CN111841615A - 一种g-C3N4/CDs/β-FeOOH光催化材料及其制备方法 - Google Patents
一种g-C3N4/CDs/β-FeOOH光催化材料及其制备方法 Download PDFInfo
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Abstract
本发明涉及一种g‑C3N4/CDs/β‑FeOOH光催化材料，其中β‑FeOOH无序负载在层状g‑C3N4上，CDs分散在β‑FeOOH和g‑C3N4的表面。其制备方法包括：分别取g‑C3N4和CDs分散水中超声并搅拌形成A溶液；取FeCl3·6H2O溶于水中形成0.15mol/L的B溶液；将B溶液倒入A溶液中搅拌，将搅拌液置于反应容器中升温至110～130℃，并保温10～15h，待反应釜冷却至室温后备用；将冷却后反应液过滤取沉淀，干燥沉淀后即得g‑C3N4/CDs/β‑FeOOH光催化材料。上述技术方案中提供的g‑C3N4/CDs/β‑FeOOH光催化材料及其制备方法，能有效解决现有单一催化剂存在的吸附能力差或易发生团聚现象影响催化效果的问题。
Description
技术领域
本发明涉及光催化材料技术领域，具体涉及一种CDs表面修饰g-C3N4/β-FeOOH光催化材料及其制备方法。
背景技术
随着现代化工及相关产业的迅速发展，有机染料、苯基酚类、双酚A、尼泊金脂类等引起的水污染日益严重。然而污水处理成本和技术有限，很多未处理或处理没有达标的工业废水随意排放，使得河流、大海等重要水域中难以分解的有毒有害有机污染物的含量急剧增加，严重影响到人们身体健康，甚至威胁到人类的生存与发展。由国际慈善机构“水援助”发表的调查报告显示，全球每天有多达6000名少年儿童因饮用水卫生状况恶劣而死亡。水污染问题现在己经成为全球最为紧迫的环境卫生安全危机之一。
为治理这些废水污染物，常用的废水处理方法主要包括化学、物理和生物等，其中光催化材料降解方法在处理这些有机污染物时，具有高效、环境友好和适用范围广等优势。g-C3N4作为一种热门的新型非金属半导体光催化材料，对可见光能够有响应，对酸、碱、光等具有优异的耐腐蚀性，受到了越来越多研究者的关注。然而g-C3N4量子效率低，吸附能力差等问题限制了其广泛应用。国内外许多学者对g-C3N4进行了改性，其中通过复合方法可以有效提高其量子效率，促进光催化反应的进行，从而达到降解有机污染物的目的。
β-FeOOH作为光催化领域的一种热门材料，其带隙约为2.12eV，能够在可见光下显现催化功能。是一种特殊的非均相体系中的光-Fenton催化剂。此外，β-FeOOH还具有如下优点：不使用表面活性剂也能很容易地获得各种形态，并且它分级支化的纳米结构电荷转移快、光捕集能力强。然而纳米级的β-FeOOH易出现团聚现象，不利于光催化的进行。上述两种单一的催化剂都分别具备优点和缺点，无法达到更加优异的光催化效果。
发明内容
本发明的目的是提供一种g-C3N4/CDs/β-FeOOH光催化材料及其制备方法，能有效解决现有单一催化剂存在的吸附能力差、光响应范围小以及光催化反应速率低的问题。
为解决上述技术问题，本发明采用了以下技术方案：
一种g-C3N4/CDs/β-FeOOH光催化材料，β-FeOOH无序负载在层状g-C3N4上，CDs分散在β-FeOOH和g-C3N4的表面。
β-FeOOH为长度0.5～1.4μm的棒状；g-C3N4为不规则片状；CDs为粒径4～6nm的粒状。
其中，g-C3N4和β-FeOOH形成复合光催化材料，该复合光催化材料中g-C3N4和β-FeOOH 重量比为3:2。
上述g-C3N4/CDs/β-FeOOH光催化材料是通过水热法一步合成的，具体包括以下步骤：
1)分别取g-C3N4和CDs分散水中超声并搅拌形成A溶液；
2)取FeCl3·6H2O溶于水中形成0.15mol/L的B溶液；
3)将B溶液倒入A溶液中搅拌，将搅拌液置于反应容器中升温至110～130℃，并保温 10～15h，待反应釜冷却至室温后备用；
4)将冷却后反应液过滤取沉淀，干燥沉淀后即得g-C3N4/CDs/β-FeOOH光催化材料。
其中，CDs占g-C3N4/CDs/β-FeOOH光催化材料重量的1％～9％。
其中，沉淀的干燥条件为55～65℃下真空干燥24h。
上述技术方案中提供的g-C3N4/CDs/β-FeOOH光催化材料，通过将β-FeOOH与g-C3N4复合，形成异质结，有效拓宽了光催化剂的光响应范围，使g-C3N4在可见光下的光催化效率增强；在此基础上用CDs对g-C3N4/β-FeOOH进行表面修饰，提供光反应活性位点，有效提高催化剂的光捕集能力和量子产率，抑制电子空穴对的复合，从而提高了其光催化反应速率。
本发明的g-C3N4利用煅烧法制备，CDs通过水热法制备，其操作简单，使用设备少，成本低、无污染，制备过程简单，绿色环保，可以实现规模生产。
附图说明
图1为本发明实施例中各样品的XRD图；
图2为本发明实施例中样品的红外光谱图；
图3(a)为本发明实施例中g-C3N4/CDs/β-FeOOH的SEM图；
图3(b～d)为本发明实施例中g-C3N4/CDs/β-FeOOH的TEM图；
图4为本发明实施例中各样品的光催化降解曲线。
具体实施方式
为了使本发明的目的及优点更加清楚明白，以下结合实施例对本发明进行具体说明。应当理解，以下文字仅仅用以描述本发明的一种或几种具体的实施方式，并不对本发明具体请求的保护范围进行严格限定。
g-C3N4/CDs/β-FeOOH光催化材料的制备步骤如下：
(1)g-C3N4的制备
称取12g尿素和16mL去离子水(质量比为3:4)，将称量好的尿素溶解在水中，磁力搅拌半小时后形成匀质的尿素水溶液，将尿素水溶液转移至坩埚后放入马弗炉中，坩埚盖盖紧后以15℃/min的升温速率升温到400℃后保温1h，再以同样的升温速率升至500℃，并保温2h。待马弗炉温度自然冷却至室温后，取出坩埚内的块体，用玛瑙研钵研磨，得到蓬松轻质的淡黄色g-C3N4粉末。
(2)CDs的制备
分别称取3g尿素与15g柠檬酸分散在50mL蒸馏水中。将溶液倒入100mL的反应釜中，升温至180℃，保温5h。待反应釜自然冷却至室温后，将反应溶液以12500RPM的转速离心以除去大颗粒。随后用透析袋(500Da)对溶液进行透析。最后，将透析所得的外部液体冷冻干燥以获得CDs固体。将CDs粉末密封并置于4℃冷藏，留待后续实验使用。
(3)g-C3N4/CDs/β-FeOOH的制备
分别取0.6g g-C3N4和0.06g CDs分散在30mL蒸馏水中超声并搅拌形成A溶液，另外称取1.215g FeCl3·6H2O加入30mL蒸馏水中搅拌分散形成B溶液。将B溶液迅速倒入A溶液中并剧烈搅拌1h，然后将溶液倒入100mL反应釜中，升温至120℃，保温12h。待反应釜自然冷却至室温后过滤，将沉淀干燥得到g-C3N4/CDs/β-FeOOH光催化材料(CCF2)。
称取0.015g实施例中的g-C3N4/CDs/β-FeOOH光催化材料分散在50mLRhB溶液(10mg/L)中，暗反应30min后，在420W金卤灯的照射下进行降解实验。实验中每间隔 10min取一次样，直至溶液变为无色透明。将取得的样进行离心(6000r/min，3min)，取上层清液待测。用紫外分光光度计进行测试，g-C3N4/CDs/β-FeOOH光催化材料的催化性能如图所示，在60min后降解率达到了100％。
按照上述方法，分别制备CF，CCF1和CCF3，其中CF中CDs的添加量为0，CF1中 CDs的添加量为0.03g，CF3中CDs的添加量为0.09g，其余条件均与CCF2制备方法相同。
图1是实施例1中的g-C3N4，β-FeOOH，CF，CCF1，CCF2和CCF3的XRD图。通过 XRD对样品的物相组成进行了分析。图1中位于27.31°处的特征峰对应了g-C3N4的(002) 晶面。β-FeOOH的衍射峰位于11.92°、16.88°、26.84°、34.08°、35.32°、44.6°、52.16°、 55.92°和64.56°，分别对应于(110)、(200)、(310)、(211)、(301)、(411)、 (600)、(521)以及(640)晶面。g-C3N4/CDs/β-FeOOH光催化材料的衍射峰与g-C3N4和β-FeOOH对应，随着CDs含量的增加，其在24.4°的位置逐渐出现了一个新的弱峰，这证明了CDs的存在，且CDs的加入并未改变g-C3N4/β-FeOOH的晶型结构。另外，相对于单物质， g-C3N4/CDs/β-FeOOH光催化材料的峰强减弱，原因是复合物中材料的相对含量降低。
图2是实施例1中的g-C3N4及其复合物的红外光谱图。图2中可见β-FeOOH在426.2cm-1处的有一吸收峰，对应了Fe-O的拉伸振动，而在690.4cm-1和846.6cm-1另有的两处吸收峰则是由于Fe-OH的收缩振动引起的。另外，g-C3N4在806cm-1、1329.77cm-1、1422.80cm-1以及1630.62cm-1处都有吸收峰，它们分别对应了三嗪的面外骨架伸缩振动、芳香化合物中的sp3 C-N键的伸缩振动和sp2 C＝N的伸缩振动。除此以外，在三元复合物中，位于2827cm-1处有一个新的吸收峰，它代表了CDs的C-H键的骨架振动。
图3为g-C3N4/CDs/β-FeOOH光催化材料的SEM和TEM图。从图3(a)可以看出，长度约为1μm的β-FeOOH负载在层状g-C3N4上。但是看不到CDs，这要是因为CDs的添加量很小，且本身尺寸也很小。图3(b)为g-C3N4/CDs/β-FeOOH的TEM图，图中可以进一步观察到棒状的β-FeOOH无序堆叠在片状g-C3N4上。图3(c)可以发现，在g-C3N4/β-FeOOH的表面存在粒径约为5nm的CDs，其中插图为CDs的晶格条纹像，条纹间距为0.205nm，对应CDs的(002)晶面。图3(d)中条纹间距0.74nm和0.34nm分别对应β-FeOOH的(110) 晶面和g-C3N4的(002)晶面。这表明了CDs负载在了基体上形成g-C3N4/CDs/β-FeOOH三元复合物。
图4为各样品在可见光照射下对RhB的光催化降解曲线。从图4中可以看出，未加入CDs的样品在经过60min的可见光照射后，降解率为71％，而加入CDs后的样品CCF1、CCF2 和CCF3的降解率分别为92％、100％、94％，其中当CDs的含量为6％时CCF2的光催化效率最高。
上面结合实施例对本发明的实施方式作了详细说明，但是本发明并不限于上述实施方式，对于本技术领域的普通技术人员来说，在获知本发明中记载内容后，在不脱离本发明原理的前提下，还可以对其作出若干同等变换和替代，这些同等变换和替代也应视为属于本发明的保护范围。
Claims (7)
1.一种g-C3N4/CDs/β-FeOOH光催化材料，其特征在于：β-FeOOH无序负载在层状g-C3N4上，CDs分散在β-FeOOH和g-C3N4的表面。
2.根据权利要求1所述的g-C3N4/CDs/β-FeOOH光催化材料，其特征在于：所述β-FeOOH为长度0.5～1.4μm的棒状；g-C3N4为不规则片状；CDs为粒径4～6nm的粒状。
3.根据权利要求1所述的g-C3N4/CDs/β-FeOOH光催化材料，其特征在于：所述g-C3N4和β-FeOOH形成复合光催化材料，该复合光催化材料中g-C3N4和β-FeOOH重量比为3:2。
4.一种如权利要求1～3任一项所述的g-C3N4/CDs/β-FeOOH光催化材料的制备方法，其特征在于：所述g-C3N4/CDs/β-FeOOH光催化材料是通过水热法一步合成的。
5.根据权利要求4所述的g-C3N4/CDs/β-FeOOH光催化材料的制备方法，其特征在于，包括以下步骤：
1)分别取g-C3N4和CDs分散水中超声并搅拌形成A溶液；
2)取FeCl3·6H2O溶于水中形成0.15mol/L的B溶液；
3)将B溶液倒入A溶液中搅拌，将搅拌液置于反应容器中升温至110～130℃，并保温10～15h，待反应釜冷却至室温后备用；
4)将冷却后反应液过滤取沉淀，干燥沉淀后即得g-C3N4/CDs/β-FeOOH光催化材料。
6.根据权利要求5所述的g-C3N4/CDs/β-FeOOH光催化材料的制备方法，其特征在于：CDs占g-C3N4/CDs/β-FeOOH光催化材料重量的1％～9％。
7.根据权利要求5所述的g-C3N4/CDs/β-FeOOH光催化材料的制备方法，其特征在于：沉淀的干燥条件为55～65℃下真空干燥24h。
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