CN107694541A - 一种硝酸盐处理剂的制备及应用 - Google Patents
一种硝酸盐处理剂的制备及应用 Download PDFInfo
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Abstract
本发明公开了一种硝酸盐处理剂的制备和应用，本发明以棉花为模板，采用共沉淀法合成具有生物形态的锌钛铁三元类水滑石，经过马弗炉焙烧，得到硝酸盐处理剂。本发明还提供上述方法制备的硝酸盐处理剂在硝酸盐废水处理中的应用。该方法制得的硝酸盐处理剂对硝酸盐有良好的吸附效果，便于分离，再生方法简单易行，在硝酸盐废水处理领域具有广阔的应用前景。
Description
技术领域
本发明属于废水处理技术领域，尤其涉及一种硝酸盐处理剂的制备及应用。
背景技术
随着工农业的不断发展，农业化肥的大量使用、生活污水的排放以及工业废水的渗漏等问题，使得水中的硝酸盐污染越来越严重。过量的硝酸盐使水体中营养物质增多，促使自养型生物旺盛生长，造成水质恶化，破坏生态环境。硝酸盐化学稳定性强，不易与其他化合物结合，但其可在人体内转化成亚硝酸盐，此外，在各种含氮有机化合物的作用下，硝酸盐和亚硝酸盐会形成“三致”物质，可引发癌症、克山病和高铁血红蛋白症等疾病。因此，去除水体中硝酸盐刻不容缓。
目前针对水体中硝酸盐的去除主要有生物法、反渗透法、离子交换法、金属催化还原法等，其中，生物反硝化法反应慢，需要有机物作为电子供体，会带来二次污染；反渗透法运行费用过高,而且不具有选择性,去除硝酸盐的同时也可能去除其他对人体有益的元素；离子交换法产生的浓缩废水较难处理；催化还原法对硝酸盐的还原一般需要采用贵金属做催化剂，一方面提高了处成本，另一方面如果催化剂选择不恰当会产生亚硝酸盐和氨氮等副产物。
层状双金属氢氧化物(LDH)，又称类水滑石(HTlc)，是一类具有超分子结构、带结构正电荷的无机层状材料，由于其具有层间阴离子的可交换性、层板阳离子的可变化性、记忆效应、表面积较大、较高的热稳定性和耐酸碱性等特殊性质，在吸附，催化、电化学等领域具有广泛的应用。常规应用于水处理过程中的水滑石一般是通过焙烧-还原法(又称结构重建法)制备，先利用共沉淀法制得水滑石，然后将其焙烧得到金属氧化物，利用金属氧化物具有“结构记忆”特性，可去除水中的阴离子。利用水滑石的阳离子可搭配性,将具有氧化催化活性的金属阳离子引入水滑石的结构,就可能得到类水滑石。类水滑石的研究目前是水处理材料的研究热点。此外，由于水滑石属于二维纳米材料，粒度小，难分离，表面具有活性羟基基团，使表面结构很不稳定，相互之间极易形成氢键产生软团聚，进而通过表面羟基缩合而产生硬团聚。因此将水滑石镶嵌到有机体模板上，经焙烧过程去除模板，可以制备出仿生态材料，增强其吸附能力。
发明内容
本发明的目的是提供一种硝酸盐处理剂的制备及应用，目的在于提供一种对硝酸盐吸附性能好且易分离易再生的水处理剂。
本发明目的通过以下技术方案得以实现。
一种硝酸盐处理剂的制备方法，其特征在于所述的硝酸盐处理剂以棉花为模板，采用共沉淀法合成具有生物形态的锌钛铁三元类水滑石，经过马弗炉焙烧，得到硝酸盐处理剂，具体步骤如下：
(1)将棉花用蒸馏水和无水乙醇洗涤3次，60℃烘干备用。
(2)将硝酸锌、硫酸钛和硝酸铁按照锌、钛、铁摩尔比(1～3):(1～3):(1～3)的比例分制得混合盐溶液A，混合液总金属离子浓度控制为0.3～1mol/L。
(3)配置共沉淀剂溶液B，B中含1～5mol/L NaOH和0.1～0.5mol/L Na2CO3，B溶液体积是A溶液的1～2倍。
(4)将处理过的棉花放入烧杯中，同时加入A+B体积的蒸馏水，棉花与蒸馏水的质量比是1：60～1：250，然后将混合盐溶液A与共沉淀剂溶液B同时滴加于其中，控制滴加速度为每秒1滴，同时磁力剧烈搅拌，滴加完毕后，继续搅拌30min，超声10min，调节pH为9.5～10.5，得到悬浮液C。
(5)将上述所得的悬浮液C置于65℃鼓风干燥箱中，陈化12h，取出沉淀物，水洗至中性，放置在鼓风干燥箱中，80℃干燥12h，制得具有生物形态的锌钛铁三元类水滑石。
(6)将上述所得的锌钛铁三元类水滑石放入马弗炉中，在300℃～500℃下焙烧2～6h，得到生物遗态锌钛铁氧化物即为硝酸盐处理剂。
所述硝酸盐处理剂用于水中硝酸盐的去除，步骤如下：
(1)将质量比为0.05％～1％的硝酸盐处理剂投入硝酸盐废水中，吸附2～6小时后，通过磁分离回收硝酸盐处理剂，水中硝酸盐被去除，硝酸盐的去除率可达88％以上；
(2)将回收的吸附饱和的硝酸盐处理剂加入适量水，置于光催化反应器中，打开紫外灯，反应0.5～2小时，利用光催化还原作用将硝酸盐处理剂上吸附的硝酸盐还原为氮气，完成硝酸盐处理剂的再生，取出再生后的硝酸盐处理剂，干燥后投入硝酸盐废水中再次使用。
本发明的有益效果：
该硝酸盐处理剂是具有超分子结构、带结构正电荷的无机层状材料，由于其具有层间阴离子的可交换性、记忆效应、表面积较大、较高的热稳定性和耐酸碱性等特殊性质，对硝酸盐有很好的吸附效果，与水滑石粉体相比，该硝酸盐处理剂避免了水滑石粉体团聚结块、硝酸根离子吸附力降低的问题，
该硝酸盐处理剂中含有磁性物质——四氧化三铁，可通过磁分离快速从水中分离，克服了普通水滑石从水中难分离的缺点。
该硝酸盐处理剂中还含有二氧化钛、铁酸锌、氧化锌等成分，其中，铁酸锌可提高二氧化钛的光催化效率，氧化锌也具有光催化作用，在紫外光照射下，硝酸盐处理剂表面吸附的硝酸盐被催化还原为氮气，完成硝酸盐处理剂的再生，方法简单易行。吸附饱和的普通水滑石需要通过焙烧进行再生，操作麻烦，费用高；该硝酸盐处理剂通过常温下的紫外光催化还原就可进行再生，极大的减少了再生费用。
此外，该硝酸盐处理剂的应用采用吸附-磁分离-光催化再生工艺，避免了直接采用光催化导致反应副产物亚硝酸盐、氨氮进入水体造成二次污染的问题。
因此本发明具有绿色环保、工艺简便和易工业化等诸多优点，在水处理领域中具有广阔的应用前景。
附图说明
图1是硝酸盐处理剂的扫描电子显微镜图。
图2是硝酸盐处理剂的X射线衍射图。
具体实施方式
为便于理解，下面结合具体实施例对本发明做进一步说明。
实施例1一种硝酸盐处理剂的制备方法，具体包括以下步骤：
(1)将棉花用蒸馏水和无水乙醇洗涤3次，60℃烘干备用。
(2)称取5.94g Zn(NO3)2·6H2O，3mL Ti(SO4)2，4.04g Fe(NO3)3·9H2O于烧杯中，加入100ml蒸馏水，制得混合盐溶液A。
(3)称取12.00g NaOH和2.67g Na2CO3于烧杯中，加入150ml蒸馏水，制得共沉淀剂溶液B。
(4)将3g处理过的棉花放入烧杯中，同时加入250ml蒸馏水，然后将混合盐溶液A与共沉淀剂溶液B同时滴加于其中，控制滴加速度为每秒1滴，同时磁力剧烈搅拌，滴加完毕后，继续搅拌30min，超声10min，调节pH＝9.5～10.5，得到悬浮液C。
(5)将所得的悬浮液C置于65℃鼓风干燥箱中，陈化12h。取出沉淀物，水洗至中性，放置在鼓风干燥箱中，80℃干燥12h，制得具有生物形态的锌钛铁三元类水滑石。
(6)将所得的锌钛铁三元类水滑石放入马弗炉中，在300℃下焙烧4h，得到生物遗态锌钛铁氧化物即为硝酸盐处理剂。
图1为硝酸盐处理剂的扫描电子显微镜图，从图1可以看出，硝酸盐处理剂保持了棉花的纤维形态，避免了水滑石粉末团聚结块，比表面积大，增强了吸附性能。
图2为硝酸盐处理剂的X射线衍射图。从图2可以看出，硝酸盐处理剂中在2θ值为29.72°、31.84°、34.34°处有明显的衍射峰，经与标准图谱对比分析，衍射峰来自四氧化三铁，硝酸盐处理剂中在2θ值为62.91°、68.19°处有明显的衍射峰，经与标准图谱对比分析，衍射峰来自二氧化钛，在2θ值为47.52°、56.33°处有明显的衍射峰，经与标准图谱对比分析，衍射峰来自氧化锌，在2θ值为34.34°、36.68°、43.13°处有明显的衍射峰，经与标准图谱对比分析，衍射峰来自铁酸锌。
实施例2一种硝酸盐处理剂的制备方法，具体包括以下步骤：
(1)将棉花用蒸馏水和无水乙醇洗涤3次，60℃烘干备用。
(2)称取11.88g Zn(NO3)2·6H2O，6mL Ti(SO4)2，8.08g Fe(NO3)3·9H2O于烧杯中，加入200ml蒸馏水，制得混合盐溶液。
(3)称取24.00gNaOH和5.34gNa2CO3于烧杯中，加入300ml蒸馏水，制得共沉淀剂。
(4)将4g处理过的棉花放入烧杯中，同时加入500ml蒸馏水，然后将混合盐溶液与共沉淀剂同时滴加于其中，控制滴加速度为每秒1滴，同时磁力剧烈搅拌，滴加完毕后，继续搅拌30min，超声10min，调节pH＝9.5～10.5。
(5)将所得的悬浮液置于65℃鼓风干燥箱中，陈化12h。取出沉淀物，水洗至中性，放置在鼓风干燥箱中，80℃干燥12h，制得具有生物形态的锌钛铁三元类水滑石。
(6)将所得的锌钛铁三元类水滑石放入马弗炉中，在450℃下焙烧4h，得到生物遗态锌钛铁氧化物即为硝酸盐处理剂。
实施例3一种水中硝酸盐处理剂的应用
在250mL锥形瓶中加入0.1g硝酸盐处理剂，再加入150mL含221mg/L硝酸盐的废水，25℃恒温水浴震荡3h。磁分离后测定上清液中硝酸盐含量，计算得硝酸盐的吸附量为300.06mg/g，硝酸盐的去除率为90.34％。
将磁分离后得到的硝酸盐处理剂，加入10mL蒸馏水，放入光催化反应器中，打开紫外灯，反应0.5h后磁分离，并放入烘箱中烘干。再加入150mL含221mg/L硝酸盐的废水，25℃恒温水浴震荡3h。磁分离后测定上清液中硝酸盐含量，计算得硝酸盐的吸附量为288.88mg/g，硝酸盐的去除率为89.56％。表明该硝酸盐处理剂已成功再生。
实施例4一种水中硝酸盐处理剂的应用
在1L含600mg/L硝酸盐的实际废水中加入1g硝酸盐处理剂，搅拌，吸附2h后，通过磁分离，回收硝酸盐处理剂，出水硝酸盐的去除率可达93.25％。将回收的吸附饱和的硝酸盐处理剂加入100mL蒸馏水置于光催化反应器中，打开紫外灯，反应1h，利用紫外光催化还原作用将硝酸盐处理剂上吸附的硝酸盐还原为氮气，完成硝酸盐处理剂的再生，取出硝酸盐处理剂，干燥后再加入1L含600mg/L硝酸盐的实际废水，搅拌，吸附2h。出水硝酸盐的去除率可达92.36％。
需要说明的是：以上所述仅为本发明的优选实施例，并不用于限制本发明，尽管参照前述实施例对本发明进行了详细的说明，对于本领域的技术人员来说，其依然可以对前述实施例所记载的技术方案进行修改，或者对其中部分技术特征进行同等替换。
凡在本发明的精神和原则之内，所做的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。
Claims (2)
1.一种硝酸盐处理剂的制备方法，其特征在于以棉花为模板，采用共沉淀法合成具有生物形态的锌钛铁三元类水滑石，经过马弗炉焙烧，得到硝酸盐处理剂，具体步骤如下：
(1)将棉花用蒸馏水和无水乙醇洗涤三次，60℃烘干备用；
(2)将硝酸锌、硫酸钛和硝酸铁按照锌、钛、铁摩尔比1～3:1～3:1～3的比例制得混合盐溶液A，混合液总金属离子浓度控制为0.3～1mol/L；
(3)配置共沉淀剂溶液B，溶液B中含1～5mol/L NaOH和0.1～0.5mol/L Na2CO3，溶液B体积是溶液A体积的1～2倍；
(4)将处理过的棉花放入烧杯中，同时加入溶液A+溶液B体积的蒸馏水，棉花与蒸馏水的质量比是1：60～1：250，然后将混合盐溶液A与共沉淀剂溶液B同时滴加于其中，控制滴加速度为每秒1滴，同时磁力剧烈搅拌，滴加完毕后，继续搅拌30min，超声10min，调节pH为9.5～10.5，得到悬浮液C；
(5)将上述所得的悬浮液C置于65℃鼓风干燥箱中，陈化12h，取出沉淀物，水洗至中性，放置在鼓风干燥箱中，80℃干燥12h，制得具有生物形态的锌钛铁三元类水滑石；
(6)将上述所得的锌钛铁三元类水滑石放入马弗炉中，在300℃～500℃下焙烧2～6h，得到生物遗态锌钛铁氧化物即为硝酸盐处理剂。
2.根据权利要求1所述的硝酸盐处理剂的制备方法，其特征在于，所述硝酸盐处理剂用于水中硝酸盐的去除，具体步骤如下：
(1)将质量比为0.05％～1％的硝酸盐处理剂投入硝酸盐废水中，吸附2～6小时后，通过磁分离回收硝酸盐处理剂，水中硝酸盐被去除，硝酸盐的去除率可达88％以上；
(2)将回收的吸附饱和的硝酸盐处理剂加入适量水，置于光催化反应器中，打开紫外灯，反应0.5～2小时，利用光催化还原作用将硝酸盐处理剂上吸附的硝酸盐还原为氮气，完成硝酸盐处理剂的再生，取出再生后的硝酸盐处理剂，干燥后投入硝酸盐废水中再次使用。
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