CN116143249A - 基于改性生物炭的高电子传递效率的光电催化三维粒子电极的制备方法及其应用 - Google Patents
基于改性生物炭的高电子传递效率的光电催化三维粒子电极的制备方法及其应用 Download PDFInfo
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Abstract
基于改性生物炭的高电子传递效率的光电催化三维粒子电极的制备方法及其应用,本发明为了解决含高浓度Cl‑废水中的难降解污染物处理效果不佳的问题。制备方法:一、以植物秸秆为原料,在真空管式炉中对植物秸秆进行热解,热解后转移到盐酸溶液中浸泡,得到生物炭;二、利用水滑石改性生物炭;三、将改性生物炭加入到AQDS溶液中,搅拌形成悬浊液,悬浊液转移到反应釜中进行水热反应,抽滤收集固相反应物,得到光电催化三维粒子电极。本发明制备得到的粒子电极的主体生物炭能在通电情况下极化,在高盐废水中,AQDS从基态跃迁到单线激发态,氯离子与三线激发态发生反应,生成三元复合物和超氯自由基,对有机污染物光电催化效果优异。
Description
技术领域
本发明属于环保和水处理技术领域,具体涉及一种基于改性生物炭的三维粒子电极的制备方法,并应用于光电催化处理高盐废水中的难降解污染物。
背景技术
随着工业、农业和人类活动的发展,水污染已成为世界各国人民面临的共同问题和挑战,部分处理或大部分未经处理的生活和工业废水是水污染的主要来源,这些污染物中的绝大多数对环境来说具有持久性,传统的废水处理技术对这些污染物的处理效果有限,这些污染物威胁着人类和动物的健康,其中,药物、化学品、染料等常见的有机污染物可以通过生物方法去除,但生物技术处理周期长,对某些污染物的去除效率低,相比之下,化学技术在高效率降解污染物方面更具优势,而在化学技术中高级氧化技术是最有效的污染物去除方法。光催化处理技术一直是研究最广泛的高级氧化技术,但受光生载流子易复合这一缺点的限制,光电催化则可以通过对***施加电流,使得光生载流子有效分离,提高污染物去除效率。
抗生素等污染物广泛存在于含盐废水中,如海水养殖废水、生产废水及海水,污水处理厂的常规处理并不能有效消除抗生素这类难降解污染物,并且,当水体中含有盐分时会导致微生物脱水和质壁分离,抑制酶活性,因此,当处理含有大量含盐废水时,会显著抑制生物处理效果。光催化处理技术能有效去除污水中的难降解物质,而氯离子被认为是空穴或羟基自由基的猝灭剂,但当氯化物浓度较高时,它会通过生成Cl2 -促进水中污染物的降解,因此,研究在含盐废水中降解难降解污染物的先进处理方法至关重要。
在三维电催化***中,每个电极粒子均独立充当了电解池,因此,电化学氧化和还原反应不仅发生在主电极上,而且发生在颗粒电极表面,但相对光电催化,其耗能更高,而目前光电催化多处于二维***电极材料的研究上,将三维电催化和光催化结合的研究很少报道。
发明内容
本发明的目的是为了解决含高浓度Cl-废水中的难降解污染物处理效果不佳的问题,而提供一种基于改性生物炭的高电子传递效率的光电催化三维粒子电极的制备方法及其应用。
本发明基于改性生物炭的高电子传递效率的光电催化三维粒子电极的制备方法按照以下步骤实现:
一、以植物秸秆为原料,在真空管式炉中对植物秸秆进行热解,热解过程通入氮气,以350~500℃的温度处理2~4h,热解后转移到盐酸溶液中浸泡,再经洗涤、干燥后得到生物炭;
二、配置MgCl2-AlCl3混合溶液,其中MgCl2的浓度为0.2~0.4mol/L,AlCl3的浓度为0.1~0.2mol/L,将生物炭浸渍于MgCl2-AlCl3混合溶液中,通过NaOH-Na2CO3混合溶液调节体系的pH至7~9,在80~90℃温度下反应20~26h,在100~120℃条件下烘干,研磨过筛得到水滑石改性生物炭;
三、将蒽醌-2,6-磺酸钠(AQDS)超声溶于水中,得到浓度为0.8~1.2g/L的AQDS溶液,将水滑石改性生物炭加入到AQDS溶液中,搅拌形成悬浊液,悬浊液转移到反应釜中在160℃~200℃温度下水热反应15~20h,抽滤收集固相反应物,经洗涤、干燥处理后得到光电催化三维粒子电极。
本发明基于改性生物炭的高电子传递效率的光电催化三维粒子电极的应用是将该光电催化三维粒子电极置于光电催化***中处理含高浓度Cl-废水中的难降解污染物。
本发明制备得到的粒子电极的主体改性生物炭能在***通电情况下极化,可完成电催化对污染物的降解过程,另外在高盐废水中,***受到光照后,AQDS从基态跃迁到单线激发态,然后跃迁到三线激发态,氯离子与三线激发态发生反应,形成一个电荷转移二元激态络合物,其与Cl-继续反应生成三元复合物和超氯自由基,然后氧气得到半醌基离子的电子,生成超氧阴离子。上述过程生成的自由基能将污水中的污染物氧化降解,在本发明中Cl-对水中污染物的降解起到了促进作用,使用水滑石改性生物炭,水滑石改性生物炭能对氯离子特异性吸附,保证活性氯离子稳定,增加了生物炭对水中氯离子的吸附效果,另外将光敏剂AQDS负载到粒子电极上,增大了受光面积,并且AQDS对可见光有响应。
附图说明
图1为本发明基于改性生物炭的高电子传递效率的光电催化三维粒子电极在光电催化***降解污染物机理图;
图2为实施例制备的BC/AQDS粒子电极在光电催化***中对磺胺甲恶唑(10mg/L)的降解曲线和对比曲线图,其中1代表有粒子电极,2代表无粒子电极;
图3为实施例制备的BC/AQDS粒子电极在光电催化***中对磺胺甲恶唑(10mg/L)的矿化曲线和对比曲线图,其中1代表有粒子电极,2代表无粒子电极。
图4为实施例制备的BC/AQDS粒子电极电镜图;
图5为实施例制备的BC/AQDS粒子电极在含氯离子或不含氯离子光电催化***中对磺胺甲恶唑(10mg/L)的降解曲线图,其中1代表含氯离子,2代表不含氯离子。
具体实施方式
具体实施方式一:本实施方式基于改性生物炭的高电子传递效率的光电催化三维粒子电极的制备方法按照以下步骤实施:
一、以植物秸秆为原料,在真空管式炉中对植物秸秆进行热解,热解过程通入氮气,以350~500℃的温度处理2~4h,热解后转移到盐酸溶液中浸泡,再经洗涤、干燥后得到生物炭;
二、配置MgCl2-AlCl3混合溶液,其中MgCl2的浓度为0.2~0.4mol/L,AlCl3的浓度为0.1~0.2mol/L,将生物炭浸渍于MgCl2-AlCl3混合溶液中,通过NaOH-Na2CO3混合溶液调节体系的pH至7~9,在80~90℃温度下反应20~26h,在100~120℃条件下烘干,研磨过筛得到水滑石改性生物炭;
三、将蒽醌-2,6-磺酸钠(AQDS)超声溶于水中,得到浓度为0.8~1.2g/L的AQDS溶液,将水滑石改性生物炭加入到AQDS溶液中,搅拌形成悬浊液,悬浊液转移到反应釜中在160℃~200℃温度下水热反应15~20h,抽滤收集固相反应物,经洗涤、干燥处理后得到光电催化三维粒子电极。
本实施方式改性生物炭具有好的吸附性,对污染物和水中氯离子的吸附效果良好,且其本身良好的电子传递效果使得整个***的电子传递更加活跃,增强了粒子电极的电催化效果,AQDS又能够对可见光响应,利用Cl-对污染物进行降解,因此整个***的光电催化效果极佳。
具体实施方式二:本实施方式与具体实施方式一不同的是步骤一中所述的植物秸秆为水稻秸秆、小麦秸秆或者玉米秸秆。
具体实施方式三:本实施方式与具体实施方式一或二不同的是步骤一中热解过程控制氮气的流量为0.15~0.2L/min,加热速率为13~16℃/min。
具体实施方式四:本实施方式与具体实施方式一至三之一不同的是步骤一中以500℃的温度处理2.5h。
具体实施方式五:本实施方式与具体实施方式一至四之一不同的是步骤一中热解后转移到1mol/L的盐酸溶液中浸泡15h~20h。
具体实施方式六:本实施方式与具体实施方式一至五之一不同的是步骤二中MgCl2-AlCl3混合溶液中MgCl2的浓度为0.3mol/L,AlCl3的浓度为0.15mol/L。
具体实施方式七:本实施方式与具体实施方式一至六之一不同的是步骤二中调节体系的pH至8。
具体实施方式八:本实施方式与具体实施方式一至七之一不同的是步骤三中水热反应的温度为180℃,反应时间为16h。
具体实施方式九:本实施方式与具体实施方式一至八之一不同的是步骤三得到的光电催化三维粒子电极的直径为2~4mm。
具体实施方式十:本实施方式与具体实施方式一至九之一不同的是每100mg三维粒子电极中蒽醌-2,6-磺酸钠的负载量为5~8mg。
具体实施方式十一:本实施方式基于改性生物炭的高电子传递效率的光电催化三维粒子电极的应用是将该光电催化三维粒子电极置于光电催化***(体系)中处理含高浓度Cl-废水中的难降解污染物。
本实施方式光电催化***(体系)中施加机械搅拌。
具体实施方式十二:本实施方式与具体实施方式十一不同的是光电催化***中施加电压为6V。
实施例:本实施例基于改性生物炭的高电子传递效率的光电催化三维粒子电极的制备方法按照以下步骤实施:
一、以水稻秸秆为原料,在真空管式炉中对植物秸秆进行热解,热解过程通入0.18L/min的氮气,加热速率为14℃/min,以500℃的温度处理2.5h,热解后将热解样品转移到浓度为1mol/L的盐酸溶液中浸泡18h,依次经乙醇和去离子水洗涤,在60℃下干燥24h后得到生物炭;
二、配置MgCl2-AlCl3混合溶液,其中MgCl2的浓度为0.3mol/L,AlCl3的浓度为0.15mol/L,将生物炭浸渍于MgCl2-AlCl3混合溶液中,通过NaOH-Na2CO3混合溶液调节体系的pH至8,在85℃温度下反应24h,在110℃条件下烘干,研磨过筛得到水滑石改性生物炭;
三、将蒽醌-2,6-磺酸钠(AQDS)超声溶于水中,得到浓度为1g/L的AQDS溶液,将水滑石改性生物炭加入到AQDS溶液中,搅拌形成悬浊液,使AQDS吸附到使AQDS吸附到改性生物炭上,悬浊液转移到反应釜中进行水热反应,水热反应的温度为180℃,水热反应时间为16h,抽滤收集固相反应物,依次经乙醇和去离子水洗涤多次去除游离的AQDS,在真空干燥箱中以60℃干燥后得到光电催化三维粒子电极(改性生物炭/AQDS粒子电极)。
对本实施例得到的光电催化三维粒子电极进行水处理实验:
将磺胺甲恶唑作为目标污染物,配置浓度为10mg/L的磺胺甲恶唑溶液,溶液中Cl-浓度为0.5mg/L,取该溶液300mL,以石磨棒为主电极,施加的电压为6V,反应器体积为500mL,BC/AQDS粒子电极占反应器体积的1/3,光源为模拟可见光光源,每隔15min取一次水样,水样过0.45μm的滤膜。在该***中,120分钟内,磺胺甲恶唑的降解率可达到98.8%,矿化率(TOC去除率)达40%以上,光电体系下以光催化作用为主,电流作用为辅。在不加粒子电极的情况下,作为对比实验,发现磺胺甲恶唑的降解率和矿化率明显降低,无粒子电极的情况下120min降解率为69%,无氯离子的情况下降解率为68%,缺少氯离子和无粒子电极均对整个体系的污染物降解影响严重。因此可以证明,该粒子电极效果显著,在光电催化***中起到的作用巨大,性能优良。
Claims (10)
1.基于改性生物炭的高电子传递效率的光电催化三维粒子电极的制备方法,其特征在于该制备方法按下列步骤实现:
一、以植物秸秆为原料,在真空管式炉中对植物秸秆进行热解,热解过程通入氮气,以350~500℃的温度处理2~4h,热解后转移到盐酸溶液中浸泡,再经洗涤、干燥后得到生物炭;
二、配置MgCl2-AlCl3混合溶液,其中MgCl2的浓度为0.2~0.4mol/L,AlCl3的浓度为0.1~0.2mol/L,将生物炭浸渍于MgCl2-AlCl3混合溶液中,通过NaOH-Na2CO3混合溶液调节体系的pH至7~9,在80~90℃温度下反应20~26h,再在100~120℃条件下烘干,研磨过筛得到水滑石改性生物炭;
三、将蒽醌-2,6-磺酸钠超声溶于水中,得到浓度为0.8~1.2g/L的AQDS溶液,将水滑石改性生物炭加入到AQDS溶液中,搅拌形成悬浊液,悬浊液转移到反应釜中在160℃~200℃温度下水热反应15~20h,抽滤收集固相反应物,经洗涤、干燥处理后得到光电催化三维粒子电极。
2.根据权利要求1所述的基于改性生物炭的高电子传递效率的光电催化三维粒子电极的制备方法,其特征在于步骤一中所述的植物秸秆为水稻秸秆、小麦秸秆或者玉米秸秆。
3.根据权利要求1所述的基于改性生物炭的高电子传递效率的光电催化三维粒子电极的制备方法,其特征在于步骤一中热解过程控制氮气的流量为0.15~0.2L/min,加热速率为13~16℃/min。
4.根据权利要求1所述的基于改性生物炭的高电子传递效率的光电催化三维粒子电极的制备方法,其特征在于步骤一中以500℃的温度处理2.5h。
5.根据权利要求1所述的基于改性生物炭的高电子传递效率的光电催化三维粒子电极的制备方法,其特征在于步骤一中热解后转移到1mol/L的盐酸溶液中浸泡15h~20h。
6.根据权利要求1所述的基于改性生物炭的高电子传递效率的光电催化三维粒子电极的制备方法,其特征在于步骤二中MgCl2-AlCl3混合溶液中MgCl2的浓度为0.3mol/L,AlCl3的浓度为0.15mol/L。
7.根据权利要求1所述的基于改性生物炭的高电子传递效率的光电催化三维粒子电极的制备方法,其特征在于步骤三得到的光电催化三维粒子电极的直径为2~4mm。
8.根据权利要求1所述的基于改性生物炭的高电子传递效率的光电催化三维粒子电极的制备方法,其特征在于每100mg三维粒子电极中蒽醌-2,6-磺酸钠的负载量为5~8mg。
9.如权利要求1制备得到的基于改性生物炭的高电子传递效率的光电催化三维粒子电极的应用,其特征在于将该基于改性生物炭的高电子传递效率的光电催化三维粒子电极置于光电催化***中处理含高浓度Cl-废水中的难降解污染物。
10.根据权利要求9所述的基于改性生物炭的高电子传递效率的光电催化三维粒子电极的应用,其特征在于光电催化***中施加电压为6V。
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