CN116081760A - 一种光/声催化剂协同光/超声催化降解敌草隆的方法 - Google Patents
一种光/声催化剂协同光/超声催化降解敌草隆的方法 Download PDFInfo
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Abstract
本发明涉及一种光/声催化剂协同光/超声催化降解敌草隆的方法,该方法具体实施步骤为在含有敌草隆的废水中,加入光/声催化剂Sr0.7Ba0.3Bi2B2O7后,同时进行光源照射和超声辐射,完成敌草隆降解。本发明中Sr0.7Ba0.3Bi2B2O7催化剂的制备方法为固相反应法。本发明制备的Sr0.7Ba0.3Bi2B2O7催化剂具有光敏和声敏性能。与现有的单一光催化降解敌草隆的技术相比,引入超声波作为共同激发源,在提高催化降解水中敌草隆效率的同时,也可以结合二者的优点,有利于解决复杂废水环境中敌草隆的降解,有很好的应用前景,为其他降解水中敌草隆的方法的联用提供了新的思路。
Description
技术领域
本发明属于农药废水处理技术领域,具体涉及一种光/声催化剂协同光/超声催化降解敌草隆的方法。
背景技术
除草剂类农药作为一种基本的农业生产资料,在预防控制或消灭危害农林业的有害植物、提高粮食综合生产能力、维护保障人类社会稳定等方面发挥着极其重要的作用。但当除草剂的使用量或毒性超出了自然环境的自降解能力,残留在土壤中的农药会随雨水渗透地表,污染水体环境,带来一系列环境和生命健康问题。因此,探究水体环境中除草剂合理降解的新方法,消除除草剂的水体污染问题十分有必要。
敌草隆(Diuron,地草净,分子式C9H10C12N2O),化学名称为N'-(3,4-二氯苯基)-N,N-二甲基脲,是一种通过抑制ATP合成、干扰植物光合作用来除草的广谱、内吸性的除草剂。作为一种能量代谢抑制药物,敌草隆与人体接触也会干扰人体内分泌系统,具有致癌、致基因突变等危害。近年来,在美国、法国、日本、马来西亚等国家的水体环境中相继检测到敌草隆的存在,敌草隆的水体污染已成为世界范围内十分严重的环境和健康问题,敌草隆也被列为环境污染和饮用水中重点监测和优先处理的对象。
目前水中敌草隆的去除方法主要有吸附法、微生物法和高级氧化技术等。其中,高级氧化技术作为敌草隆水中降解研究最多的技术,主要利用催化剂、光、电等组分在体系中生成强氧化性物质,氧化分解敌草隆生成二氧化碳或其他无害离子。虽然这些高级氧化技术在破坏敌草隆研究中极具前景,但单一的氧化处理技术因其作用机理都存在着自身的局限性,如芬顿催化法对废水浓度、过氧化氢含量、pH值等有要求,光催化法中光的穿透能力有限、对浑浊废水效果有限。结合不同手段的优点,规避缺点,将有利于解决复杂废水环境中敌草隆的处理问题,对生态环境和长期人类健康十分有益。
发明内容
本发明的目的是提供一种光/声催化剂协同光/超声催化降解敌草隆的方法,该方法将穿透能力强的超声波引入光催化降解体系,通过光/超声联用、协同降解敌草隆。
本发明的目的可以通过以下技术方案来实现:一种光/声催化剂协同光/超声催化降解敌草隆的方法,该方法具体实施步骤为在含有敌草隆的废水中,加入光/声催化剂Sr0.7Ba0.3Bi2B2O7后,同时进行光源照射和超声辐射,完成敌草隆降解。
进一步地,所述的光/声催化剂Sr0.7Ba0.3Bi2B2O7的制备方法为先将一定比例的碳酸锶、碳酸钡、氧化铋以及硼酸在研钵中研磨混合均匀,再将混合物倒入坩埚中置于马弗炉中煅烧,冷却至室温后,再次研磨即得到粉末状光/声催化剂Sr0.7Ba0.3Bi2B2O7。
更进一步地,所述的碳酸锶、碳酸钡、氧化铋以及硼酸的摩尔比为0.7:0.3:1:2。
更进一步地,所述的碳酸锶、碳酸钡、氧化铋以及硼酸的研磨混合时间为30-45min。
更进一步地,所述的煅烧的升温程序为以6℃/min的升温速率升温至500℃煅烧2h,再以相同的升温速率继续升温至660℃煅烧6h;所述的煅烧在空气气氛下进行。
更进一步地,所述的混合物煅烧冷却后的研磨时间为20-40min。
进一步地,所述的光源包括氙灯;所述的氙灯的光照功率为0.8-1.2W/cm2。
进一步地,所述的超声辐射的超声源包括超声仪或超声发生器;所述的超声辐射的超声频率为0.5-1.0MHz,声强为1.5-2.0W/cm2。
进一步地,所述的光源照射和超声辐射的时间为10~60min。
进一步地,当废水中敌草隆浓度为10mg/L时,所使用的光/声催化剂Sr0.7Ba0.3Bi2B2O7的用量为0.5-1.0mg/mL。
与现有技术相比,本发明具有以下优点:
1、本发明将超声引入光催化降解敌草隆体系,提出了光/超声联用催化降解敌草隆的新方法,其中,通过固相反应法制得的Sr0.7Ba0.3Bi2B2O7催化剂为光/声催化剂,其同时具有光敏和声敏性能。在光或超声的照射下,Sr0.7Ba0.3Bi2B2O7催化剂均可以被激发产生电子空穴对,并进一步生成高氧化活性的物质降解敌草隆,且在光与超声共同照射下,降解效果最佳;
2、本发明一种光/声催化剂协同光/超声催化降解敌草隆的方法作为催化降解水中敌草隆的新方法,利用单一催化剂Sr0.7Ba0.3Bi2B2O7和不同照射源(氙灯和超声发生器),可适用于不同复杂环境(浑浊、深层)的含敌草隆废水降解,且使用的照射源功率较低,有很好的应用前景,为其他方法的联用提供了新的思路。
附图说明
图1为光/声催化剂Sr0.7Ba0.3Bi2B2O7的制备流程示意图;
图2为光/声催化剂Sr0.7Ba0.3Bi2B2O7的粉末X射线衍射图;
图3为光/超声协同催化降解敌草隆的降解示意图;
图4为实施例1和对比例1中检测敌草隆降解的紫外-可见吸收谱图;
图5为对比例2和对比例3中检测敌草隆降解的紫外-可见吸收谱图;
图6为实施例1和对比例1、2、3中敌草隆降解的速率对比图。
具体实施方式
下面将结合附图和实施例对本发明进行详细说明。需要指出的是,对本领域的普通技术人员来说,在不脱离本发明构思的前提下,还可以做出若干变化和改进。这些都属于本发明的保护范围。
本发明中,室温指环境温度为10℃~30℃。
以下实施例中所使用的试剂皆为市售试剂;以下实施例中使用的各种设备皆为市售设备。
本发明中,敌草隆的降解通过紫外可见吸收光谱在200~400nm范围内监测,其特征吸收峰在248nm。
实施例1
通过固相反应法制备Sr0.7Ba0.3Bi2B2O7的步骤如图1所示:准确称取0.2g碳酸锶(SrCO3)、0.12g碳酸钡(BaCO3)、0.98g氧化铋(Bi2O3)以及0.25g硼酸(H3BO3)混合置于玛瑙研钵中研磨30~45min。研磨结束后,将混合物转移至坩埚中,于空气环境中500℃煅烧2h除去水分和碳酸盐(升温速率为6℃/min),随后仍以同样的升温速率继续升温至660℃煅烧6h,冷却至室温后,重新研磨20-40min,得到白色产物Sr0.7Ba0.3Bi2B2O7。随后,通过X射线粉末衍射仪(D8DaVinci,德国布鲁克公司)鉴定物质种类,从图2数据可以看出,制得的材料的衍射峰与晶体结构数据库ICSD#245017(SrBi2B2O7)类似,由于掺杂了更大离子半径的钡离子(Ba2+:Sr2+:),其位于27-29°的衍射峰发生轻微的偏移,进一步证明了所得产物为Sr0.7Ba0.3Bi2B2O7。
该实施例制备的光/声催化剂对敌草隆的降解和检测方法如图3所示:准确称取5mg敌草隆溶于500mL去离子水中,得到浓度为10mg/L的敌草隆溶液,随后称取5mg的Sr0.7Ba0.3Bi2B2O7分散于5mL配置好的敌草隆溶液,避光,涡旋震荡混合均匀。随后,使用氙灯(HSX-F300,1.0W/cm2)和超声发生器(WED-100,1.0MHz,2.0W/cm2)共同照射样品10~60min,在不同的时间点(0、10、20、30、40、50、60min)离心样品取2mL上清液置于石英比色皿中通过紫外可见分光光度计(UV-2450,日本岛津公司)检测200~400nm范围内吸光度的变化。敌草隆的特征吸收峰为248nm,其降解情况如图4(a)所示,随着光和超声照射时间的增加,敌草隆于248nm处的特征吸收峰逐渐降低,表明水中的敌草隆在逐渐降解。
对比例1
准确称取5mg的Sr0.7Ba0.3Bi2B2O7分散于5mL配置好的敌草隆溶液(10mg/L),涡旋振荡混合均匀,避光保存,在不同时间点(0、10、20、30、40、50、60min)离心取上清液2mL置于石英比色皿中检测在248nm处的吸光度变化。本对比例的降解情况如图4(b)所示,本对比例对应的吸收谱图在不同时间点未发生明显变化,在248nm处的吸光度基本未变,表明催化剂在未加光和超声照射的情况下,不能产生活性氧物质催化降解敌草隆。
对比例2
准确称取5mg的Sr0.7Ba0.3Bi2B2O7分散于5mL配置好的敌草隆溶液,避光、涡旋震荡混合均匀后,仅使用超声发生器(WED-100,1.0MHz,2.0W/cm2)照射样品,在不同的时间点(0、10、20、30、40、50、60min)离心样品,取2mL上清液用于紫外-可见吸收光谱的测定,其结果如图5(a)所示,敌草隆在248nm处的吸光度逐渐降低,表明在超声处理下,Sr0.7Ba0.3Bi2B2O7可以作为声敏剂有效产生活性氧物质催化降解敌草隆。
对比例3
取5mg的Sr0.7Ba0.3Bi2B2O7分散于5mL配置好的敌草隆溶液,避光、涡旋震荡混合均匀后,仅使用氙灯(1.0W/cm2)照射样品,在不同的时间点(0、10、20、30、40、50、60min)离心样品,取2mL上清液用紫外-可见分光光度计测定敌草隆的降解情况。该对比例的结果如图5(b)所示,敌草隆在248nm处的吸光度缓慢降低,这可能是因为Sr0.7Ba0.3Bi2B2O7较大的能隙(2.7eV),氙灯在紫外蓝光区域的强度较弱,照射材料后产生较少的电子空穴对和活性氧物质,有望采用特定波长的激光或提高整体照射功率来提高催化效率。
检测数据分析:根据如下公式将上述所得的吸收谱图转化为敌草隆的降解率:降解率(%)=100×(初始吸光度-不同时间点检测吸光度)÷初始吸光度。具体结果如图6所示,在光或超声照射下,均可以降解敌草隆,且光和超声共同照射下敌草隆降解的更快更多,而单一激发源照射下,超声处理比氙灯照射降解更快,可能由于材料能隙较大(2.7eV),且氙灯光谱分布较广,在蓝光紫外区域强度较弱,激发材料产生的活性氧物质较少,可以选用能量更汇聚的激光或提高氙灯照射功率来优化降解条件。
综上所述,本发明提供了一种光/声催化剂Sr0.7Ba0.3Bi2B2O7协同光/超声催化降解敌草隆的方法,其中,Sr0.7Ba0.3Bi2B2O7既可同时作为光敏和声敏材料,在光或超声照射下均可以产生活性氧物质降解敌草隆,且二者同时照射情况下降解更快。
由于光/超声催化效率与催化剂浓度、照射源的波段、功率等密切相关,熟悉本领域的技术人员可以容易地对这些实施例和对比例做出各种修改,并把在此说明的一般性原理应用到其他实施例中。因此,本发明不限于上述实施例和对比例,本领域技术人员根据本发明的揭示,不脱离本发明范畴的改进和修改都应该在本发明的保护范围之内。
Claims (10)
1.一种光/声催化剂协同光/超声催化降解敌草隆的方法,其特征在于,在含有敌草隆的废水中,加入光/声催化剂Sr0.7Ba0.3Bi2B2O7后,同时进行光源照射和超声辐射,完成敌草隆降解。
2.根据权利要求1所述的一种光/声催化剂协同光/超声催化降解敌草隆的方法,其特征在于,所述的光/声催化剂Sr0.7Ba0.3Bi2B2O7的制备方法为先将一定比例的碳酸锶、碳酸钡、氧化铋以及硼酸研磨混合均匀,再将混合物倒入坩埚中煅烧,冷却至室温后,再次研磨即得到粉末状光/声催化剂Sr0.7Ba0.3Bi2B2O7。
3.根据权利要求2所述的一种光/声催化剂协同光/超声催化降解敌草隆的方法,其特征在于,所述的碳酸锶、碳酸钡、氧化铋以及硼酸的摩尔比为0.7:0.3:1:2。
4.根据权利要求2所述的一种光/声催化剂协同光/超声催化降解敌草隆的方法,其特征在于,所述的碳酸锶、碳酸钡、氧化铋以及硼酸的研磨混合时间为30-45min。
5.根据权利要求2所述的一种光/声催化剂协同光/超声催化降解敌草隆的方法,其特征在于,所述的煅烧的升温程序为以6℃/min的升温速率升温至500℃煅烧2h,再以相同的升温速率继续升温至660℃煅烧6h;所述的煅烧在空气气氛下进行。
6.根据权利要求2所述的一种光/声催化剂协同光/超声催化降解敌草隆的方法,其特征在于,所述的混合物煅烧冷却后的研磨时间为20-40min。
7.根据权利要求1所述的一种光/声催化剂协同光/超声催化降解敌草隆的方法,其特征在于,所述的光源包括氙灯;所述的氙灯的光照功率为0.8-1.2W/cm2。
8.根据权利要求1所述的一种光/声催化剂协同光/超声催化降解敌草隆的方法,其特征在于,所述的超声辐射的超声源包括超声仪或超声发生器;所述的超声辐射的超声频率为0.5-1.0MHz,声强为1.5-2.0W/cm2。
9.根据权利要求1所述的一种光/声催化剂协同光/超声催化降解敌草隆的方法,其特征在于,所述的光源照射和超声辐射的时间为10~60min。
10.根据权利要求1所述的一种光/声催化剂协同光/超声催化降解敌草隆的方法,其特征在于,当废水中敌草隆浓度为10mg/L时,所使用的光/声催化剂Sr0.7Ba0.3Bi2B2O7的用量为0.5-1.0mg/mL。
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