CN103920451B - 一种锌铝水滑石空心微米球的制备方法及甲基橙系印染废水的处理方法 - Google Patents
一种锌铝水滑石空心微米球的制备方法及甲基橙系印染废水的处理方法 Download PDFInfo
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Abstract
本发明公开了一种锌铝水滑石空心微米球的制备方法及甲基橙系印染废水的处理方法,其中锌铝水滑石空心微米球的制备方法是首先配制CO(NH2)2、Zn2+和Al3+混合溶液,于90‑140℃恒温晶化12‑24h,冷却至室温后依次经过滤、去离子水洗涤、干燥得到混合物前驱体;将所述混合物前驱体于280‑360℃灼烧2‑6小时,得到锌铝复合氧化物;将所述锌铝复合氧化物加入0.01‑0.1mol/L的Na2CO3溶液中搅拌1‑5h,过滤、去离子水洗涤并于60℃干燥后得到锌铝水滑石。本发明制备的锌铝水滑石空心微米球具有良好的吸附性能,用于甲基橙模拟印染废水的吸附容量大,吸附废水浓度高,吸附后产物可再生循环利用。
Description
一、技术领域
本发明涉及一种用于甲基橙系印染废水的吸附剂的制备方法以及甲基橙系印染废水的处理方法。
二、背景技术
甲基橙系染料中含偶氮键、芳香环的复杂有机化合物,具有耐日晒、稳定性强、抗氧化性好等特点,在厌氧条件下甲基橙氮链会降解产生芳香胺类化合物,这类物质具有一定毒性和致癌性,极大威胁着人体健康。偶氮染料废水成分复杂、色度高、可生化性差而难以找到经济有效的治理方法。而吸附法以其高效低耗、工艺简单及运行可靠等优点,通常被用作单独的净化手段或作为生物净化的必要补充。在吸附法研究中,开发高效廉价的吸附剂是实现有效治理染料废水的关键。
水滑石类插层材料是一种由带正电荷的金属氢氧化物层板和带负电荷的层间阴离子构成的层状双羟基金属复合氢氧化物(LDHs),在催化、环保、生物医药等领域得到了广泛地应用。传统合成方法制备的LDHs材料团聚严重,且LDHs的形貌、粒径、比表面积难以控制,这极大地限制了LDHs材料在催化和吸附领域的应用。以零维、一维、二维纳米结构为基本组成单元,按照一定方式组装成的多级纳米结构LDHs,不仅具有纳米结构单元所具有的特殊性质,而且具有微米与亚微米尺度的结构稳定性、良好的分散性和较高的比表面积,因此成为人们近年来研究的热点。而在如何得到尺寸较小、粒径均匀、结构可调、低成本高性能的多级纳米结构LDHs方面,尚存在亟待解决的问题,例如:合成LDH材料时多用到模板或表面活性剂,合成条件苛刻等。
三、发明内容
本发明旨在提供一种锌铝水滑石空心微米球的制备方法及甲基橙系印染废水的处理方法,所要解决的技术问题是制备得到一种对印染废水吸附容量高的吸附剂,并提高其在水体中的分散性能。
本发明所称甲基橙系印染废水是指通过甲基橙对产品进行染色后产生的废水。
本发明制备工艺简单,制备过程没有用到表面活性剂,产品可回收利用,符合环保要求。
本发明锌铝水滑石空心微米球的制备方法如下:
1)配制CO(NH2)2、Zn2+和Al3+混合溶液,混合溶液中Zn2+和Al3+的摩尔量之和与CO(NH2)2的摩尔量之比为1:6-10;Zn2+和Al3+的摩尔量之比为2-4:1。将配制的混合溶液转移至聚四氟乙烯高压釜中,于90-140℃恒温晶化12-24h,冷却至室温后依次经过滤、去离子水洗涤、干燥得到混合物前驱体;
2)将所述混合物前驱体于280-360℃灼烧2-6小时,得到锌铝复合氧化物;
3)将所述锌铝复合氧化物加入0.01-0.1mol/L的Na2CO3溶液中搅拌1-5h,过滤、去离子水洗涤并于60℃干燥后得到锌铝水滑石空心微米球。
本发明制备的锌铝水滑石呈空心球状,粒径均匀,为3-5μm,分散性较好。本发明制备的锌铝水滑石空心微米球的化学式为:Zn0.71Al0.29(OH)2(CO3)0.145·xH2O,x为结晶水数量,取值范围为0.5-9。
将本发明制备的锌铝水滑石空心微米球按照20-100mg/L的比例投入含有甲基橙的模拟印染废水中,印染废水中甲基橙的浓度≤1000mg/L,用0.01mol·L-1的NaOH溶液或0.01mol·L-1的HCl溶液调节水体pH为2-12,优选pH值为3,于25-55℃温度下进行吸附处理20h,优选温度为25℃,过滤除去滤饼,滤液即为去除甲基橙后的水体。本发明锌铝水滑石空心微米球在吸附处理甲基橙后,在300-500℃温度下焙烧2-5小时后即可再生为锌铝复合氧化物,可作为吸附剂循环利用。
向待处理的甲基橙溶液中加入一定量的锌铝水滑石空心微米球,恒温搅拌,每隔一段时间取样,经离心分离,测定上清液中甲基橙浓度。
甲基橙浓度的测定采用可见分光光度法。
吸附剂对溶液中甲基橙的吸附量qe用式(1)计算:
其中,C0和Ct分别是起始和处理后甲基橙的质量浓度,V为溶液体积,m为吸附剂质量。
本发明制备的锌铝水滑石空心微米球对模拟废水中的甲基橙有很高的吸附容量。如在100mL甲基橙溶液中加入50mg锌铝水滑石、甲基橙溶液浓度500mg·L-1、控体系pH值3、温度25℃、吸附时间20h的条件下,吸附饱和吸附量可以达到735.3mg·g-1,明显优于一般的吸附材料。
本发明锌铝水滑石空心微米球的制备工艺简单,用于甲基橙模拟印染废水的吸附容量大,吸附废水浓度高,吸附后产物可再生循环利用。
四、附图说明
图1是实施例1得到的锌铝水滑石空心微米球的XRD图。图1中出现了相对衍射强度较大的(003)、(006)、(012)、(110)晶面的水滑石特征衍射峰,各衍射峰强度高,峰型尖锐对称,基线平稳,表明样品具有较好的水滑石层状结构。
图2是实施例1得到的锌铝水滑石空心微米球的FESEM图。
图3是实施例1得到的锌铝水滑石空心微米球的FETEM图。
图4是实施例1中饱和吸附量与溶液浓度的关系图。
图5是实施例2中去除率与吸附温度的关系图。
图6是实施例3中去除率与溶液初始pH值的关系图。
图7是实施例3中锌铝水滑石循环利用次数对甲基橙吸附效率的影响图。从图7中可以看出,循环使用4次后对甲基橙的去除率仍然可以达到85%。
五、具体实施方式
本发明采用日本理学Riguku D/max-γB型X射线粉末衍射仪测定样品的晶体结构;采用FEI Sirion-200型场发射扫描电子显微镜与JEM-2100F型场发射透射电子显微镜对样品的形貌和微观结构进行分析。
实施例1:
1、吸附剂的制备
1)分别称取1.20g CO(NH2)2、0.425g Zn(NO3)2·6H2O和0.214g Al(NO3)3·9H2O溶于40mL去离子水中,得到混合溶液;将配好的混合溶液转移到聚四氟乙烯高压釜中,放入烘箱,在100℃下恒温晶化24h后将反应釜取出,冷却至室温;将所得沉淀过滤,并用去离子水反复洗涤数次,然后烘干得到混合物前驱体;
2)将步骤1)制得的混合物前驱体在300℃下灼烧4h制得锌铝复合氧化物;
3)将步骤2)制得的铝复合氧化物加入到0.05mol·L-1的Na2CO3溶液中搅拌2h后过滤,去离子水洗涤3次,在60℃下干燥6h得到锌铝水滑石空心微米球。
2、吸附处理
分别取五份50mg上述锌铝水滑石空心微米球并分别加入到含甲基橙质量浓度为100mg·L-1、200mg·L-1、300mg·L-1、400mg·L-1、500mg·L-1的100mL废水中,控制pH为3,温度为25℃,振荡吸附时间为20h,振荡后离心分离,取上清液测定吸附后的溶液浓度,得到材料对甲基橙的饱和吸附量见图4。
图1是所得锌铝水滑石空心微米球的XRD图,图1中出现了相对衍射强度较大的(003)、(006)、(012)、(110)晶面的水滑石特征衍射峰,各衍射峰强度高,峰型尖锐对称,基线平稳,表明样品具有较好的水滑石层状结构。图2和图3分别是锌铝水滑石空心微米球的FESEM和FETEM图,图中显示,所述的锌铝水滑石呈空心球状,粒径均匀,约为3-5μm,分散性较好。由图4可知,废水中甲基橙浓度为500mg·L-1时,锌铝水滑石空心微米球对甲基橙的饱和吸附量高达735.3mg·g-1。
实施例2:
1、吸附剂的制备
1)分别称取1.00g CO(NH2)2、0.425g Zn(NO3)2·6H2O和0.214g Al(NO3)3·9H2O溶于40mL去离子水中,得到混合溶液;将配好的混合溶液转移到聚四氟乙烯高压釜中,放入烘箱,在100℃下恒温晶化24h后将反应釜取出,冷却至室温;将所得沉淀过滤,并用去离子水反复洗涤数次,然后烘干得到混合物前驱体;
2)将步骤1)制得的混合物前驱体在300℃下灼烧4h制得锌铝复合氧化物;
3)将步骤2)制得的铝复合氧化物加入到0.07mol·L-1的Na2CO3溶液中搅拌2h后过滤,去离子水洗涤3次,在60℃下干燥6h得到锌铝水滑石空心微米球。
2、吸附处理
分别取五份50mg上述锌铝水滑石空心微米球并分别加入到五份含甲基橙质量浓度为200mg·L-1的100mL废水中,控制pH为3,温度分别为25℃、35℃、45℃、55℃,振荡吸附时间为20h,振荡后离心分离,取上清液测定吸附后的溶液浓度,得到材料对甲基橙的去除率见图5。由图5可知在温度为25℃时去除率最大。
实施例3:
1、吸附剂的制备
1)分别称取1.00g CO(NH2)2、0.425g Zn(NO3)2·6H2O和0.178g Al(NO3)3·9H2O溶于40mL去离子水中,得到混合溶液;将配好的混合溶液转移到聚四氟乙烯高压釜中,放入烘箱,在100℃下恒温晶化24h后将反应釜取出,冷却至室温;将所得沉淀过滤,并用去离子水反复洗涤数次,然后烘干得到混合物前驱体;
2)将步骤1)制得的混合物前驱体在300℃下灼烧4h制得锌铝复合氧化物;
3)将步骤2)制得的铝复合氧化物加入到0.09mol·L-1的Na2CO3溶液中搅拌2h后过滤,去离子水洗涤3次,在60℃下干燥6h得到锌铝水滑石空心微米球。
2、吸附处理
分别取10份50mg上述锌铝水滑石空心微米球并分别加入到10份质量浓度为200mg·L-1的100mL甲基橙废水中,10份甲基橙废水的pH值分别为2、3、4、5、6、7、8、9、10、12,振荡吸附时间为20h,振荡后离心分离,取上清液测定吸附后的溶液浓度,得到材料对甲基橙的去除率见图6。由图6可知在pH值为3时去除率最大。
Claims (2)
1.一种甲基橙系印染废水的处理方法,其特征在于:
将锌铝水滑石空心微米球按照20-100mg/L的比例投入甲基橙系印染废水中,调节水体pH为2-12,于25-55℃温度下进行吸附处理18-22h,过滤除去滤饼,滤液即为去除甲基橙后的水体;
所述锌铝水滑石空心微米球是按以下步骤制备得到的:
1)配制CO(NH2)2、Zn2+和Al3+混合溶液,将混合溶液转移至聚四氟乙烯高压釜中,于90-140℃恒温晶化12-24h,冷却至室温后依次经过滤、去离子水洗涤、干燥得到混合物前驱体;混合溶液中Zn2+和Al3+的摩尔量之和与CO(NH2)2的摩尔量之比为1:6-10;Zn2+和Al3+的摩尔量之比为2-4:1;
2)将所述混合物前驱体于280-360℃灼烧2-6小时,得到锌铝复合氧化物;
3)将所述锌铝复合氧化物加入0.01-0.1mol/L的Na2CO3溶液中搅拌1-5h,过滤、去离子水洗涤并于60℃干燥后得到锌铝水滑石空心微米球。
2.根据权利要求1所述的处理方法,其特征在于:
水体pH值调节为3,吸附处理温度为25℃。
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