CN113731410A - 一种Ag2V4O11/g-C3N4复合光催化剂的制备方法和应用 - Google Patents
一种Ag2V4O11/g-C3N4复合光催化剂的制备方法和应用 Download PDFInfo
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Abstract
本发明公开了一种Ag2V4O11/g‑C3N4复合光催化剂的制备方法和应用。在加热的磁力搅拌下,将AgNO3水溶液加入NH4VO3水溶液中,生成黄色絮状物;用HNO3调节溶液pH至2.2~2.6;继续在加热条件下搅拌;加入一定量的g‑C3N4,超声处理并搅拌后,进行水热反应得到产物;将产物用水和无水乙醇洗涤数次,干燥获得Ag2V4O11/g‑C3N4复合光催化剂。本发明通过简单的制备方法得到Ag2V4O11/g‑C3N4复合光催化剂,环境友好、催化效率高,具有广泛的应用前景。
Description
技术领域
本发明涉及一种Ag2V4O11/g-C3N4复合光催化剂的制备方法和应用,属于光催化剂及其制备技术领域。
背景技术
在提高人类的生活水平的同时,工业化和科技的飞速发展也引发了一系列环境问题。其中,水污染问题收到了国内外学者的持续而广泛的关注。
与各种水污染物相比,有机染料是最重要的环境污染物之一。染料废水色度高,化学性质稳定,对环境和生物体都具有毒害作用,所以,对染料废水的处理很重要。
1972年Fujishima 同Honda(Fujishima A, Honda K. Electrochemicalphotolysis of water at a semiconductor electrode[J]. Nature, 1972, 238(5358):37-38)首次提出了利用TiO2作为阳极材料,在紫外线辐照下水解产氢,这一发现标志着多相光催化技术开创性时期的开始。光催化降解方法因其操作便捷、适用范围广、环境友好和可循环利用等优点而被广泛研究。
石墨相氮化碳(g-C3N4)是一种非金属有机半导体光催化剂,禁带宽度2.7 eV,具有可见光活性,因其成本低廉,合成便捷,能带结构合适,可调性高,化学性质稳定和对热稳定优点,被广泛应用于光催化领域。然而,g-C3N4比表面积小,可见光响应范围窄,量子产率低,电子-空穴对易复合等问题,限制了其在光催化领域的应用。为改善这些缺陷,研究人员做了许多尝试,其中,异质结的构建是最为有效的方法之一。
Ag2V4O11属于过渡V族氧化物,由于其禁带宽度窄(1.8~2.08 eV)、电子转移速率快和能带结构合适,近年来,许多研究将Ag2V4O11应用于光催化领域。
发明内容
本发明旨在提供一种Ag2V4O11/g-C3N4复合光催化剂的制备方法及其应用,以拓宽g-C3N4的可见光响应范围,抑制其光生载流子复合,提高其光催化活性。
本发明中,采用Ag2V4O11改性g-C3N4可以促进半导体光生电子-空穴对的分离和迁移,缩短g-C3N4的禁带宽度,提高其光催化活性。
本发明提供了一种Ag2V4O11/g-C3N4复合光催化剂的制备方法,包括以下步骤:
(1)将160 ~ 220 mg 的AgNO3溶解在20 mL蒸馏水中,得到溶液A;
(2)在加热的磁力搅拌下,将220 ~ 300 mg的NH4VO3溶解在50 mL蒸馏水中,得到溶液B;
(3)在搅拌状态下,将溶液A滴加到溶液B中,用HNO3 调节溶液pH至2.2~2.6,在加热条件下持续搅拌30~60 min;
(4)室温下,在上述混合溶液中加入0.1 ~ 2 g 的g-C3N4,超声30~120 min,并在室温下搅拌10~24 h。
(5)将步骤(4)获得的混合液倒入高压釜中,在160~190 ℃进行水热反应16 h。反应产物用蒸馏水和无水乙醇分别洗涤数次,在50~80 ℃下干燥8~24 h。
上述制备方法中,所述AgNO3水溶液的浓度为8~11 g/L。
上述制备方法中,所述NH4VO3水溶液的浓度4.4~6 g/L。
上述制备方法中,所述步骤(2)和(3)中,溶液的加热温度为20~60 ℃。
本发明提供了上述制备方法制得的Ag2V4O11/g-C3N4复合光催化剂。
本发明提供了上述Ag2V4O11/g-C3N4复合光催化剂在光催化反应降解活性蓝19中的应用。
上述的应用,向250 mL,20 mg/L的活性蓝19溶液中加入0.1~0.4 g/L 的Ag2V4O11/g-C3N4催化剂,黑暗条件下超声分散10 min后,置于暗箱中磁力搅拌30 min达到吸附-解吸平衡;之后采用300 W氙灯并加420 nm滤光片作为可见光源,反应时间为60 min,每隔10min取一个样,离心后取上清液,测其吸光度;根据吸光度的值算出相应的浓度值;根据去除率公式(1)即可获得活性蓝19的去除率:
其中:C0是活性蓝19的初始浓度,mg·L-1;
Ct是t时刻后活性蓝19的浓度,mg·L-1。
本发明的有益效果:
(1)本发明利用一锅水热法合成了Ag2V4O11/g-C3N4复合光催化剂,操作便捷,合成简单。
(2)本发明利用带隙窄、可见光响应范围宽、光生载流子复合率低的Ag2V4O11改性g-C3N4,拓宽其可见光响应范围,提高其量子产率,降低其光生电子-空穴复合率,进而达到提高g-C3N4的光催化性能的目的。
(3)本发明制备的催化剂在降解模型污染物活性蓝19时,可在60 min内达到完全降解。
(4)本发明制备的催化剂降解效果好、用量少、环境友好,可在水污染领域广泛应用。
附图说明
图1为实施例1中制备的g-C3N4、Ag2V4O11和Ag2V4O11/g-C3N4复合材料的X射线衍射图谱;
图2为实施例1中制备的Ag2V4O11/g-C3N4复合材料的SEM图;
图3为实施例1中制备的g-C3N4、Ag2V4O11和Ag2V4O11/g-C3N4复合催化剂的紫外-可见漫反射光谱图;
图4为实施例1中制备的g-C3N4、Ag2V4O11和Ag2V4O11/g-C3N4复合催化剂的带隙图;
图5为实施例1中制备的g-C3N4、Ag2V4O11和Ag2V4O11/g-C3N4复合催化剂的PL图;
图6为实施例1中制备的g-C3N4、Ag2V4O11和Ag2V4O11/g-C3N4复合催化剂对20 mg/L活性蓝19的降解效果图。
具体实施方式
下面通过实施例来进一步说明本发明,但不局限于以下实施例。
实施例1
(1)称取200 mg AgNO3溶解在20 mL蒸馏水中,得到溶液A;
(2)在40 ℃的磁力搅拌下,将274 mg NH4VO3溶解在50 mL蒸馏水中,得到溶液B;
(3)将溶液A倾倒入溶液B中,用1 M HNO3 调节溶液pH至2.45,在加热条件下持续搅拌30 min;
(4)室温下,加入0.2955 g g-C3N4,超声60 min,搅拌11 h;
(5)将步骤(4)获得的混合液在180 ℃下进行水热反应16 h,反应产物用蒸馏水和无水乙醇分别洗涤三次,在60 ℃下干燥14 h。
应用试验:
配制250 mL 20 mg/L的活性蓝19溶液,然后加入0.05 g Ag2V4O11/g-C3N4催化剂,分别进行光催化反应。黑暗条件下超声分散10 min后,置于暗箱中磁力搅拌20 min达到吸附平衡;之后采用300 W氙灯并加420 nm滤光片作为可见光源,反应时间为60 min,每隔10min取一个样,离心后测其吸光度。然后以时间(t)为横坐标,C/C0为纵坐标绘制曲线,如图6所示。
图1为实施例1中制备的g-C3N4、Ag2V4O11和Ag2V4O11/g-C3N4复合催化剂的X射线衍射图谱,通过与标准卡片(JCPDS 87-1526)对比可知,单体g-C3N4在13.1°和27.92°处分别有两个明显的衍射峰,分别对应于(001)和(002)晶面。单体Ag2V4O11显示了相对标准卡(JCPDS49-0166)的主要特征峰。在Ag2V4O11/g-C3N4的XRD图谱中发现了g-C3N4和Ag2V4O11和的特征峰,说明Ag2V4O11成功复合到g-C3N4中。
图2 为实施例1中制备样品Ag2V4O11/g-C3N4的SEM图,由图可观察到Ag2V4O11纳米线从不同方向插入块状g-C3N4中,被小块的g-C3N4部分或完全的紧密包裹。
图3为实施例1中制备g-C3N4、Ag2V4O11和Ag2V4O11/g-C3N4复合催化剂的DRS图谱。经对比发现,相较于单体g-C3N4而言,二元复合物Ag2V4O11/g-C3N4的可见光吸收边由470 nm红移至495 nm,拓宽了可见光响应范围。
图4为实施例1中制备g-C3N4、Ag2V4O11和Ag2V4O11/g-C3N4复合催化剂的hv图谱。由图发现,禁带宽度由g-C3N4的2.74 eV缩小到了Ag2V4O11/g-C3N4的2.64 eV.
图5为实施例1制备g-C3N4、Ag2V4O11和Ag2V4O11/g-C3N4复合催化剂的PL图谱。可以观察到,g-C3N4在~470 nm处有较强的发射峰,Ag2V4O11/g-C3N4复合催化剂在~470 nm处发射峰极低,催化剂的光生电子空穴对复合现象得到了有效抑制。
图6为实施例1中制备g-C3N4、Ag2V4O11和Ag2V4O11/g-C3N4复合催化剂在可见光下对20mg/L 活性蓝19的降解曲线。实验发现,经过60 min的可见光照射后,单体g-C3N4仅能降解44.44%的活性蓝19,二元复合物Ag2V4O11/g-C3N4对活性蓝19溶液的60 min降解率为100%。
实施例2
(1)称取180 mg AgNO3溶解在20 mL蒸馏水中,得到溶液A;
(2)在20 ℃的磁力搅拌下,将247 mg NH4VO3溶解在50 mL蒸馏水中,得到溶液B;
(3)将溶液A逐滴加入溶液B中,用1 M HNO3 调节溶液pH至2.55,在加热条件下持续搅拌40 min;
(4)室温下,加入0.4 g g-C3N4,超声90 min,搅拌14 h;
(5)将步骤(4)获得的混合液在170 ℃下进行水热反应16 h,反应产物用蒸馏水和无水乙醇分别洗涤三次,在70 ℃下干燥10 h。
应用试验:
配制250 mL 20 mg/L的活性蓝19溶液,然后加入0.05 g Ag2V4O11/g-C3N4催化剂,分别进行光催化反应。黑暗条件下超声分散10 min后,置于暗箱中磁力搅拌20 min达到吸附平衡;之后采用300 W氙灯并加420 nm滤光片作为可见光源,反应时间为60 min,每隔10min取一个样,离心后测其吸光度。然后以时间(t)为横坐标,C/C0为纵坐标绘制曲线,测试该二元催化剂的降解性能。实验发现,经过60 min的可见光照射后,二元复合物Ag2V4O11/g-C3N4对活性蓝19溶液的60 min降解率为98.9%。
实施例3
(1)称取170 mg AgNO3溶解在10 mL蒸馏水中,得到溶液A;
(2)在60 ℃的磁力搅拌下,将233 mg NH4VO3溶解在50 mL蒸馏水中,得到溶液B;
(3)将溶液A倾倒入溶液B中,用1 M HNO3 调节溶液pH至2.50,在加热条件下持续搅拌50 min;
(4)室温下,加入1.0 g g-C3N4,超声120 min,搅拌24 h;
(5)将步骤(4)获得的混合液在170 ℃下进行水热反应16 h,反应产物用蒸馏水和无水乙醇分别洗涤三次,在70 ℃下干燥20 h。
应用试验:
配制250 mL 20 mg/L的活性蓝19溶液,然后加入0.05 g 20% Ag2V4O11/g-C3N4催化剂,分别进行光催化反应。黑暗条件下超声分散10 min后,置于暗箱中磁力搅拌20 min达到吸附平衡;之后采用300 W氙灯并加420 nm滤光片作为可见光源,反应时间为60 min,每隔10 min取一个样,离心后测其吸光度。然后以时间(t)为横坐标,C/C0为纵坐标绘制曲线,测试该二元催化剂的降解性能。实验发现,经过60 min的可见光照射后,二元复合物Ag2V4O11/g-C3N4对活性蓝19溶液的60 min降解率为99.8%。
Claims (7)
1.一种Ag2V4O11/g-C3N4复合光催化剂的制备方法,其特征在于包括以下步骤:
(1)将160 ~ 220 mg的AgNO3超声溶解在20 mL蒸馏水中,得到溶液A;
(2)在加热、磁力搅拌下,将220 ~ 300 mg 的NH4VO3溶解在50 mL蒸馏水中,加热得到溶液B;
(3)在搅拌状态下,将溶液A滴加入溶液B中,用HNO3 调节溶液pH至2.2~2.6,在加热条件下持续搅拌30~60 min;
(4)室温下,在上述混合溶液中加入0.1 ~ 2 g 的g-C3N4,超声30~120 min并在室温下搅拌10~24 h;
(5)将步骤(4)获得的混合液倒入到高压釜中,进行水热反应,反应产物用蒸馏水和无水乙醇分别洗涤数次,在50~80 ℃下干燥8~24 h。
2.根据权利要求1所述的Ag2V4O11/g-C3N4复合光催化剂的制备方法,其特征在于:所述步骤(2)和(3)中,加热温度为20~60 ℃。
3.根据权利要求1所述的Ag2V4O11/g-C3N4复合光催化剂的制备方法,其特征在于:所述步骤(5)中,水热反应的温度为160~190 ℃,反应时间为16 h。
4.一种权利要求1~3任一项所述的制备方法制得的Ag2V4O11/g-C3N4复合光催化剂。
5.一种权利要求4所述的Ag2V4O11/g-C3N4复合光催化剂在光催化反应降解活性蓝19的应用。
6.根据权利要求5所述的应用,其特征在于:每L活性蓝19溶液中,催化剂的用量为0.1~ 0.4 g。
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