化树脂复合物的制备方法，其特征在于：包括以下步骤：将阴离子交换树脂加入到0.1-1M磷酸盐溶液中，振荡吸附交换2-8h，过滤干燥后，将阴离子交换树脂加入到0.05-0.5M的AgNO3溶液中反应10-60min，过滤后烘干，然后在惰性气体保护下，或者在抽真空条件下，200-250℃煅烧4-10h，即制得Ag/Ag3PO4/碳化树脂复合物；所述Ag/Ag3PO4/碳化树脂复合物为球形，直径在200-500μm之间，含有Ag3PO4、Ag、碳化的阴离子交换树脂。
2.根据权利要求1所述的Ag/Ag3PO4/碳化树脂复合物的制备方法，其特征在于：所述磷酸盐溶液包括磷酸氢二钠水溶液。
3.根据权利要求1所述的Ag/Ag3PO4/碳化树脂复合物的制备方法，其特征在于：所述阴离子交换树脂包括强碱性阴离子交换树脂或弱碱性阴离子交换树脂。
4.根据权利要求1所述的Ag/Ag3PO4/碳化树脂复合物的制备方法，其特征在于：所述抽真空条件为将管式炉抽真空至0.01-0.05Pa。
5.根据权利要求1所述的Ag/Ag3PO4/碳化树脂复合物的制备方法，其特征在于：所述惰性气体为氮气，所述氮气流量为10-40mL/min。
6.一种采用权利要求1-5中任一项所述的制备方法制得的Ag/Ag3PO4/碳化树脂复合物。
7.根据权利要求6所述的Ag/Ag3PO4/碳化树脂复合物，其特征在于：所述Ag/Ag3PO4/碳化树脂复合物为球形，直径在200-500μm之间，含有Ag3PO4、Ag、碳化的阴离子交换树脂。
8.一种采用权利要求1-5中任一项所述的制备方法制得的Ag/Ag3PO4/碳化树脂复合物在降解有机污染物中的应用。
9.根据权利要求8所述的Ag/Ag3PO4/碳化树脂复合物在降解有机污染物中的应用，其特征在于：将0.05g Ag/Ag3PO4/碳化树脂复合物置于50mL、5mg/L亚甲基蓝水溶液中，在100w紫外灯或100w日光灯照射下进行脱色。
10.根据权利要求8所述的Ag/Ag3PO4/碳化树脂复合物在降解有机污染物中的应用，其特征在于：将0.2g Ag/Ag3PO4/碳化树脂复合物置于100mL CODcr为210mg/L的生活污水中，在100w紫外灯或100w日光灯下照射180min。
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