CN115069303A - 一种酞菁铁基材料的制备方法及在降解双酚a中的应用 - Google Patents
一种酞菁铁基材料的制备方法及在降解双酚a中的应用 Download PDFInfo
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Abstract
本发明公开了一种酞菁铁基材料的制备方法及在降解双酚A中的应用，属于高级氧化领域。该催化材料采用普通单层石墨烯、酞菁铁为原料，经过一系列处理工序后成功制备出复合催化材料。该催化材料相比其他金属‑碳材料，具有更高的降解速率以及循环稳定性。本材料在20min内可完全去除污染物，且在实际污水处理厂出水中也表现出优异的性能。金属材料在活化过氧单硫酸盐时经常会发生金属团聚导致催化效率降低，或者会发生金属离子的浸出导致水环境受到危害。因此将金属材料负载在碳材料上可以避免类似问题的产生。本发明中，所使用的材料和方法对环境友好，所得的催化材料性能优异，是非常有前景的催化材料。
Description
技术领域
本发明属于高级氧化领域，具体涉及一种酞菁铁基复合材料制备方法及活化过氧单硫酸盐产生活性自由基降解双酚A。
背景技术
双酚A在工业上常被用来合成聚碳酸酯和环氧树脂等材料，作为一种内分泌干扰物广泛存在于水环境中，对生态环境和人类健康构成了极大的威胁。近年来，高级氧化工艺因其对有机污染物的高分解效率和矿化率而被广泛研究。与使用羟基自由基作为氧化剂的传统高级氧化相比，硫酸根自由基具有更高的氧化还原电位(2.6-3.1V)、更长的半衰期(30-40μs)和广泛的适用pH范围(2.0-8.0)。因此，基于硫酸根自由基的高级氧化已被广泛研究，以在实际修复处理中获得更好的性能。
过渡金属可以通过活化过氧单硫酸盐产生具有高活性的硫酸根自由基与双酚A反应。其中金属铁及其氧化物由于环境友好性而受到广泛关注，然而金属铁位点在反应过程易出现聚集以及金属离子浸出的问题。碳和碳基材料被认为是铁基催化剂的理想载体，因为它们具有出色的支持和协同催化作用。除此之外，在碳材料中引入杂原子氮，可以为反应创造新的活性位点。
酞菁铁具有优异的Fe-N4活性位点，将其负载在缺陷石墨烯上，不仅增加了酞菁铁的分散性，同时缺陷位点对于金属铁位点的电子密度进行进一步调节。因此，该材料有广阔的应用前景。
发明内容
本发明利用来源丰富的单层石墨烯、酞菁铁作为原料，制备了可用于活化过氧单硫酸盐产生活性自由基降解双酚A的复合材料。
本发明制备过程简单，不需要昂贵设备，所得产品性能优异，循环稳定性好，在高级氧化降解污染物应用中具有光明的前景。
一种酞菁铁基材料的制备方法及在降解双酚A中的应用，其制作过程包括以下步骤：
(1)把适量普通单层石墨烯置于管式炉内，通入氨气进行高温加热，得到掺氮石墨烯；
(2)上述得到的掺氮石墨烯继续置于管式炉内，通入氩气进行高温加热，从而得到缺陷石墨烯；
(3)取适量的酞菁铁，将其与上述得到的缺陷石墨烯混合后，置于乙醇中进行超声处理和搅拌处理；
(4)将超声搅拌后的样品置于真空烘箱中进行干燥，随后取出干燥后的样品，即得到目标催化材料：酞菁铁/缺陷石墨烯复合材料；
(5)对得到的酞菁铁/缺陷石墨烯复合材料进行活化过氧单硫酸盐降解双酚A测试。作为本发明的一个优选方案，上述酞菁铁和缺陷石墨烯的质量比为1：1。
本发明具有以下优点：
本发明利用来源丰富的单层石墨烯、酞菁铁作为原料，制备了可用于高级氧化领域的具有优异催化效率和催化稳定性的复合催化材料。
本发明中得到的催化材料在活化过氧单硫酸盐降解双酚A中，其性能优异，在加入过氧单硫酸盐20min后对双酚A即可达到完全降解。明显优于普通传统的金属-碳材料复合催化材料的降解效率。
本发明制备过程简单，不需要昂贵设备，所得催化材料循环稳定性能好，在将来高级氧化应用中具有光明的前景。
附图说明
图1是具体实施例1、2得到的酞菁铁/缺陷石墨烯的扫描电镜图，可以看出该材料呈现出2维超薄片状结构。
图2是酞菁铁/缺陷石墨烯活化过氧单硫酸盐降解双酚A的性能图。
图3是酞菁铁/缺陷石墨烯活化过氧单硫酸盐降解双酚A在实际污水处理厂二沉池出水的降解性能图。
具体实施方式
以下结合具体实施例，对本发明进行详细说明。
实施例1
(1)将10mg酞菁铁和10mg缺陷石墨烯分别超声溶于30mL乙醇中，超声处理2h。在超声的条件下将酞菁铁溶液缓慢滴入缺陷石墨烯溶液中得到两者混合的悬浊液，再将其超声2h，搅拌2h后，放入真空烘箱内，60℃干燥24h得到酞菁铁/缺陷石墨烯复合材料。
(2)首先将酞菁铁/缺陷石墨烯复合材料放入双酚A溶液中搅拌至吸附平衡，之后加入过氧单硫酸盐，所制得的材料可以活化过氧单硫酸盐产生活性自由基去攻击双酚A，从而使双酚A矿化为小分子物质，最后变为二氧化碳和水。定时取样，将样品注入高效液相色谱内分析双酚A的浓度。
(3)进行降解实验的条件为：双酚A溶液的浓度为20ppm，酞菁铁/缺陷石墨烯复合材料的浓度为0.2g/L，过氧单硫酸盐的浓度为0.2g/L，整个实验在黑暗条件下进行。
(4)进行测试的实验条件为：在使用高效液相色谱仪时，使用的流动相时液相色谱级甲醇和二次水的混合物。该流动相的配置方法为：将体积比为7：3的甲醇和二次水充分混合，抽滤两次，最后再超声半小时。在波长为275nm处，通过峰面积大小分析水中双酚A的浓度。通过降解后双酚A的峰面积与初始双酚A的峰面积之比，可算出在不同时间段内双酚A的降解率。
实施例2
(1)将10mg酞菁铁和10mg缺陷石墨烯分别超声溶于30mL乙醇中，超声处理2h。在超声的条件下将酞菁铁溶液缓慢滴入缺陷石墨烯溶液中得到两者混合的悬浊液，再将其超声2h，搅拌2h后，放入真空烘箱内，60℃干燥24h得到酞菁铁/缺陷石墨烯复合材料。
(2)首先将酞菁铁/缺陷石墨烯复合材料放入双酚A的污水处理厂二沉池出水中搅拌至吸附平衡，之后加入过氧单硫酸盐，所制得的材料可以活化过氧单硫酸盐产生活性自由基去攻击双酚A，从而使双酚A矿化为小分子物质，最后变为二氧化碳和水。定时取样，将样品注入高效液相色谱内分析双酚A的浓度。
(3)进行降解实验的条件为：双酚A溶液的浓度为20ppm，酞菁铁/缺陷石墨烯复合材料的浓度为0.2g/L，过氧单硫酸盐的浓度为0.2g/L，整个实验在黑暗条件下进行。
(4)进行测试的实验条件为：在使用高效液相色谱仪时，使用的流动相时液相色谱级甲醇和二次水的混合物。该流动相的配置方法为：将体积比为7∶3的甲醇和二次水充分混合，抽滤两次，最后再超声半小时。在波长为275nm处，通过峰面积大小分析水中双酚A的浓度。通过降解后双酚A的峰面积与初始双酚A的峰面积之比，可算出在不同时间段内双酚A的降解率。
Claims (6)
1.一种酞菁铁基材料的制备方法，其特征在于，包括以下步骤：
(1)把适量普通单层石墨烯置于管式炉内，通入氨气进行高温加热，得到掺氮石墨烯；
(2)上述得到的掺氮石墨烯继续置于管式炉内，通入氩气进行高温加热，从而得到缺陷石墨烯；
(3)取适量的酞菁铁，将其与上述得到的缺陷石墨烯混合后，置于乙醇中进行超声处理和搅拌处理；
(4)将超声搅拌后的样品置于真空烘箱中进行干燥，随后取出干燥后的样品，即得到酞菁铁/缺陷石墨烯复合材料。
2.根据权利要求书1所述的制备方法，其特征在于，步骤(1)中所述的普通单层石墨烯取100mg，管式炉加热的温度为600℃，升温速度5℃/min，保温时间1h。
3.根据权利要求书1所述的制备方法，其特征在于，步骤(2)管式炉加热的温度为1000℃，升温速度5℃/min，保温时间1h。
4.根据权利要求书1所述的制备方法，其特征在于，步骤(3)中所述的取用的酞菁铁质量为30mg，缺陷石墨烯质量为30mg，乙醇所取的体积为150mL，超声处理条件为超声4h，搅拌处理条件为搅拌2h。
5.根据权利要求书1所述的制备方法，其特征在于，步骤(4)中所述，真空烘箱的干燥温度定为60℃，烘干时间为12h。
6.如权利要求1所述的酞菁铁基材料在降解双酚A中的应用，其特征在于，所述酞菁铁/缺陷石墨烯复合材料用于活化过氧单硫酸盐降解双酚A。
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