CN106830277A - 一种紫外过硫酸盐去除污水中非甾体抗炎药的高级氧化方法 - Google Patents
一种紫外过硫酸盐去除污水中非甾体抗炎药的高级氧化方法 Download PDFInfo
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Abstract
本发明公开了一种紫外过硫酸盐去除污水中非甾体抗炎药的高级氧化方法,污水自流至二沉池,进行沉淀分离,加入NaS2O8溶液,开启UV灯管,进行光氧化反应,对出水进行结果分析,然后送入接触消毒池与ClO2反应消毒,最后安全排放。本发明使用UV高级氧化工艺,可有效去除污水中的非甾体抗炎药,使污水排放达到要求,降低了非甾体抗炎药的环境风险,本方法具有设备简单、操作简便、经济合理等优点,同时有高效的处理效果和高稳定性。
Description
技术领域
本发明涉及残留非甾体抗炎药处理技术领域,具体是一种紫外过硫酸盐去除污水中非甾体抗炎药的高级氧化方法。
背景技术
非甾体抗炎药是一类临床中广泛应用的消炎药物,在我国每年的用量仅次于抗感染药。按化学结构非甾体抗炎药可分为以下种类:甲酸类,如阿司匹林;乙酸类,如双氯芬酸、吲哚美辛;丙酸类,如布洛芬、萘普生;昔康类,如吡罗昔康、美洛昔康;昔布类,如塞来昔布、罗非昔布;吡唑酮类,如保泰松、氨基比林;其他,如尼美舒利。这些药物经人服用后不能全部被人体吸收,剩余部分会随尿液、粪便排出体外进入环境。而污水处理厂是其主要集聚地。作为一类新型污染物,现有毒性研究表明非甾体抗炎药会对青鳉鱼、斑马鱼、大型蚤、浮萍等水生生物产生生态毒性。药物的大量使用及滥用,使得该类物质及其活性组分被持续不断地输入到水体环境中,药物的特性(旋光性、半挥发性、极性及高毒性等点)和水体环境自身存在的演变规律决定了这些物质将在水体环境中进行持续不断地长距离迁移扩散,并形成普遍性累积,其归趋的不确定性给人类健康形成了不可预测的潜在风险。因此,如何在污水处理系统中有效去除非甾体抗炎药日益受到人们的关注。
研究表明,污水处理厂现有处理技术不能有效去除非甾体抗炎药,导致这些药物随污水厂尾水源源不断输入环境水体中并形成普遍性累积,能够长期作用于水生态系统,对水环境产生潜在威胁,进而直接或间接影响饮用水质量,危害人体健康。
污水的深度处理工艺作为保障污水安全排放的重要环节,研究不同的深度处理工艺对非甾体抗炎药去除的效果具有重要意义。目前的一些深度处理工艺中,活性炭吸附、混凝沉淀、氯化消毒对非甾体抗炎药去除效果不理想。过氧化氢对非甾体抗炎药没有去除效果,臭氧高级氧化工艺在实际污水处理厂的投加剂量和接触时间下,也只能部分去除非甾体抗炎药。使用UV高级氧化工艺去除实际污水中的非甾体抗炎药尚无系统的研究。
发明内容
本发明解决的技术问题是提供一种紫外过硫酸盐去除污水中非甾体抗炎药的高级氧化方法,该方法对于双氯芬酸、布洛芬、萘普生均有更优的去除效果,能有效去除污水中的非甾体抗炎药。
本发明的技术方案是:一种紫外过硫酸盐去除污水中非甾体抗炎药的高级氧化方法,主要包括以下步骤:
步骤一:污水重力自流至二沉池,通过二沉池进行沉淀分离,然后取分离后的上清液,利用高效液相色谱串联质谱法对上清液中残留的非甾体抗炎药浓度进行检测,并记录检测数据;
步骤二:取二沉池分离后的上清液,在上清液中加入质量浓度为50-70%的NaS2O8溶液,使得NaS2O8与非甾体抗炎药的摩尔浓度比为(1-100):1,得到反应液,然后将反应液放入光反应器中反应,使用UV光照5-10min,通过电磁搅拌保持反应液中的各成分浓度均匀,光照功率为22W。
步骤三:将步骤二中反应结束后的溶液进行处理结果分析,使用高效液相色谱串联质谱法进行非甾体抗炎药浓度检测,计算去除率并进行动力学模拟,然后送入接触消毒池与ClO2反应消毒杀死病原微生物,最后将接触消毒池的出水排放。
进一步的,所述的二沉池为竖流式沉淀池,池体截面为圆形,污水自上而下流动,流速为15-25mm/s,底部设置螺旋形挡板使污水在池中均匀分布,过水断面上升速度为0.6-0.8mm/s,沉淀时间采用1.5-2.5h,悬浮物沉降进入池底锥形沉泥斗中,澄清水从池四周沿周边溢流堰流出,堰前设挡板及浮渣槽以截留浮渣保证出水水质,靠池壁设有排泥管,排泥管管径为300-400mm,靠静水压将泥定期排出。
进一步的,所述的非甾体抗炎药浓度的检测方法为:
(1)提取样品:取500mL水样用0.22μm混合纤维膜过滤,过滤后存于4℃冰箱中以待后续的固相萃取操作以及随之的非甾体抗炎药浓度测定,每个实验重复三次,取平均值±标准偏差进行分析;
(2)样品纯化:选用的固相萃取柱为CNW HLB(60mg,3mL)水相——有机平衡小柱,具体步骤如下:
a.用3mL甲醇平衡CNW HLB小柱;
b.用3mL纯水洗涤CNW HLB小柱;
c.将50mL水样以5mL/min的速度通过CNW HLB小柱;
d.用3mL5%甲醇再次洗涤CNW HLB小柱;
e.用6mL甲醇溶液洗脱,洗脱液氮吹定容至1mL,存于4℃冰箱,以待后续的上机检测;
(3)液质联用检测非甾体抗炎药浓度:选用的液质联用仪,采用电喷雾离子源(ESI),负电离多反应监测模式(MRM);液相分离选用的色谱柱为Acquity UPLC BEH C18色谱柱(2.1×50mm,1.7um),柱温保持在30℃,所选用的流动相为水(A)和甲醇(B),流动相使用前超声脱气,液相流速为0.1mL/min,A相比例20%,B相比例80%,等度洗脱5min。进样量为10μL,采用自动进样器进样。
进一步的,所述的非甾体抗炎药的去除率=(1-Ct/C0)×100%,其中,C0为初始浓度,Ct为反应时间t时的非甾体抗炎药浓度,动力学模拟时,纵坐标为Ln(C0/Ct),其中C0为初始浓度,Ct为反应时间t时的非甾体抗炎药浓度,所述的非甾体抗炎药的浓度单位为μg/L。
进一步的,所述的光反应器由石英玻璃制成,中间竖直放置石英管套,石英管内放置紫外灯,通过紫外灯发出紫外光,进行光反应作用。
进一步的,所述的紫外灯为低压汞灯,发出254nm单色紫外光,石英管壁外壁紫外光强度为1.35mW/cm2。
进一步的,所述的接触消毒池上接有ClO2发生器,所述的ClO2发生器是一种复合式多级二氧化氯发生器,是由釜式反应器通过耐酸导管和水射式真空机组组成,釜式反应器采用的是两级或多级反应器,主反应釜内设有空气分布器,副反应釜设置了平衡管,使反应更彻底,反应后的残液可达标排放。生成的二氧化氯制得水溶液,也可以制得稳定二氧化氯溶液,利用反应原理:NaClO3+2HCl=ClO2+1/2Cl2+NaCl+H2O,可以与ClO2反应消毒杀灭水中的致病微生物。
本发明的有益效果是:
1、本发明使用UV高级氧化工艺,通过催化分解氧化剂NaS2O8,产生氧化性极强的硫酸根自由基(·SO4 -)从而使水中多种污染物分解或矿化,可有效去除污水中的非甾体抗炎药,使污水排放达到要求,避免了对环境的污染,
2、本发明的方法处理效果好,也更为经济,具有设备简单、操作简便、费用便宜等优点,且无污染、稳定性高。
3、本发明弥补了目前污水净化工艺的不足,改进现有技术对非甾体抗炎药效果差、运行不稳定的缺点,填补了国内外有关水源中非甾体抗炎药去除技术的空白。
说明书附图
图1是本发明的一种紫外过硫酸盐去除污水中非甾体抗炎药的高级氧化方法的操作流程图;
图2是本发明的一种紫外过硫酸盐去除污水中非甾体抗炎药的高级氧化方法中光照时间对非甾体抗炎药降解的影响关系图;
图3是本发明的一种紫外过硫酸盐去除污水中非甾体抗炎药的高级氧化方法氧化剂浓度对非甾体抗炎药去除效果的影响关系图;
具体实施方式
下面结合具体实施方式对本发明作进一步说明。
实施例1:该实施例是以南京某市政污水处理厂的二级生物出水为对象进行的,一种紫外过硫酸盐去除污水中非甾体抗炎药的高级氧化方法,主要包括以下步骤:
步骤一:污水通过管道,依靠污水重力自流至二沉池,通过二沉池进行沉淀分离,二沉池为竖流式沉淀池,池体截面为圆形,污水自上而下流动,流速为15mm/s,底部设置螺旋形挡板使污水在池中均匀分布,过水断面上升速度为0.6mm/s,沉淀时间采用1.5h,悬浮物沉降进入池底锥形沉泥斗中,澄清水从池四周沿周边溢流堰流出,堰前设挡板及浮渣槽以截留浮渣保证出水水质,靠池壁设有排泥管,排泥管管径为300mm,靠静水压将泥定期排出;然后取分离后的上清液,利用高效液相色谱法对上清液中残留的非甾体抗炎药浓度进行检测,并记录检测数据;
步骤二:取二沉池分离后的上清液,在上清液中加入质量浓度为50-70%的NaS2O8溶液,使得NaS2O8与非甾体抗炎药的摩尔浓度比为60:1,得到反应液,然后将反应液放入光反应器中反应,使用UV光照5min,通过电磁搅拌保持反应液中的各成分浓度均匀,光照功率为22W。光反应器由石英玻璃制成,中间竖直放置石英管套,石英管内放置紫外灯,通过紫外灯发出紫外光,进行光反应作用。紫外灯为低压汞灯,发出254nm单色紫外光,石英管壁外壁紫外光强度为1.35mW/cm2;
步骤三:将步骤二中反应结束后的溶液进行处理结果分析,使用高效液相色谱串联质谱法进行非甾体抗炎药浓度检测,计算去除率并进行动力学模拟,然后送入接触消毒池与ClO2反应消毒。接触消毒池上接有ClO2发生器,ClO2发生器是一种复合式多级二氧化氯发生器,是由釜式反应器通过耐酸导管和水射式真空机组组成,釜式反应器采用的是两级或多级反应器,主反应釜内设有空气分布器,副反应釜设置了平衡管,使反应更彻底,反应后的残液可达标排放。生成的二氧化氯制得水溶液,也可以制得稳定二氧化氯溶液,利用反应原理:NaClO3+2HCl=ClO2+1/2Cl2+NaCl+H2O,可以与ClO2反应消毒杀灭水中的致病微生物;最后将接触消毒池的出水排放。
实施例2:该实施例是以南京某市政污水处理厂的二级生物出水为对象进行的,一种紫外过硫酸盐去除污水中非甾体抗炎药的高级氧化方法,主要包括以下步骤:
步骤一:污水通过管道,依靠污水重力自流至二沉池,通过二沉池进行沉淀分离,二沉池为竖流式沉淀池,池体截面为圆形,污水自上而下流动,流速为15mm/s,底部设置螺旋形挡板使污水在池中均匀分布,过水断面上升速度为0.6mm/s,沉淀时间采用1.5h,悬浮物沉降进入池底锥形沉泥斗中,澄清水从池四周沿周边溢流堰流出,堰前设挡板及浮渣槽以截留浮渣保证出水水质,靠池壁设有排泥管,排泥管管径为300mm,靠静水压将泥定期排出;然后取分离后的上清液,利用高效液相色谱法对上清液中残留的非甾体抗炎药浓度进行检测,并记录检测数据;
步骤二:取二沉池分离后的上清液,在上清液中加入质量浓度为60%的NaS2O8溶液,使得NaS2O8与非甾体抗炎药的摩尔浓度比为50:1,得到反应液,然后将反应液放入光反应器中反应,使用UV光照7.5min,通过电磁搅拌保持反应液中的各成分浓度均匀,光照功率为22W。光反应器由石英玻璃制成,中间竖直放置石英管套,石英管内放置紫外灯,通过紫外灯发出紫外光,进行光反应作用。紫外灯为低压汞灯,发出254nm单色紫外光,石英管壁外壁紫外光强度为1.35mW/cm2;
步骤三:将步骤二中反应结束后的溶液进行处理结果分析,使用高效液相色谱串联质谱法进行非甾体抗炎药浓度检测,计算去除率并进行动力学模拟,然后送入接触消毒池与ClO2反应消毒。接触消毒池上接有ClO2发生器,ClO2发生器是一种复合式多级二氧化氯发生器,是由釜式反应器通过耐酸导管和水射式真空机组组成,釜式反应器采用的是两级或多级反应器,主反应釜内设有空气分布器,副反应釜设置了平衡管,使反应更彻底,反应后的残液可达标排放。生成的二氧化氯制得水溶液,也可以制得稳定二氧化氯溶液,利用反应原理:NaClO3+2HCl=ClO2+1/2Cl2+NaCl+H2O,可以与ClO2反应消毒杀灭水中的致病微生物;最后将接触消毒池的出水排放。
实施例3:该实施例是以南京某市政污水处理厂的二级生物出水为对象进行的,一种紫外过硫酸盐去除污水中非甾体抗炎药的高级氧化方法,主要包括以下步骤:
步骤一:污水通过管道,依靠污水重力自流至二沉池,通过二沉池进行沉淀分离,二沉池为竖流式沉淀池,池体截面为圆形,污水自上而下流动,流速为15mm/s,底部设置螺旋形挡板使污水在池中均匀分布,过水断面上升速度为0.6mm/s,沉淀时间采用1.5h,悬浮物沉降进入池底锥形沉泥斗中,澄清水从池四周沿周边溢流堰流出,堰前设挡板及浮渣槽以截留浮渣保证出水水质,靠池壁设有排泥管,排泥管管径为300mm,靠静水压将泥定期排出;然后取分离后的上清液,利用高效液相色谱法对上清液中残留的非甾体抗炎药浓度进行检测,并记录检测数据;
步骤二:取二沉池分离后的上清液,在上清液中加入质量浓度为70%的NaS2O8溶液,使得NaS2O8与非甾体抗炎药的摩尔浓度比为100:1,得到反应液,然后将反应液放入光反应器中反应,使用UV光照10min,通过电磁搅拌保持反应液中的各成分浓度均匀,光照功率为22W。光反应器由石英玻璃制成,中间竖直放置石英管套,石英管内放置紫外灯,通过紫外灯发出紫外光,进行光反应作用。紫外灯为低压汞灯,发出254nm单色紫外光,石英管壁外壁紫外光强度为1.35mW/cm2;
步骤三:将步骤二中反应结束后的溶液进行处理结果分析,使用高效液相色谱串联质谱法进行非甾体抗炎药浓度检测,计算去除率并进行动力学模拟,然后送入接触消毒池与ClO2反应消毒。接触消毒池上接有ClO2发生器,ClO2发生器是一种复合式多级二氧化氯发生器,是由釜式反应器通过耐酸导管和水射式真空机组组成,釜式反应器采用的是两级或多级反应器,主反应釜内设有空气分布器,副反应釜设置了平衡管,使反应更彻底,反应后的残液可达标排放。生成的二氧化氯制得水溶液,也可以制得稳定二氧化氯溶液,利用反应原理:NaClO3+2HCl=ClO2+1/2Cl2+NaCl+H2O,可以与ClO2反应消毒杀灭水中的致病微生物;最后将接触消毒池的出水排放。
应当注意,以上实施例中所涉及的数值范围都可以实现,篇幅所限,在此不进行其他值的列举。
一、实施例结果分析:
(1)取500ml水样用0.22μm混合纤维膜过滤,过滤后存于4℃冰箱中以待后续的固相萃取操作以及随之的非甾体抗炎药浓度测定。每个实验重复三次,取平均值±标准偏差进行分析。简单的实验流程如图1所示。
(2)三种非甾体抗炎药浓缩纯化
选用的固相萃取柱为上海安谱提供的CNW HLB(60mg,3mL)水相——有机平衡小柱。具体步骤如下:
a)用3mL甲醇平衡CNW HLB小柱;
b)用3mL纯水洗涤CNW HLB小柱;
c)将50mL水样以5mL/min的速度通过CNW HLB小柱;
d)用3mL 5%甲醇再次洗涤CNW HLB小柱;
e)用6mL甲醇溶液洗脱,洗脱液氮吹定容至1mL,存于4℃冰箱,以待后续的上机检测;
(3)液质联用检测非甾体抗炎药浓度:
所选用的液质联用仪器为美国Waters公司的Xevo TQ-S UPLC-MS液质联用仪,采用电喷雾离子源(ESI),负电离多反应监测模式(MRM)。多反应监测的参数见表1。
表1.非甾体抗炎药的多反应监测参数
液相分离选用的色谱柱为Acquity UPLC BEH C18色谱柱(2.1×50mm,1.7um),柱温保持在30℃。所选用的流动相为水(A)和甲醇(B)。流动相使用前超声脱气。液相流速为0.1mL/min,A相比例20%,B相比例80%,等度洗脱5min。进样量为10μL,采用自动进样器进样。
二、非甾体抗炎药去除率分析
本发明中非甾体抗炎药的浓度单位为μg/L
非甾体抗炎药的去除率=(1-Ct/C0)×100%,C0为初始浓度,Ct为反应时间t时的非甾体抗炎药浓度。动力学模拟时,纵坐标为Ln(C0/Ct),其中C0为初始浓度,Ct为反应时间t时的非甾体抗炎药浓度,测定的非甾体抗炎药包括双氯芬酸、布洛芬、萘普生。
经分析可知:
1、UV光照时间对目标污染物去除的影响
光照时间对三种非甾体抗炎药降解的影响如图2所示。双氯芬酸、布洛芬、萘普生三种非甾体抗炎药都可以在紫外光的照射下直接光解,三种非甾体抗炎药的降解反应均为一级反应动力学,反应速率常数分别为5.04×10-3s-1、0.291×10-3s-1、0.208×10-3s-1。
2、NaS2O8与非甾体抗炎药的摩尔浓度比对目标污染物去除的影响
如图3所示,使用22W低压汞灯照射5min时,NaS2O8与非甾体抗炎药的摩尔浓度在1:1~100:1时,随着氧化剂浓度的增加,所有目标污染物的去除率均增加。一般而言,当NaS2O8浓度过大时,·SO4 -产率增加,因此反应速率不断加快。本案例中三种非甾体抗炎药随着氧化剂投加量的增加,去除率也逐步增加。考虑到实际工艺运行的去除效果,选择100:1的氧化剂投加量为最优投加量。使用UV/NaS2O8工艺降解非甾体抗炎药时,三种物质的降解速率都有很大提高,5min去除率可以达到95%。
3、光源强度对目标污染物去除的影响
本实验选择了两种UV/AOP工艺中常见的紫外灯光源,分别为22W低压汞灯和300W的中压汞灯,100:1氧化剂投加量,5分钟反应条件下,对目标污染物的去除效果如表2所示。当使用22W低压汞灯时,对三种非甾体抗炎药已经有很好的去除效果,从能耗角度考虑,选择22W低压汞灯作为光源。
表2.两种光源对非甾体抗炎药的去除效果对比
综上所述,本发明的方法可有效去除污水中的非甾体抗炎药。由此表明,本发明方法中的各种组分和参数均是最佳选择,可实现本发明方法的最佳效果。
以上所述,仅是本发明的较佳实施例而已,并非是对本发明作其它形式的限制,任何熟悉本专业的技术人员可能利用上述揭示的技术内容加以变更或改型为等同变化的等效实施例。但是凡是未脱离本发明技术方案内容,依据本发明的技术实质对以上实施例所作的任何简单修改、等同变化与改型,仍属于本发明技术方案的保护范围。
Claims (7)
1.一种紫外过硫酸盐去除污水中非甾体抗炎药的高级氧化方法,其特征在于,主要包括以下步骤:
步骤一:污水重力自流至二沉池,通过二沉池进行沉淀分离,然后取分离后的上清液,对上清液中残留的非甾体抗炎药浓度进行检测,并记录检测数据;
步骤二:取二沉池分离后的上清液,在上清液中加入质量浓度为50-70%的NaS2O8溶液,使得NaS2O8与非甾体抗炎药的摩尔浓度比为(1-100):1,得到反应液,然后将反应液放入光反应器中反应,使用UV光照5-10min,通过电磁搅拌保持反应液中的各成分浓度均匀,光照功率为22W。
步骤三:将步骤二中反应结束后的溶液进行处理结果分析,使用高效液相色谱串联质谱法进行非甾体抗炎药浓度检测,计算去除率并进行动力学模拟。然后,送入接触消毒池与ClO2反应消毒,最后将接触消毒池的出水排放。
2.根据权利要求1所述的一种紫外过硫酸盐去除污水中非甾体抗炎药的高级氧化方法,其特征在于,所述的二沉池为竖流式沉淀池,池体截面为圆形,污水自上而下流动,流速为15-25mm/s,底部设置螺旋形挡板使污水在池中均匀分布,过水断面上升速度为0.6-0.8mm/s,沉淀时间采用1.5-2.5h,悬浮物沉降进入池底锥形沉泥斗中,澄清水从池四周沿周边溢流堰流出,堰前设挡板及浮渣槽以截留浮渣保证出水水质,靠池壁设有排泥管,排泥管管径为300-400mm,靠静水压将泥定期排出。
3.根据权利要求1所述的一种紫外过硫酸盐去除污水中非甾体抗炎药的高级氧化方法,其特征在于,所述的非甾体抗炎药浓度的检测方法为:
(1)提取样品:取500mL水样用0.22μm混合纤维膜过滤,过滤后存于4℃冰箱中以待后续的固相萃取操作以及随之的非甾体抗炎药浓度测定,每个实验重复三次,取平均值±标准偏差进行分析;
(2)样品纯化:选用的固相萃取柱为CNW HLB(60mg,3mL)水相——有机平衡小柱,具体步骤如下:
a.用3mL甲醇平衡CNW HLB小柱;
b.用3mL纯水洗涤CNW HLB小柱;
c.将50mL水样以5mL/min的速度通过CNW HLB小柱;
d.用3mL5%甲醇再次洗涤CNW HLB小柱;
e.用6mL甲醇溶液洗脱,洗脱液氮吹定容至1mL,存于4℃冰箱,以待后续的上机检测;
(3)液质联用检测非甾体抗炎药浓度:选用的液质联用仪,采用电喷雾离子源(ESI),负电离多反应监测模式(MRM);液相分离选用的色谱柱为Acquity UPLC BEH C18色谱柱(2.1×50mm,1.7μm),柱温保持在30℃,所选用的流动相为水(A)和甲醇(B),流动相使用前超声脱气,液相流速为0.1mL/min,A相比例20%,B相比例80%,等度洗脱5min。进样量为10μL,采用自动进样器进样。
4.根据权利要求1所述的一种紫外过硫酸盐去除污水中非甾体抗炎药的高级氧化方法,其特征在于,本发明所述非甾体抗炎药的去除率=(1-Ct/C0)×100%,其中,C0为初始浓度,Ct为反应时间t时的非甾体抗炎药浓度,动力学模拟时,纵坐标为Ln(C0/Ct),其中C0为初始浓度,Ct为反应时间t时的非甾体抗炎药浓度,所述的非甾体抗炎药的浓度单位为μg/L。
5.根据权利要求1所述的一种紫外过硫酸盐去除污水中非甾体抗炎药的高级氧化方法,其特征在于,所述的光反应器由石英玻璃制成,中间竖直放置石英管套,石英管内放置紫外灯,通过紫外灯发出紫外光。
6.根据权利要求4所述的一种紫外过硫酸盐去除污水中非甾体抗炎药的高级氧化方法,其特征在于,所述的紫外灯为低压汞灯,发出254nm单色紫外光,石英管壁外壁紫外光强度为1.35mW/cm2。
7.根据权利要求1所述的一种紫外过硫酸盐去除污水中非甾体抗炎药的高级氧化方法,其特征在于,所述的接触消毒池上接有ClO2发生器,与ClO2反应消毒杀灭水中的致病微生物。
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