CN106582599A - 用于还原处理废水中Cr(VI)的碳气凝胶材料及其制备方法 - Google Patents
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Abstract
本发明公开了一种用于还原处理废水中Cr(VI)的碳气凝胶材料及其制备方法,属于光催化材料的合成技术领域。本发明的技术方案要点为:首先采用改进的Hummers’法以石墨粉为原料制备氧化石墨烯,再将制备的氧化石墨烯配制成质量浓度为2‑10mg/mL的氧化石墨烯水溶液,调节氧化石墨烯水溶液的pH值为2‑13,然后置于微波炉中在400‑800W功率加热条件下还原,经透析处理后冷冻干燥得到宏观整体块状碳气凝胶材料。本发明提供了一种能够在自然太阳光照射下高效还原含铬废水中Cr(VI)的宏观整体块状碳气凝胶材料,该碳气凝胶材料能够通过简单的工艺制得,并且能够通过弹性形变实现其回收重复循环使用。
Description
技术领域
本发明属于光催化材料的合成技术领域,具体涉及一种用于还原处理废水中Cr(VI)的碳气凝胶材料及其制备方法。
背景技术
铬是一种具有银白色金属光泽、延展性良好、熔点高和耐腐蚀等特性的坚硬金属,常用来作装饰性镀层和防腐耐磨材料。因此,铬及其化合物在工业上应用广泛,含铬废水主要来自冶金、电镀、制革、铬盐及铬化物的生产等行业。在重金属污染种类中,铬污染排在第2位,仅次于铅。所有铬的化合物都有毒性,其中Cr(VI)毒性最大。Cr(VI)为吞入性毒物/吸入性毒物,皮肤接触可能导致敏感;更可能造成遗传性基因缺陷,吸入可能致癌,对环境有持久危险性。过量的(超过10ppm)Cr(VI)对水生物有致死作用,受污染饮用水中的Cr(VI)可致癌。鉴于此,美国环境保护局(EPA)将Cr(VI)确定为17种高度危险的毒性物质之一,我国工业废水排放标准中Cr(VI)为第一类污染物。国家《电镀污染物排放标准》GB 21900-2008对于Cr(VI)的排放标准做了更加严格的要求,规定电镀企业排放废水中总铬含量不得超过1.0mg/L,Cr(VI)含量不得超过0.2mg/L。
长期以来,含铬废水处理就是一个比较棘手的环境问题,是工业废水处理中一个重要的研究领域。含铬废水污染源复杂,污染防治技术也种类繁多。目前,国内外处理含铬废水的传统方法有化学沉淀法、吸附法、离子交换树脂法和电解法等。传统的Cr(VI)处理技术虽然可以在一定程度上去除Cr(VI),但每种方法都存在着一定的弊端。如何寻找一种经济、高效的Cr(VI)去除方法逐渐成为人们研究的热点。
光催化法是近年来在处理水中污染物方面迅速发展起来的新方法,光催化法处理含铬废水能够综合利用太阳光和人工光,无需投加还原剂就可以将Cr(VI)转化为毒性较低的Cr(III),不仅降低了成本,而且无二次污染。但是由于催化剂的流失问题,导致催化剂重复利用效率较低,目前还未能工业化应用。
发明内容
本发明解决的技术问题是提供了一种可回收利用且在自然太阳光照射下用于还原处理废水中Cr(VI)的碳气凝胶材料及其制备方法。
本发明为解决上述技术问题采用如下技术方案,用于还原处理废水中Cr(VI)的碳气凝胶材料的制备方法,其特征在于具体步骤为:首先采用改进的Hummers’法以石墨粉为原料制备氧化石墨烯,再将制备的氧化石墨烯配制成质量浓度为2-10mg/mL的氧化石墨烯水溶液,调节氧化石墨烯水溶液的pH值为2-13,然后置于微波炉中在400-800W功率加热条件下还原,经透析处理后冷冻干燥得到宏观整体块状碳气凝胶材料。
进一步优选,所述氧化石墨烯水溶液的质量浓度为6mg/mL,调节氧化石墨烯水溶液的pH值为10,微波加热功率为600W,经过自然太阳光照射8h,制得的宏观整体块状碳气凝胶材料对含铬废水中Cr(VI)的去除率为99.89%。
本发明所述的用于还原处理废水中Cr(VI)的碳气凝胶材料,其特征在于是由上述方法制备得到的,利用碳气凝胶材料的还原性在自然太阳光照射下实现含铬废水中Cr(VI)的还原,同时利用碳气凝胶材料的弹性形变实现碳气凝胶材料的回收重复循环使用。
本发明的石墨烯是从石墨材料中剥离出来、由碳原子组成的只有一层原子厚度的二维晶体。从表面化学的角度来看,石墨烯的性质类似于石墨,具有一定的还原性。碳气凝胶代表着一类新型的整体性碳质材料,不仅具有石墨烯片的固有性质,而且在各种应用方面的性能都得到了提高,其发达的孔隙、超低的密度以及优异的光学特性赋予了宏观碳气凝胶材料在工业化应用中具有极大的发展潜力,是近年来的研究热点。碳气凝胶材料可任意调节形状,弹性也很好,能够吸收光能转化为热能,从而加速废水中物质的转化速率,极好的疏水性能,内部的空隙水可以通过挤压排除,便于回收重复循环使用。如果将碳气凝胶材料用于含Cr(VI)废水的处理,有望发挥碳气凝胶材料的可塑性和还原特性等优势。
本发明提供了一种能够在自然太阳光照射下高效还原含铬废水中Cr(VI)的宏观整体块状碳气凝胶材料,该碳气凝胶材料能够通过简单的工艺制得,并且能够通过弹性形变实现其回收重复循环使用。
附图说明
图1是本发明在最优条件下制得的宏观整体块状碳气凝胶材料的拉曼光谱图;
图2是本发明在最优条件下制得的宏观整体块状碳气凝胶材料的扫描电镜图。
具体实施方式
以下通过实施例对本发明的上述内容做进一步详细说明,但不应该将此理解为本发明上述主题的范围仅限于以下的实施例,凡基于本发明上述内容实现的技术均属于本发明的范围。
实施例1
首先采用改进的Hummers’法以石墨粉为原料制备氧化石墨烯(S. Y. Dong, J. Y.Sun, Y. K. Li, C. F. Yu, Y. H. Li, J. H. Sun, ZnSnO3 hollow nanospheres/reduced graphene oxide nanocomposites as high-performance photocatalysts fordegradation of metronidazole, Appl. Catal. B Environ. 144 (2014) 386-393),再将制备的氧化石墨烯分别配制成质量浓度为2mg/mL、4mg/mL、6mg/mL、8mg/mL、10mg/mL的氧化石墨烯水溶液,调节氧化石墨烯水溶液的pH值为10,然后置于微波炉中在600W功率加热条件下还原,经透析处理后冷冻干燥得到宏观整体块状碳气凝胶材料。经过自然太阳光照射8h,该宏观整体块状碳气凝胶材料对含铬废水中Cr(VI)的去除率分别为80.5%、92.65%、99.89%、99.5%和99.62%。
实施例2
首先采用改进的Hummers’法以石墨粉为原料制备氧化石墨烯。鉴于催化剂回收问题和还原去除效率,本实施例选择质量浓度为6mg/mL的氧化石墨烯水溶液作为最佳氧化石墨烯浓度,调节氧化石墨烯水溶液的pH值分别为2、5、8、10和13,然后置于微波炉中在600W功率加热条件下还原,经透析处理后冷冻干燥得到宏观整体块状碳气凝胶材料。经过自然太阳光照射8h,该宏观整体块状碳气凝胶材料对含铬废水中Cr(VI)的去除率分别为68.95%、81.89%、92.66%、99.89%和99.97%。
实施例3
首先采用改进的Hummers’法以石墨粉为原料制备氧化石墨烯。鉴于催化剂回收问题和还原去除效率,本实施例选择质量浓度为6mg/mL的氧化石墨烯水溶液作为最佳氧化石墨烯浓度,调节氧化石墨烯水溶液的pH值为10,然后置于微波炉中分别在400W、600W和800W功率加热条件下还原,经透析处理后冷冻干燥得到宏观整体块状碳气凝胶材料。经过自然太阳光照射8h,该宏观整体块状碳气凝胶材料对含铬废水中Cr(VI)的去除率分别为78.26%、99.89%和99.09%。
图1是在最优条件下制得的宏观整体块状碳气凝胶材料的拉曼光谱图,由图可知,石墨烯的两个典型特征峰均在样品中被检测到,分别是在1360cm-1附近的D峰和1597cm-1附近的G峰。
图2是在最优条件下制得的宏观整体块状碳气凝胶材料的扫描电镜图,由图可知,制备的碳气凝胶呈多孔结构,由石墨烯片层结构堆积而成一定的骨架结构。
基于以上实施例,选取质量浓度为6mg/mL的氧化石墨烯水溶液为制备浓度,调节氧化石墨烯水溶液的pH值为10,微波加热功率为600W,在此条件下制备的宏观整体块状碳气凝胶材料的光催化性能最优。通过进一步的光催化还原实验,分别采用本条件下制备的碳气凝胶材料对质量浓度为10mg/L含Cr(VI)废水的暗态吸附和自然太阳光光催化还原实验,同时做含Cr(VI)废水的空白光解实验,经过8h反应,含铬废水中Cr(VI)的去除率分别为0.25%、99.89%和0.12%。经过5次循环降解实验,碳气凝胶材料对含铬废水中Cr(VI)的去除率未发生明显变化。相比于传统的还原Cr(VI)的光催化材料,该方法制得的碳气凝胶材料能够响应自然太阳光,具有可见光催化活性,并且便于回收重复循环利用。
以上实施例描述了本发明的基本原理、主要特征及优点,本行业的技术人员应该了解,本发明不受上述实施例的限制,上述实施例和说明书中描述的只是说明本发明的原理,在不脱离本发明原理的范围下,本发明还会有各种变化和改进,这些变化和改进均落入本发明保护的范围内。
Claims (3)
1.用于还原处理废水中Cr(VI)的碳气凝胶材料的制备方法,其特征在于具体步骤为:首先采用改进的Hummers’法以石墨粉为原料制备氧化石墨烯,再将制备的氧化石墨烯配制成质量浓度为2-10mg/mL的氧化石墨烯水溶液,调节氧化石墨烯水溶液的pH值为2-13,然后置于微波炉中在400-800W功率加热条件下还原,经透析处理后冷冻干燥得到宏观整体块状碳气凝胶材料。
2.根据权利要求1所述的用于还原处理废水中Cr(VI)的碳气凝胶材料的制备方法,其特征在于:所述氧化石墨烯水溶液的质量浓度为6mg/mL,调节氧化石墨烯水溶液的pH值为10,微波加热功率为600W,经过自然太阳光照射8h,制得的宏观整体块状碳气凝胶材料对含铬废水中Cr(VI)的去除率为99.89%。
3.一种用于还原处理废水中Cr(VI)的碳气凝胶材料,其特征在于是由权利要求1或2所述的方法制备得到的,利用碳气凝胶材料的还原性在自然太阳光照射下实现含铬废水中Cr(VI)的还原,同时利用碳气凝胶材料的弹性形变实现碳气凝胶材料的回收重复循环使用。
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