CN116371393A - 一种高效杀菌降解有机污染物的方法 - Google Patents
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Abstract
本发明涉及光催化材料技术领域，具体涉及一种高效杀菌降解有机污染物的方法，包括：获得光催化介孔材料；获得石墨烯包覆的光催化介孔复合材料；使用石墨烯包覆的光催化介孔复合材料和次氯酸盐处理水体，所述石墨烯包覆的光催化介孔复合材料在自然光照下生成电子空穴，电子空穴激发吸附于石墨烯包覆的光催化介孔复合材料上的ClO‑产生ClO自由基，ClO自由基在石墨烯包覆的光催化介孔复合材料上形成限域反应以增强其氧化能力，通过石墨烯包覆的光催化介孔复合材料光催化成产生的电子空穴和羟基自由基协同ClO自由基，能够实现高效、快速、长期和稳定的杀菌并降解有机污染物。
Description
技术领域
本发明涉及光催化材料技术领域，具体涉及一种协高效杀菌降解有机污染物的方法。
背景技术
作为一种高效的杀毒剂和氧化剂，次氯酸及次氯酸盐类自20世纪八十年代起至今在国内广泛用于水处理、医疗卫生、食品加工等领域。与传统消毒剂相比，次氯酸及次氯酸盐类在消毒过程中效率更高，产生的副产物更少，并且价格低廉。其中，次氯酸钠是废水处理和饮用水消毒中最常用的试剂。由于其极强的氧化性，除了具有强效的杀菌效果，次氯酸钠被认为可以有效去除水环境中的各类难降解有机污染物。已有大量文献报道次氯酸钠可以与多种有机污染物特别是酚类化合物发生反应。次氯酸钠降解各类有机物的具体路径由具体有机物的化学结构与性质决定。通常在氯化处理废水的过程中，次氯酸钠投加量为1-4mg/L，最短接触时间为15min。
对于水体中有机物，特别是对于难降解有机污染物高效、迅速处理的方法一直是值得研究的方向。但是，直接使用次氯酸及次氯酸盐类进行难降解有机污染物的处理，还是存在处理效率低，有机污染物清除效果不理想的问题。中国专利CN114477418A公开了一种零价铁强化次氯酸盐去除水中有机污染物的方法，通过零价铁与次氯酸盐发生的多相微界面区域内的氧化还原反应，体系中产生多种类高赋存量的活性氧化物种，使水中污染物的去除效率增加。但是采用上述操作手段存在材料不能再生、有机污染物清除效率仍然不能满足应用需求的问题。亟需对新型的利用次氯酸及次氯酸盐类清除难降解有机污染物的手段进行探索，为更有效地治理有机污染以及节约处理成本创造条件。
发明内容
本发明意在提供一种高效杀菌降解有机污染物的方法，以解决现有技术中使用次氯酸及次氯酸盐类进行难降解有机污染物处理时效率不理想的技术问题。
为达到上述目的，本发明采用如下技术方案：
一种高效杀菌降解有机污染物的方法，包括以下步骤：
S1：将介孔材料与光催化材料进行搅拌研磨复合，获得光催化介孔材料；
S2：将所述光催化介孔材料与石墨烯搅拌研磨复合，获得石墨烯包覆的光催化介孔复合材料；
S3：使用石墨烯包覆的光催化介孔复合材料和次氯酸盐处理水体，所述石墨烯包覆的光催化介孔复合材料在自然光照下生成电子空穴，电子空穴激发吸附于石墨烯包覆的光催化介孔复合材料上的ClO-产生ClO自由基，ClO自由基在石墨烯包覆的光催化介孔复合材料上形成限域反应以增强其氧化能力，通过石墨烯包覆的光催化介孔复合材料光催化成产生的电子空穴和羟基自由基协同ClO自由基实现高效杀菌降解有机污染物；其中，生成ClO自由基的反应过程可以包括：
ClO-@光催化介孔复合材料+电子空穴→ClO自由基；
杀菌及降解有机物包括：
ClO自由基+光催化介孔复合材料+细菌/有机物→CO2+H2O+Cl-/ClO-。
所述ClO-@光催化介孔复合材料是指ClO-附着在石墨烯包覆的光催化介孔复合材料上。这里，需要说明的是上述列举的反应过程是示意性过程，并不是实际的化学反应公式。
本技术方案的原理以及有益效果在于：
光催化技术是一种高效、经济和省时的杀菌以及去除有机污染物的方法，因其在处理过程中不产生二次污染物而在各种高级氧化工艺技术中脱颖而出，被认为是降解工业废水的重要技术。本技术方案首次利用介孔光催化技术生成次氯酸自由基，进一步通过吸附和限域反应加强次氯酸盐氧化降解有机物，进一步提升了次氯酸及次氯酸盐类在清除水体有机物污染的效果。并且本方案制备的石墨烯包覆的光催化介孔复合材料可回收再利用，大大节约了成本，为更有效地治理有机污染以及节约处理成本创造条件。针对现有水处理技术中还未见联合光催化介孔材料和次氯酸盐构成双催化体系，也未见利用光催化电子空穴生成次氯酸自由基以加强次氯酸盐降解有机物能力的报道。
更具体地，本技术方案结合石墨烯包覆的光催化介孔复合材料和次氯酸及次氯酸盐类进行水体有机物清除的原理以及过程为：石墨烯包覆的光催化介孔复合材料在光照射下(自然光照环境)，生成电子空穴对，会激发次氯酸根产生ClO自由基，ClO自由基在墨烯包覆的光催化介孔复合材料上形成限域反应，会进一步增强ClO自由基的氧化能力，协同介孔复合材料的光催化过程中产生的空穴对以及羟基自由基，能够加快细菌及有机物的氧化过程，实现高效、快速、长期和稳定的杀菌及降解有机污染物。通过石墨烯包覆的光催化介孔复合材料和次氯酸及次氯酸盐类的协同，在清除水体有机物及杀菌上产生了协同增效的效果。
与现有技术相比，本发明提供的一种高效杀菌降解有机污染物的方法，利用介孔材料上进行的光催化及限域反应进一步加强次氯酸盐的强氧化性，由此结合了介孔光催化技术与次氯酸盐处理污水的工艺，可得到超快速降解水体有机物的效果。
进一步，所述介孔材料与光催化材料的质量比为1:(0.1～0.8)，优选地，介孔材料与光催化材料的质量比可以为1:0.6。所述光催化介孔材料与石墨烯的质量比为1:(0.01-2)，优选地，光催化介孔材料与石墨烯的质量比为1:1.6。
采用上述技术方案，介孔材料与光催化材料的质量比设置为1:(0.1～0.8)，在确保光催化材料有好的催化效率的同时有较好的利用率，光催化材料的用量需在上述范围内，若量太少，催化效率低；若量太多，会在介孔材料中堆积，利用效率低。
石墨烯能够进一步为光催化材料提供结合位点，能够进一步加大光催化材料使用量的同时确保有好的分散性以提高光催化材料的利用效率。本申请质量石墨烯的加入，配合介孔光催化材料，协同在可见光照条件下即可触发产生具有强氧化活性的次氯酸根自由基。石墨烯能够加大比表面积形成限域反应，从而利用多孔光催化技术对次氯酸盐的氧化性能进一步加强。
进一步，次氯酸盐在水体中的质量百分比浓度为0.1～20％；石墨烯包覆的光催化介孔复合材料在水体中的质量百分比浓度为0.001～1％。
随着石墨烯包覆的光催化介孔复合材料与次氯酸盐使用量的增加，其褪色时间没有大幅度的缩短，结合使用成本考虑，石墨烯包覆的光催化介孔复合材料的质量百分浓度在1％以下(0.001～1％)，次氯酸盐的质量百分浓度在20％以下(0.1～20％)。
进一步，所述介孔材料的比表面积≥150m2/g，孔径为0.1～10nm，孔容≥0.1cm3/g，所述介孔材料具有表面亲水性，接触角≤30°。
进一步，所述在S1和S2中，搅拌研磨复合为物理搅拌研磨复合；物理搅拌研磨复合的方法为：使用球磨、砂磨或气流磨，通过高速剪切的方式进行至少两种原料的混合。
通过物理搅拌研磨复合，多孔材料与光催化材料、石墨烯通过物理吸附与静电力吸附的方式进行复合。
进一步，使用球磨进行物理搅拌研磨复合，球磨转速为100～1500r/min，球磨时间为2～4h。
转速和球磨时间能够影响光催化材料、石墨烯以及介孔材料的结合性能。在本申请的转速和球磨时间下，能够使光催化材料更好均匀的分散；石墨烯能够更高的包覆在介孔材料的表面，石墨烯更好的包覆也能增加光催化材料的结合位点。
进一步，所述介孔材料包括介孔氧化硅、介孔碳、介孔硅、炭黑、凹凸棒、膨润土、硅藻土、三维石墨烯、金属有机物框架材料、共价有机框架材料、二维的金属碳化物和氮化物中的至少一种。
进一步，所述光催化材料包括氧化钛、氧化锌、氧化钨、氮化碳、卤素银系光催化材料、磷酸银、三氧化二铟、钛酸锶、钒酸铋、硫化锌、硫化铜和氧化亚铜中的至少一种。
进一步，所述光催化材料的粒径为1-10nm。
光催化材料的粒径为1-10nm，会使禁带变宽，从而使电子-空穴对具有更强的氧化-还原能力，催化活性将随尺寸量子化程度的提高而增加。尺寸的量子化也使半导体获得更大的电荷迁移速率，空穴与电子复合的几率大大减小，也有利于提高光催化反应的效率。
进一步，所述光催化介孔材料的比表面积≥50m2/g,孔径为0.1-3nm,孔容≥0.1cm3/g,光吸收波段为200-1200nm。
进一步，所述S3中还可以施加电压以进行电催化，加快降解速度。电催化的电流密度可以为0.1A/cm2～0.4A/cm2，例如，电流密度可以为0.15A/cm2、0.2A/cm2、0.25A/cm2或者0.3A/cm2。
附图说明
图1为本方案的石墨烯包覆的光催化介孔复合材料的工作原理示意图。
图2为实验例的原始茶叶水和褪色后的茶叶水的典型图片。
具体实施方式
下面结合实施例对本发明做进一步详细的说明，但本发明的实施方式不限于此。若未特别指明，下述实施例以及实验例所用的技术手段为本领域技术人员所熟知的常规手段，且所用的材料、试剂等，均可从商业途径得到。
实施例1
本方案制备的一种降解水体有机物的原理如图1所示。图1中的石墨烯/光催化介孔复合材料即为石墨烯包覆的光催化介孔复合材料。石墨烯包覆的光催化介孔复合材料由如下方法制备而成：
本实施例具体使用的介孔材料为介孔碳，比表面积为200m2/g，孔径为1nm，孔容为0.5cm/g，接触角为10°；使用的光催化材料为ZnO，粒径为5nm(要求为纳米级别，优选范围为1-10nm)；本技术方案可以使用任意型号的石墨烯，在本实施例中具体使用的石墨烯规格为GHP-20(青岛岩海谈碳材料有限公司，粉末状，粒径18μm，片径厚度1-15nm)。
质量比具体如下：ZnO：介孔材料＝0.2:1；ZnO-介孔材料：石墨烯＝1:1。
先将ZnO和介孔材料以规定比例加入球磨机，以800r/min的转速进行物理搅拌研磨3h，制得ZnO-介孔材料。然后，将ZnO-介孔材料和石墨烯以规定比例加入球磨机，以1000r/min的转速进行物理搅拌研磨3h，制得石墨烯包覆的光催化介孔复合材料。
获得的石墨烯包覆的光催化介孔复合材料的比表面积为700m2/g,孔容≥0.8cm3/g,光吸收波段为200-1200nm。
将上述获得的石墨烯包覆的光催化介孔复合材料与次氯酸钠加入茶叶水中，然后，置于自然光下，记录其褪色时间。其中，石墨烯包覆的光催化介孔复合材料在水体中的质量百分浓度0.1％，次氯酸钠在水体中的质量百分浓度为1％，茶叶水的浓度为100mg/mL(酚类物质，图2左)，完全褪色的茶叶水呈无色透明状(图2右)。本实验例使用茶叶水模拟含有机物的污水，在实际应用时，对水体进行有机物处理，可以将次氯酸盐在水体中的质量百分比浓度维持在0.1～20％，将石墨烯包覆的光催化介孔复合材料在水体中的质量百分比浓度维持在0.001～1％。
对比例1
与实施例1获得的石墨烯包覆的光催化介孔复合材料相同。将获得的石墨烯包覆的光催化介孔复合材料加入浓度为100mg/ml的茶叶水，其中，石墨烯包覆的光催化介孔复合材料在水体中的质量百分浓度0.1％。
表1：实施例1与对比例1降解有机物的效果数据
从表1中的实施例1可以看出，通过石墨烯包覆的光催化介孔复合材料与次氯酸钠的协同作用，可以快速降解有机物。对比例1没有使用次氯酸钠，褪色时间是使用次氯酸钠的1000多倍，这说明石墨烯包覆的光催化介孔复合材料和次氯酸盐共同使用，在有机物清除上具有协同增效的效果。
实施例2
相比于实施例1而言，其ZnO与介孔材料的质量比为0.4:1，其他不变。
实施例3
相比于实施例1而言，其ZnO与介孔材料的质量比为0.6:1，其他不变。
实施例4
相比于实施例1而言，其ZnO与介孔材料的质量比为0.8:1，其他不变。
表2：实施例1～4降解有机物的效果数据
对比实施例1～实施例4可以看出，随着ZnO光催化材料含量的增加，有助于提升降解速度，但ZnO含量占比达到ZnO-介孔材料质量的80％后，降解速度反而有所下降，降解所需时间有所增加。因此，优选地，ZnO等光催化材料与介孔材料的质量比为0.6:1，此时的有机物的降解效率最高。
实施例5
本实施例基本同实施例1，不同点在于ZnO-介孔材料与石墨烯的质量比，详见表3。
实施例6
本实施例基本同实施例1，不同点在于ZnO-介孔材料与石墨烯的质量比，详见表3。
实施例7
本实施例基本同实施例1，不同点在于ZnO-介孔材料与石墨烯的质量比，详见表3。
实施例8
本实施例基本同实施例1，不同点在于ZnO-介孔材料与石墨烯的质量比，详见表3。
表3：实施例1、5-8的参数设置以及有机物降解效果数据
对比是实施例1、实施例5-8可以看出，随着石墨烯含量的提高，有利于有机物的降解。当ZnO-介孔材料与石墨烯的质量比在1:1.6时，此时的有机物降解效率最高，因此，优选地，ZnO-介孔材料与石墨烯的质量比为1:1.6；此后，随着石墨烯含量的继续增加，降解效率不再增加，降解时间开始变长。
发明人也尝试将实施例1-8中的石墨烯包覆的光催化介孔复合材料用于实际有机废水(污水)的处理中，发现：实施例3与实施例1、2、4的石墨烯包覆的光催化介孔复合材料的作用效果差异更加明显(相对于处理对象是茶水)；实施例7与实施例1、5、6、8的石墨烯包覆的光催化介孔复合材料的作用效果差异更加明显(相对于处理对象是茶水)。实施例3和实施例7的材料对于复杂成分的污水(相对于成分相对单一的茶水)的作用效果更为显著和优异。这说明，采用如下的参数设置：“ZnO等光催化材料与介孔材料质量比为0.6:1”，“ZnO-介孔材料与石墨烯质量比为1:1.6”，可保证复合材料具有理想的实际应用价值。
对比例2
本对比例基本同实施例1，不同点在于，在制备石墨烯包覆的光催化介孔复合材料时，两次球磨得转速和时间为2000r/min和5h。使用本方案的石墨烯包覆的光催化介孔复合材料和次氯酸钠进行水体有机物清除实验，物料的用量参见实施例1，测得平均褪色时间为7s(n＝10)。本对比例的产品在有机物清楚效率上比较不理想，发明人分析原因在于：由于球磨时间过长，转速过大，较为严重地影响了光催化材料、石墨烯以及介孔材料的结合性能。所以将球磨时间和转速控制在本方案规定的范围内(100～1500r/min、2～4h)，是保证石墨烯包覆的光催化介孔复合材料和次氯酸钠产生协同增效作用的较为关键的技术参数。
以上所述的仅是本发明的实施例，方案中公知的具体技术方案和/或特性等常识在此未作过多描述。应当指出，对于本领域的技术人员来说，在不脱离本发明技术方案的前提下，还可以作出若干变形和改进，这些也应该视为本发明的保护范围，这些都不会影响本发明实施的效果和专利的实用性。本申请要求的保护范围应当以其权利要求的内容为准，说明书中的具体实施方式等记载可以用于解释权利要求的内容。
Claims (10)
1.一种高效杀菌降解有机污染物的方法，其特征在于，包括以下步骤：
S1：将介孔材料与光催化材料进行搅拌研磨复合，获得光催化介孔材料；
S2：将所述光催化介孔材料与石墨烯搅拌研磨复合，获得石墨烯包覆的光催化介孔复合材料；
S3：使用石墨烯包覆的光催化介孔复合材料和次氯酸盐处理水体，所述石墨烯包覆的光催化介孔复合材料在自然光照下生成电子空穴，电子空穴激发吸附于石墨烯包覆的光催化介孔复合材料上的ClO-产生ClO自由基，ClO自由基在石墨烯包覆的光催化介孔复合材料上形成限域反应以增强其氧化能力，通过石墨烯包覆的光催化介孔复合材料光催化协同ClO自由基以实现高效杀菌降解有机污染物，反应过程包括：
ClO-@光催化介孔复合材料+电子空穴→ClO自由基；
ClO自由基+光催化介孔复合材料+细菌/有机物→CO2+H2O+Cl-/ClO-。
2.根据权利要求1所述的一种高效杀菌降解有机污染物的方法，其特征在于，所述介孔材料与光催化材料的质量比为1:(0.1～0.8)；所述光催化介孔材料与石墨烯的质量比为1:(0.01～2)。
3.根据权利要求1或2所述的一种高效杀菌降解有机污染物的方法，其特征在于，次氯酸盐在水体中的质量百分比浓度为0.1～20％；石墨烯包覆的光催化介孔复合材料在水体中的质量百分比浓度为0.001～1％。
4.根据权利要求1或2所述的一种高效杀菌降解有机污染物的方法，其特征在于，所述介孔材料的比表面积≥150m2/g，孔径为0.1～10nm，孔容≥0.1cm3/g，所述介孔材料具有表面亲水性，接触角≤30°。
5.根据权利要求1或2所述的一种高效杀菌降解有机污染物的方法，其特征在于，所述在S1和S2中，搅拌研磨复合为物理搅拌研磨复合；物理搅拌研磨复合的方法为：使用球磨、砂磨或气流磨，通过高速剪切的方式进行至少两种原料的混合。
6.根据权利要求5所述的一种高效杀菌降解有机污染物的方法，其特征在于，使用球磨进行物理搅拌研磨复合，球磨转速为100～1500r/min，球磨时间为2～4h。
7.根据权利要求1、2或6所述的一种高效杀菌降解有机污染物的方法，其特征在于，所述介孔材料包括介孔氧化硅、介孔碳、介孔硅、炭黑、凹凸棒、膨润土、硅藻土、三维石墨烯、金属有机物框架材料、共价有机框架材料、二维的金属碳化物和氮化物中的至少一种。
8.根据权利要求1、2或6所述的一种高效杀菌降解有机污染物的方法，其特征在于，所述光催化材料包括氧化钛、氧化锌、氧化钨、氮化碳、卤素银系光催化材料、磷酸银、三氧化二铟、钛酸锶、钒酸铋、硫化锌、硫化铜和氧化亚铜中的至少一种。
9.根据权利要求8所述的一种高效杀菌降解有机污染物的方法，其特征在于，所述光催化材料的粒径为1-10nm。
10.根据权利要求1、2或6所述的一种高效杀菌降解有机污染物的方法，其特征在于，所述光催化介孔材料的比表面积≥50m2/g,孔径为0.1-3nm,孔容≥0.1cm3/g,光吸收波段为200-1200nm。
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