CN111530420A - 一种农林废弃物多孔碳基复合吸附材料的制备方法 - Google Patents
一种农林废弃物多孔碳基复合吸附材料的制备方法 Download PDFInfo
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Abstract
一种农林废弃物多孔碳基复合吸附材料的制备方法,涉及农林废弃物处理以及含含砷废水处理技术领域,首先将铜盐、镁盐、银盐溶于水中并加入适量稀硝酸混合均匀,再加入农林废弃物多孔碳并混合均匀,然后通过超声波微波组合反应器进行反应,制备获得农林废弃物多孔碳基复合吸附材料。本发明以农林废弃物多孔碳为主要载体物质,以一定含量和组成的CuO‑MgO‑Ag2O为吸附材料的填充剂,制备的C‑CuO‑MgO‑Ag2O(7:2:1:1)改性农林废弃物多孔碳的吸附效果最好,吸附量达到282mg/g。证实这些农林废弃物多孔碳基复合吸附材料C‑CuO‑MgO‑Ag2O可以用于含砷工业生活污水废水环境治理中。
Description
技术领域
本发明涉及农林废弃物处理以及含含砷废水处理技术领域,具体是涉及一种农林废弃物多孔碳基复合吸附材料的制备方法。
背景技术
砷污染是指由砷或其化合物所引起的环境污染。砷和含砷金属的开采、冶炼,用砷或砷化合物作原料的玻璃、颜料、原药、纸张的生产以及煤的燃烧等过程,都可产生含砷废水、废气和废渣,对环境造成污染。大气含砷污染除岩石风化、火山爆发等自然原因外,主要来自工业生产及含砷农药的使用、煤的燃烧。含砷废水、农药及烟尘都会污染土壤。砷在土壤中累积并由此进入农作物组织中。砷和砷化物一般可通过水、大气和食物等途径进入人体,造成危害。元素砷的毒性极低,砷化物均有毒性,三价砷化合物比其他砷化合物毒性更强。
2004年12月15日,世界卫生组织官员公布,全球至少有5000多万人口正面临着地方性砷中毒的威胁,其中,大多数为亚洲国家,而中国正是受砷中毒危害最为严重的国家之一。土壤中的重金属污染致使许多地方的作物减产。砷在土壤中累积并由此进入农作物组织中。砷对农作物产生毒害作用最低浓度为3mg/L,对水生生物的毒性亦很大。砷和砷化物一般可通过水、大气和食物等途径进入人体,造成危害。元素砷的毒性极低,砷化物均有毒性,三价砷化合物比其他砷化合物毒性更强。砷污染中毒事件(急性砷中毒)或倒置的公害病(慢性砷中毒)已屡见不鲜。一旦出现砷污染,需要及时的治理,以防止出现更大范围的危害,以保障广大人民群众的生命健康安全。砷污染治理的方法主要有化学方法、物理方法和生物方法:
化学方法:是指用化学试剂使砷变为人体难以吸收的砷化合物,如,在含砷废水中投加石灰、硫酸亚铁和液氯(或漂白粉),将砷沉淀,然后对废渣进行处理,也可以让含砷废水通过硫化铁滤床或用硫酸铁、氯化铁氢氧化铁凝结沉淀等。
物理法:主要是让含砷污水通过特殊的过滤器,使砷富集起来变废为宝,如,活性炭过滤法等。
生物方法:主要是指在砷污染的土壤或水体中种植能吸收砷的植物,以达到吸收砷的目的,如美国科学家发现了一种蕨类植物可吸收污染土壤中的砷。
近年来,随着经济和科学技术的飞速发展,多孔碳材料是一种无污染、无害环境的吸附剂材料。大量的实验和研究表明,负载改性填充剂的多孔碳材料由于其独特的性能,比单一碳材料具有更好的吸附和催化性能,可以应用于含砷废水的处理。
多孔碳材料常见的合成方法有碳化法、物理化学活化法、催化活化法、有机凝胶碳化法、自组装法和模板法等。催化活化法金属易进入并滞留在活性炭内部,有机凝胶碳化法设备昂贵制备过程较繁琐,且有机气凝胶的前驱体使用酚、醛类等有毒性的有机物,对工作人员和环境有一定的危险性。传统模板法的模板合成过程较为繁琐、成本较为高昂等,都限制了其在工业生产的大规模应用。
发明内容
本发明要解决的技术问题是提出一种农林废弃物多孔碳基复合吸附材料的制备方法,以制备可以用于含砷废水处理的吸附材料。
为了实现上述目的,本发明所采用的技术方案为:一种农林废弃物多孔碳基复合吸附材料的制备方法,首先将铜盐、镁盐、银盐溶于水中并加入适量稀硝酸混合均匀,再加入农林废弃物多孔碳并混合均匀,然后通过超声波微波组合反应器进行反应,制备获得农林废弃物多孔碳基复合吸附材料C-CuO-MgO-Ag2O,具体步骤如下:
1)、称取硝酸铜、氧化镁、硝酸银加入烧杯中,使用蒸馏水和稀硝酸溶解,然后加入农林废弃物多孔碳,并加入氨水调节溶液的pH值至5-12,充分搅拌;
2)、将溶液置于超声波微波组合反应器中进行反应,采用超声波1000W+微波800W双功能化反应30min;
3)、反应结束后,将样品放入150℃烘箱中干燥3h,获得农林废弃物多孔碳基复合吸附材料C-CuO-MgO-Ag2O。
作为本发明的农林废弃物多孔碳基复合吸附材料的制备方法的优选技术方案,所述农林废弃物多孔碳的制备方法为:将农林废弃物经过酸洗、脱灰,并在惰性气氛中活化造孔,得到农林废弃物多孔碳材料。所述农林废弃物选自树皮、秸秆、锯末、甘蔗渣、橘皮、柚子皮、椰子壳、稻糠中的一种或多种的组合。获得农林废弃物多孔碳基复合吸附材料C-CuO-MgO-Ag2O中C、CuO、MgO和Ag2O的掺杂摩尔比为7:1~2:1~2:1~2。
本发明提供一种依据上述方法制备的农林废弃物多孔碳基复合吸附材料C-CuO-MgO-Ag2O,微观形态孔道结构明显,微结构呈现多级多尺度,尺寸范围在500nm-3um之间。
与现有技术相比,本发明的有益效果表现在:
本发明以农林废弃物多孔碳为主要载体物质,以一定含量和组成的CuO-MgO-Ag2O为吸附材料的填充剂,以最新发展的微波超声波组合法制备性能优良的多元复合吸附材料。采用仪器表征手段XRD,SEM对其结构进行表征,并对吸附性能进行了测试,筛选出性能优良的CuO-MgO-Ag2O改性农林废弃物多孔碳吸附材料。实验发现C-CuO-MgO-Ag2O(7:2:1:1)改性农林废弃物多孔碳的吸附效果最好,吸附量达到282mg/g。证实这些农林废弃物多孔碳基复合吸附材料C-CuO-MgO-Ag2O可以用于含砷工业生活污水废水环境治理中,并将富集砷用于制备GaAs,InA、等Ⅲ-V族化合物半导体材料及硅、锗单晶掺杂剂,也用于制备As2Se3(红外线透射玻璃、激光印刷机等)等领域。
附图说明
以下结合实施例和附图对本发明的农林废弃物多孔碳基复合吸附材料的制备方法作出进一步的详述。
图1是实施例1~7制备各系列复合吸附材料的XRD图。
图2依次是实施例1制备复合吸附材料的低、中、高倍率SEM图。
图3是实施例1~7制备各系列复合吸附材料的吸附残余砷离子百分比曲线图。
图4是实施例1~7制备各系列复合吸附材料的吸附量曲线图。
具体实施方式
实施例1
本实施中,制得的农林废弃物多孔碳基复合吸附材料C-CuO-MgO-Ag2O中,C、CuO、MgO和Ag2O的掺杂摩尔比为7:2:1:1。制备方法步骤如下:
1)、将树皮、秸秆、锯末、甘蔗渣、橘皮、柚子皮、椰子壳、稻糠等农林废弃物经过酸洗、脱灰,并在惰性气氛中活化造孔,得到农林废弃物多孔碳材料。
2)、称取硝酸铜、氧化镁、硝酸银加入烧杯中,使用蒸馏水和稀硝酸溶解,然后加入农林废弃物多孔碳,并加入氨水调节溶液的pH值至11,充分搅拌;
3)、将溶液置于超声波微波组合反应器中进行反应,采用超声波1000W+微波800W双功能化反应30min;
4)、反应结束后,将样品放入150℃烘箱中干燥3h,获得农林废弃物多孔碳基复合吸附材料C-CuO-MgO-Ag2O(7:2:1:1)。
实施例2
本实施例中,制得的农林废弃物多孔碳基复合吸附材料C-CuO-MgO-Ag2O中,C、CuO、MgO和Ag2O的掺杂摩尔比为7:2:2:1,制备方法同实施例1,获得农林废弃物多孔碳基复合吸附材料C-CuO-MgO-Ag2O(7:2:2:1)。
实施例3
本实施例中,制得的农林废弃物多孔碳基复合吸附材料C-CuO-MgO-Ag2O中,C、CuO、MgO和Ag2O的掺杂摩尔比为7:1:2:1,制备方法同实施例1,获得农林废弃物多孔碳基复合吸附材料C-CuO-MgO-Ag2O(7:1:2:1)。
实施例4
本实施例中,制得的农林废弃物多孔碳基复合吸附材料C-CuO-MgO-Ag2O中,C、CuO、MgO和Ag2O的掺杂摩尔比为7:1:1:2,制备方法同实施例1,获得农林废弃物多孔碳基复合吸附材料C-CuO-MgO-Ag2O(7:1:1:2)。
实施例5
本实施例中,制得的农林废弃物多孔碳基复合吸附材料C-CuO-MgO-Ag2O中,C、CuO、MgO和Ag2O的掺杂摩尔比为7:1:1:1,制备方法同实施例1,获得农林废弃物多孔碳基复合吸附材料C-CuO-MgO-Ag2O(7:1:1:1)。
实施例6
本实施例中,制得的农林废弃物多孔碳基复合吸附材料C-CuO-MgO-Ag2O中,C、CuO、MgO和Ag2O的掺杂摩尔比为7:2:1:2,制备方法同实施例1,获得农林废弃物多孔碳基复合吸附材料C-CuO-MgO-Ag2O(7:2:1:2)。
实施例7
本实施例中,制得的农林废弃物多孔碳基复合吸附材料C-CuO-MgO-Ag2O中,C、CuO、MgO和Ag2O的掺杂摩尔比为7:1:2:2,制备方法同实施例1,获得农林废弃物多孔碳基复合吸附材料C-CuO-MgO-Ag2O(7:1:2:2)。
图1是实施例1~7制备各系列复合吸附材料的XRD图。由图1可知,样品的衍射强峰与农林废弃物多孔碳基复合吸附材料C-CuO-MgO-Ag2O基本相对应。XRD衍射图有明显的MgO,CuO,Ag2O的衍射峰,而且都比较尖锐,说明合成的复合吸附剂在物相上与实验设计目标物农林废弃物多孔碳相吻合。
图2依次是实施例1制备复合吸附材料的低、中、高倍率SEM图。从图2可知,实施例1制备得到了具有片形、球形状、多面体形状的混合结构的C-CuO-MgO-Ag2O改性农林废弃物多孔碳吸附复合材料,其中孔道结构明显,微结构呈现多级多尺度,尺寸范围在500nm-3um之间。
图3为日光照条件下,不同组成的系列农林废弃物多孔碳复合吸附剂材料对含砷污水溶液去除率的影响。其中,样品C-CuO-MgO-Ag2O改性农林废弃物多孔碳吸附材料用量为50mg,吸附时间为80min,含砷污水溶液体积为150mL,初始浓度均为100mg/L。由图3可知,实施例1制备的农林废弃物多孔碳基复合吸附材料C-CuO-MgO-Ag2O(7:2:1:1)的吸附效果最好,去除率达到99.2%,且所有不同组成的系列产品在随时间的延长,吸附去除效果越好。
图4为日光照条件下,不同组成的系列农林废弃物多孔碳复合材料对含砷(三价砷和五价砷)溶液吸附量与去除时间、物质组成的曲线。其中,样品C-CuO-MgO-Ag2O农林废弃物多孔碳吸附材料用量为50mg,吸附时间为140min,含砷(三价砷和五价砷)溶液体积为500mL。由图4可知,实施例1制备的农林废弃物多孔碳基复合吸附材料C-CuO-MgO-Ag2O(7:2:1:1)的吸附效果最好,吸附量达到282mg/g,且所有不同组成的系列产品在随时间的延长,吸附去除效果越好,在吸附时间达到60分钟后,随着时间的增加,吸附量基本上达到稳定,说明吸附过程主要在60分钟内完成,而且吸附效果很好。所制备的目标产品达到了实验的设计的预期目标,证实这些微波超声波组合法制备的C-CuO-MgO-Ag2O改性农林废弃物多孔碳吸附材料可以用于含砷重金属溶液的工业污水废水环境治理中。
以上内容仅仅是对本发明的构思所作的举例和说明,所属本技术领域的技术人员对所描述的具体实施例做各种各样的修改或补充或采用类似的方式替代,只要不偏离发明的构思或者超越本权利要求书所定义的范围,均应属于本发明的保护范围。
Claims (5)
1.一种农林废弃物多孔碳基复合吸附材料的制备方法,其特征在于,首先将铜盐、镁盐、银盐溶于水中并加入适量稀硝酸混合均匀,再加入农林废弃物多孔碳并混合均匀,然后通过超声波微波组合反应器进行反应,制备获得农林废弃物多孔碳基复合吸附材料C-CuO-MgO-Ag2O,具体步骤如下:
1)、称取硝酸铜、氧化镁、硝酸银加入烧杯中,使用蒸馏水和稀硝酸溶解,然后加入农林废弃物多孔碳,并加入氨水调节溶液的pH值至5-12,充分搅拌;
2)、将溶液置于超声波微波组合反应器中进行反应,采用超声波1000W+微波800W双功能化反应30min;
3)、反应结束后,将样品放入150℃烘箱中干燥3h,获得农林废弃物多孔碳基复合吸附材料C-CuO-MgO-Ag2O。
2.如权利要求1所述的制备方法,其特征在于,所述农林废弃物多孔碳的制备方法为:将农林废弃物经过酸洗、脱灰,并在惰性气氛中活化造孔,得到农林废弃物多孔碳材料。
3.如权利要求2所述的制备方法,其特征在于,所述农林废弃物选自树皮、秸秆、锯末、甘蔗渣、橘皮、柚子皮、椰子壳、稻糠中的一种或多种的组合。
4.如权利要求1所述的制备方法,其特征在于,获得农林废弃物多孔碳基复合吸附材料C-CuO-MgO-Ag2O中C、CuO、MgO和Ag2O的掺杂摩尔比为7:1~2:1~2:1~2。
5.如权利要求1~4任一项所述方法制备的农林废弃物多孔碳基复合吸附材料C-CuO-MgO-Ag2O,其特征在于,微观形态孔道结构明显,微结构呈现多级多尺度,尺寸范围在500nm-3um之间。
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