CN106179521A - 一种负载复合光催化剂的磁性凹凸棒粘土的制备方法 - Google Patents
一种负载复合光催化剂的磁性凹凸棒粘土的制备方法 Download PDFInfo
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Abstract
本发明公开了一种负载复合光催化剂的磁性凹凸棒粘土的制备方法,步骤:(a)将凹凸棒粘土粉体与水混合,搅拌干燥,得到提纯凹凸棒粘土;(b)加入到盐酸溶液,用纯水冲洗,加入硝酸银,加热烘干、过筛,得到酸改性凹凸棒土;(c)加入到FeCl3溶液中浸泡,超声分散;加入FeCl3溶液,超声分散,滴加氨水,超声、离心,洗涤至中性,得到磁性凹凸棒土;(d)加入到无水乙醇溶液,超声清洗,再加入六水硝酸锌和六水三氯化铁,充分搅拌,滴加NaOH,调节pH值;再离心、洗涤、干燥,再与十六烷基三甲基溴化铵、蒸馏水、无水乙醇混合,用蒸馏水和无水乙醇交替离心洗涤、抽滤,干燥,制得负载复合光催化剂的磁性凹凸棒黏土。它具有很强的吸附性能和载体性能。
Description
技术领域
本发明涉及一种负载复合光催化剂的磁性凹凸棒粘土的制备方法,属于污水处理技术领域。
背景技术
近年来,关于凹凸棒土作为吸附剂处理工业废水的研究己有报道。凹凸棒土是一种具有优异的吸附性能和一定的离子交换能力的含水富镇硅酸盐粘土矿物。活化后的凹凸棒土对重金属离子有很好的吸附净化作用,具有处理效率高,吸附成本低等特点。
在凹凸棒粘土作为吸附剂应用于水体去除重金属污染中,一般对凹凸棒粘土进行酸活化、碱活化、盐活化和热活化等。这种方法的去除机理一般是静电吸附、离子交换等作用。虽然有一定的效果,但是在去除重金属过程中,容易受到Na+ , Ca2 +等阳离子的竞争吸附影响。对于凹凸棒粘土有机改性研究,主要集中在应用一些偶联剂或者一些阳离子表面活性剂进行改性,将有机基团嫁接在凹凸棒土的表面,进而增强其疏水性,形成对重金属离子和有机污染物的吸附活性中心,提高对有机污染物和重金属的吸附去除,而且能够尽可能的忽略掉离子间的竞争吸附。
纳米ZnO是一种性能优良的光催化剂,可以有效地降解水中的有害有机物如有机氯化物、活性剂、农药、色素等,纳米级粒子的反应速度是普通粒子的100-1000倍,并且与普通粒子相比,它基本不会引起光的散射,它的比表面积很大并且能带也很宽,所以它被认为是极具应用前景的光催化剂之一。纳米化六方晶系纤锌矿结构的ZnO颗粒,其在光、电、敏感等领域表现出不凡的纳米效应和对有机污染物的高光催化降解活性,使其在处理有机污染方面具有潜在的应用经济价值。但是,用于光催化剂的纳米ZnO存在回收困难的问题,这些光催化剂在水溶液中会分散存在,因此在回收以及再利用上存在着不利之处。而凹凸棒粘土是一种多孔型链层状含水富镁铝硅酸盐类粘土矿物,近年来,关于凹凸棒土作为吸附剂处理工业废水的研究己有报道,凹凸棒黏土具有很强的吸附性能和载体性能,还具有发达的孔道,较大的比表面积,改性后的凹凸棒土对重金属离子有很好的吸附净化作用,且价格低廉,吸附成本低等特点。
发明内容
本发明的目的是为了解决现有技术中存在的缺陷,提供一种负载复合光催化剂的磁性凹凸棒粘土的制备方法,该方法制备的磁性凹凸棒粘土能在降解难的印染废水实现磁控分离,达到循环再利用。
为了达到上述目的,本发明提供了一种负载复合光催化剂的磁性凹凸棒粘土的制备方法,包括以下步骤:
(a)提纯凹凸棒粘土:
首先,将凹凸棒粘土粉碎过筛,得到颗粒大小为100目的凹凸棒粘土粉体,将凹凸棒粘土粉体与水以重量比为1:(8~ 10)的比例混合,以转速度为200~300 r/min搅拌2 h,搅拌后再过滤、干燥,得到提纯后的凹凸棒粘土;
(b)制备酸改性凹凸棒粘土
将上述的提纯后的凹凸棒粘土加入到浓度为5%的盐酸溶液中,以转速度为250~300r/min进行搅拌酸化改性2~3 h;搅拌后再用纯水冲洗至pH值为中性,再加入硝酸银,直至沉淀消失;然后加热至105~110 ℃下烘干,过200目筛,得到酸改性后的凹凸棒土粉末保存于干燥箱中备用;
(c)制备磁改性凹凸棒粘土
取1.0g酸改性凹凸棒土加入到50mL的浓度为0.15 ~0.2mol L-1FeCl3溶液中浸泡,超声分散3h,得到超声后的第一分散溶液a;再加入50mL的浓度为0.4~0.45mol L-1FeCl3溶液,继续超声分散2 h,递滴加浓度8mol L-1的氨水溶液至pH值为10.5~11.5,继续超声1~2h,得到超声后的第二分散溶液b; 再进行离心,离心后的沉淀物用蒸馏水溶液洗涤至pH值为中性,离心后进行干燥,得到磁性凹凸棒土,保存于干燥箱中备用;
(d)制备负载复合光催化剂的凹凸棒粘土的负载光催化剂
继步骤(c)之后,取上述步骤(a)得到的提纯后的凹凸棒粘土3g加入到50mL无水乙醇溶液中,使其充分均匀混合,采用超声波清洗机超声清洗15min,静置10~12 h,再加入浓度为6mmol L-1的六水硝酸锌Zn(N03)2·6H20和浓度为4mmol的六水三氯化铁(FeCl3·6H2O), 充分搅拌,向混合溶液中滴加浓度为0.10 mol L-1的NaOH,调节pH值为7~8,搅拌15min;再将混合液在3500r/min转速下进行离心,然后洗涤、干燥,再与0.lg的十六烷基三甲基溴化铵、30mL的蒸馏水、15mL的无水乙醇混合,混合后放入水热反应釜中,加热180~200℃,水热反应24h,反应后用蒸馏水和无水乙醇交替离心洗涤、减压抽滤,再加热至350℃下干燥2h,经研磨、过200目筛,制得负载复合光催化剂的磁性凹凸棒黏土。
本发明与现有技术相比具有以下优点:该方法制备的载复合光催化剂的磁性的凹凸棒黏土是负载两种存在互补的复合光催化剂,具有很强的吸附性能和载体性能,在降解难的印染废水实现磁控分离,实现循环再利用。
具体实施方式
下面,结合具体实例对本发明进一步说明。
实施例
本发明一种负载复合光催化剂的磁性凹凸棒粘土的制备方法,其特征在于具体如下的过程和步骤:
(a)提纯凹凸棒粘土:
首先,将凹凸棒粘土粉碎过筛,得到颗粒大小为100目的凹凸棒粘土粉体,将凹凸棒粘土粉体与水以重量比为1: 10的比例混合,以转速度为200~300 r/min搅拌2 h,搅拌后再过滤、干燥,得到提纯后的凹凸棒粘土;
(b)制备酸改性凹凸棒粘土
将上述的提纯后的凹凸棒粘土加入到浓度为5%的盐酸溶液中,以转速度为250~300r/min进行搅拌酸化改性3 h;搅拌后再用纯水冲洗至pH值为中性,再加入硝酸银,直至沉淀消失;然后加热至110℃下烘干,过200目筛,得到酸改性后的凹凸棒土粉末保存于干燥箱中备用;
(c)制备磁改性凹凸棒粘土
取1.0g酸改性凹凸棒土加入到50mL的浓度为0.15~0.2mol L-1FeCl3溶液中浸泡,超声分散3h,得到超声后的第一分散溶液a;再加入50mL的浓度为0.4~0.45mol L-1FeCl3溶液,继续超声分散2h,递滴加浓度8mol L-1的氨水溶液至pH值为10.5~11.5,继续超声1~2h,得到超声后的第二分散溶液b; 再进行离心,离心后的沉淀物用蒸馏水溶液洗涤至pH值为中性,离心后进行干燥,得到磁性凹凸棒土,保存于干燥箱中备用;
(d)制备负载复合光催化剂的凹凸棒粘土的负载光催化剂
继步骤(c)之后,取上述步骤(a)得到的提纯后的凹凸棒粘土3g加入到50mL无水乙醇溶液中,使其充分均匀混合,采用超声波清洗机超声清洗15min,静置10~12h,再加入浓度为6mmol L-1的六水硝酸锌Zn(N03)2·6H20和浓度为4mmol的六水三氯化铁(FeCl3·6H2O), 充分搅拌,向混合溶液中滴加浓度为 0.10 mol L-1的NaOH,调节pH值为7~8,搅拌15min;再将混合液在3500r/min转速下进行离心,然后洗涤、干燥,再与0.lg的十六烷基三甲基溴化铵、30mL的蒸馏水、15mL的无水乙醇混合,混合后放入水热反应釜中,加热到180~ 200℃,水热反应24h,反应后用蒸馏水和无水乙醇交替离心洗涤、减压抽滤,再加热至350℃下干燥2h,经研磨、过200目筛,制得负载复合光催化剂的磁性凹凸棒黏土。
为了验证本发明制备的负载复合光催化剂的磁性凹凸棒黏土在印染废水的脱色降解效果,分别进行如下测试:
测试例1
将100mg负载复合光催化剂的磁性凹凸棒黏土加入到50mL浓度为100mg/L的模拟印染废水的甲基橙溶液中,温度调节为25℃,在模拟自然光的照射5h,并采用150 r/min的振荡器震荡,测得甲基橙的脱色率为74.2%,且磁控回收洗脱后进行重复利用,其具有较好的再生利用性能。
测试例2
将100mg负载复合光催化剂的磁性凹凸棒黏土加入到50mL印染废水(从印染厂提取)的尾水中,温度调节为25℃,在模拟自然光的照射5h,并采用150 r/min的振荡器不断震荡,测得甲基橙的脱色率为71.8%,且磁控回收洗脱后进行重复利用,其具有较好的再生利用性能。
Claims (1)
1.一种负载复合光催化剂的磁性凹凸棒粘土的制备方法,其特征在于,该方法包括以下步骤:
(a). 提纯凹凸棒粘土:首先,将凹凸棒粘土粉碎过筛,得到颗粒大小为100目的凹凸棒粘土粉体,将凹凸棒粘土粉体与水以重量比为1:(8~ 10)的比例混合,以转速度为200~300 r/min搅拌2 h,搅拌后再过滤、干燥,得到提纯后的凹凸棒粘土;
(b). 制备酸改性凹凸棒粘土: 将上述的提纯后的凹凸棒粘土加入到浓度为5%的盐酸溶液中,以转速度为250~300 r/min进行搅拌酸化改性2~3 h;搅拌后再用纯水冲洗至pH值为中性,再加入硝酸银,直至沉淀消失;然后加热至105~110 ℃下烘干,过200目筛,得到酸改性后的凹凸棒土粉末保存于干燥箱中备用;
(c). 制备磁改性凹凸棒粘土: 取1.0g酸改性凹凸棒土加入到50mL的浓度为0.15 ~0.2mol L-1FeCl3溶液中浸泡,超声分散3h,得到超声后的第一分散溶液a;再加入50mL的浓度为0.4~0.45mol L-1FeCl3溶液,继续超声分散2 h,递滴加浓度8mol L-1的氨水溶液至pH值为10.5~11.5,继续超声1~2 h,得到超声后的第二分散溶液b; 再进行离心,离心后的沉淀物用蒸馏水溶液洗涤至pH值为中性,离心后进行干燥,得到磁性凹凸棒土,保存于干燥箱中备用;
(d). 制备负载复合光催化剂的凹凸棒粘土的负载光催化剂: 继步骤(c)之后,取上述步骤(a)得到的提纯后的凹凸棒粘土3g加入到50mL无水乙醇溶液中,使其充分均匀混合,采用超声波清洗机超声清洗15min,静置10~12 h,再加入浓度为6mmol L-1的六水硝酸锌Zn(N03)2·6H20和浓度为4mmol的六水三氯化铁(FeCl3·6H2O), 充分搅拌,向混合溶液中滴加浓度为0.10 mol L-1的NaOH,调节pH值为7~8,搅拌15min;再将混合液在3500r/min转速下进行离心,然后洗涤、干燥,再与0.lg的十六烷基三甲基溴化铵、30mL的蒸馏水、15mL的无水乙醇混合,混合后放入水热反应釜中,加热180~200℃,水热反应24h,反应后用蒸馏水和无水乙醇交替离心洗涤、减压抽滤,再加热至350℃下干燥2h,经研磨、过200目筛,制得负载复合光催化剂的磁性凹凸棒黏土。
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