CN108862538B - 纳米零价铁活化过碳酸钠降解双酚a的方法 - Google Patents
纳米零价铁活化过碳酸钠降解双酚a的方法 Download PDFInfo
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Abstract
本发明公开了纳米零价铁活化过碳酸钠降解双酚A的方法,制备纳米零价铁后催化活化过碳酸钠降解双酚A,反应条件温和,易于操作;采用纳米零价铁作为反应体系的催化剂活化氧化剂过碳酸钠生成·OH和O2 ·‑自由基,对双酚A进行降解,降解过程简单,降解效率高;催化剂可回收再利用,氧化剂便于储存运输、活性高且稳定。
Description
技术领域
本发明属于分析化学技术领域,具体涉及纳米零价铁活化过碳酸钠降解双酚A的方法。
背景技术
随着我国工业的快速发展,含有各种污染物的工业生产废水大量排放,对环境造成了日益严重的影响。双酚A(BPA)作为全球生产量最大的化工原料之一,同时也是一种代表性的环境内分泌干扰物。即使其浓度很低时,仍可以对生物有机体正常的生长繁殖及内分泌造成不利影响。相关技术中,采用传统Fenton试剂对双酚A进行处理,存在着大量Fe2+难以分离回收再利用、反应后产生大量铁泥处理成本高、液态H2O2不便储存运输且易分解不稳定等问题。
发明内容
有鉴于此,本发明的实施例提供了一种可循环重复利用、氧化剂便于储存运输且稳定、对环境无二次污染的纳米零价铁活化过碳酸钠降解双酚A的方法。
为解决上述技术问题,本发明实施例采用的技术方案是,纳米零价铁活化过碳酸钠降解双酚A的方法,包括以下步骤:
(1)制备纳米零价铁(nFe0);
(2)取适量的双酚A溶液、过碳酸钠溶液混合均匀,调节溶液pH值;
(3)向上述溶液中加入纳米零价铁,并进行搅拌降解水体中的双酚A;
(4)降解反应完成后回收溶液中的纳米零价铁。
优选地,所述步骤(1)中,纳米零价铁的制备包括以下步骤:
(1-1)采用除氧超纯水分别配制FeSO4·7H2O和NaBH4溶液,将NaBH4溶液逐滴加入FeSO4·7H2O溶液中,同时搅拌;
(1-2)滴加完毕后,继续机械搅拌20min-30min后分离黑色颗粒,并依次用无氧水、无水乙醇洗涤所得到的黑色颗粒,真空干燥后得到纳米零价铁。
优选地,所述步骤(2)中,温度为25±2℃,溶液pH值为4±0.1。
优选地,所述步骤(3)中,纳米零价铁的浓度为0.1g/L。
与相关技术比较,本发明的实施例提供的技术方案带来的有益效果是:本发明的纳米零价铁活化过碳酸钠降解双酚A的方法简单,反应条件温和,易于操作;采用纳米零价铁作为反应体系的催化剂活化过碳酸钠生成·OH和O2 ·-自由基,对双酚A进行降解,降解过程简单,降解效率高;催化剂可回收再利用,过碳酸钠便于储存运输、活性高且稳定。
附图说明
图1是本发明实施例纳米零价铁活化过碳酸钠降解双酚A的方法流程图;
图2是本发明实施例制备的纳米零价铁的扫描电镜图;
图3是本发明实施例制备的纳米零价铁的扫描电镜图;
图4是本发明实施例降解反应前后nFe0的X-衍射射线图;
图5是本发明实施例制备的纳米零价铁的比表面积测试图;
图6是本发明实施例不同反应体系降解双酚A的对比示意图;
图7是本发明实施例纳米零价铁/过氧化氢体系与纳米零价铁/过碳酸钠体系降解双酚A过程氧化剂利用率对比示意图;
图8是本发明实施例制备的纳米零价铁循环利用催化降解双酚A的示意图。
具体实施方式
为使本发明的目的、技术方案和优点更加清楚,下面将结合附图对本发明实施方式作进一步地描述。
请参考图1,本发明的实施例提供了纳米零价铁活化过碳酸钠降解双酚A的方法,包括以下步骤:
(1)制备纳米零价铁(nFe0);
具体地,采用除氧超纯水分别配制FeSO4·7H2O和NaBH4溶液,将NaBH4溶液逐滴加入FeSO4·7H2O溶液中,同时搅拌;NaBH4溶液滴加完毕后,继续机械搅拌后分离黑色颗粒,并依次用无氧水、无水乙醇洗涤所得到的黑色颗粒,真空干燥后得到纳米零价铁;
参照附图2、3,制备的纳米零价铁呈球形颗粒,颗粒之间团聚成链状结构;
(2)取适量的双酚A溶液、过碳酸钠(SPC)溶液在一定温度下混合均匀,调节溶液pH值;温度为25±2℃,溶液pH值为4±0.1;
(3)向上述溶液中加入纳米零价铁,同时进行搅拌降解水体中的双酚A;纳米零价铁的浓度为0.1g/L;
(4)降解反应完成后回收溶液中的纳米零价铁。反应完成后所述纳米零价铁表面生成铁氧化物。
本发明实施例的方法简单,易于操作,降解条件温和,采用nFe0催化活化过碳酸钠降解双酚A的效率高,降解反应的产物为二氧化碳和水,不会对环境造成二次污染。
实施例二
根据本发明实施例一的方法采用纳米零价铁降解双酚A,包括以下步骤:
(1)制备纳米零价铁(nFe0);所述纳米零价铁的制备过程为:
(1-1)先将超纯水煮沸20min,然后向超纯水中通入30min的高纯氮气以去除其中的氧气冷却得到无氧水,称取0.01mol的FeSO4·7H2O和0.02mol的NaBH4分别溶解于50ml的无氧水中得到FeSO4溶液和NaBH4溶液;
(1-2)将配置好的FeSO4·7H2O溶液置于装有机械搅拌的三口烧瓶中,用胶头滴管向其中缓慢均匀的滴加NaBH4溶液,滴加过程中机械搅拌,Fe2+与BH4 -离子的反应如下所示:
Fe2++2BH4 -+6H2O→nFe0+2B(OH)3+7H2;
(1-3)滴加完毕后,继续机械搅拌20~30min,然后用强力磁铁分离黑色颗粒,并依次用无氧水、无水乙醇洗涤三次所述黑色颗粒,最后将黑色颗粒放入真空干燥箱中60℃烘干得到纳米零价铁;
参照附图4、5,本发明实施例制备的nFe0为单质铁,粒径为116.8nm的球形颗粒,纯度高没有被氧化,且nFe0在44.68°和65.03°出现了明显的衍射峰,峰形尖锐,nFe0结晶度很高;nFe0属于带有H3滞后环的第IV类等温线,为单位子层吸附,材料具有发达的孔隙结构,吸附效果较好;nFe0的比表面积为77.66m2/g,孔隙直径为8.76nm;
(2)在250mL的烧瓶中加入100mL的反应溶液,其中双酚A的浓度为0.1mmol/L,过碳酸钠的浓度为3mmol/L,混合均匀;
(3)向上述溶液中加入0.01g纳米零价铁,机械搅拌30min,在固定的反应时间间隔内取样1mL,与1mL淬灭剂甲醇混合,取样时间为0min、1min、2min、3min、5min、7min、10min、20min、30min;样品经0.22μm有机滤膜过滤后,用高效液相色谱(HPLC)测定溶液中剩余双酚A的浓度;
并在相同条件下分别进行单独nFe0、单独SPC、nFe0/H2O2体系的对照降解双酚A,其中,过碳酸钠投加后的浓度为3mmol/L,nFe0的投加量为0.01g,H2O2投加后的浓度为4.5mmol/L;
参照附图6、7,当反应体系中只存在nFe0时,双酚A几乎不被降解,这说明nFe0对BPA分子吸附的作用力较弱;当反应体系中只存在过碳酸钠时,双酚A在30min内仅被降解了4%左右,表明过碳酸钠没有被活化,虽然过碳酸钠本身具有一定氧化性,但是在降解双酚A的过程中起主要氧化去除作用的是羟基自由基,所以过碳酸钠在没有被活化时,对双酚A降解效果差。
nFe0/H2O2体系对双酚A有较好的降解效果,反应7min后可以达到89%,酸性条件下nFe0会与H+缓慢反应生成Fe2+,Fe2+再与H2O2反应产生大量强氧化的·OH;但在nFe0/SPC体系中,双酚A的降解速率提升明显,这是由于过碳酸钠水溶液呈较强的碱性,存在HO2 -,而HO2 -比H2O2更容易分解产生活性氧,其次nFe0/SPC体系中SPC水解产生的H2O2能够被更好的有效利用产生·OH,而不是无效分解为H2O和O2,因此降解效率更高,7min内几乎可以完全去除水体中的双酚A。
对比两种体系,nFe0/H2O2体系中的氧化剂分解速率更快,在30min内H2O2被完全消耗掉,但降解效率低于nFe0/SPC体系中,说明nFe0/H2O2体系中的H2O2进行了更多的无效分解,产生了H2O和O2,而不是·OH;而nFe0/SPC体系中30min内H2O2也几乎被消耗完全,说明该反应体系能够有效充分利用氧化剂,具有持久稳定降解污染物能力;
(4)降解反应完成后回收溶液中的纳米零价铁。
参照附图8,本发明实施例制备的纳米零价铁材料具有良好的磁性,通过磁铁分离的方式,对反应后的催化剂进行回收后再利用;每轮催化降解反应结束后,利用磁铁对催化剂进行分离,催化剂通过多次清洗、烘干后再进行下一轮重复性实验;nFe0催化剂在循环使用过程中表现出较好的催化效果,从降解曲线的变化中也观察到经过三轮反应后催化剂的催化效率有一定下降,这可能是由于:(1)催化剂表面生成了氧化物层,阻碍了反应的进行,降低催化效果;(2)nFe0的蚀溶导致有效的活性催化位点减少。其余同实施例一。
在本文中,所涉及的前、后、上、下等方位词是以附图中零部件位于图中以及零部件相互之间的位置来定义的,只是为了表达技术方案的清楚及方便。应当理解,所述方位词的使用不应限制本申请请求保护的范围。
在不冲突的情况下,本文中上述实施例及实施例中的特征可以相互结合。
以上所述仅为本发明的较佳实施例,并不用以限制本发明,凡在本发明的精神和原则之内,所作的任何修改、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.纳米零价铁活化过碳酸钠降解双酚A的方法,其特征是,包括以下步骤:
(1)制备纳米零价铁,所述纳米零价铁的制备过程包括如下:将0.01mol的FeSO4·7H2O和0.02mol的NaBH4分别溶解于50ml的无氧水中得到FeSO4溶液和NaBH4溶液,将配置好的NaBH4溶液缓慢均匀滴加至FeSO4溶液中,过程中保持搅拌,然后分离出溶液中的黑色颗粒,黑色颗粒经洗涤、干燥后得到纳米零价铁;所述纳米零价铁的粒径为116.8nm,比表面积为77.66m2/g,孔隙直径为8.76nm;
(2)取适量的双酚A溶液和过碳酸钠溶液混合均匀,调节溶液pH值;
(3)向上述溶液中加入适量的纳米零价铁,并进行搅拌,所述纳米零价铁的浓度为0.1g/L;
(4)降解反应完成后回收溶液中的纳米零价铁。
2.根据权利要求1所述的纳米零价铁活化过碳酸钠降解双酚A的方法,其特征是,所述步骤(2)中,温度为25±2℃,溶液pH值为4±0.1。
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