CN112354554A - 一种MgAl-LDH/N-(BiO)2CO3复合材料的制备方法 - Google Patents
一种MgAl-LDH/N-(BiO)2CO3复合材料的制备方法 Download PDFInfo
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Abstract
本发明公开了一种MgAl‑LDH/N‑(BiO)2CO3复合材料的制备方法，包括下述步骤：首先将柠檬酸铋铵水热处理后，之后加入硝酸镁和硝酸铝，氢氧化钠得到MgAl‑LDH/N‑(BiO)2CO3复合材料。所述方法成本低、操作简单、高效节能，得到的复合材料应用于光催化降解染料污水中的污染物。
Description
技术领域
本发明应用于光催化降解染料污水中的污染物，具体涉及一种MgAl-LDH/N-(BiO)2CO3复合材料的制备方法。
背景技术
随着社会的快速发展，环境问题日益突出，特别是水污染问题。近年来，我国各类印染废水排放量不断在增加，导致水体有机物浓度相应增加。这些污染物很难降解，直接排放到江河湖泊中势必会污染水体，进入食物链后将会对环境和人体健康造成重大危害。而且传统的纺织产业在加工过程中，一些化学物质会通过挥发过程进入空气中，这些物质再通过呼吸和皮肤渗透进入动物体内。一些自由态的或者吸附在悬浮固体表面的重金属离子是致癌的，因此，印染废水的处理是非常重要的。近年来，光催化作用被广泛应用到各研究领域中，将光催化应用于染料污水处理成为了目前的研究热点。近年来，铋系氧化物由于其高的化学稳定性和较好的光催化活性已被证明是一种有发展前景的光催化剂，其中新型半导体材料Bi2O2CO3因其高偶极、间接带隙的独特特性，高氧化还原电位，电子空穴低重组率，容易形成氧空位，化学性质稳定等优点，被作为光催化材料广泛应用。但是Bi2O2CO3半导体光响应范围窄，量子效率低，带隙较宽，降低了对太阳光的利用率，影响了其在光催化领域的进一步应用。通过过渡金属、非金属的负载或掺杂以及与半导体材料复合可以提升Bi2O2CO3的光催化性能。LDHs具有较高的正电荷密度以及较大的阴离子交换容量，且层板金属离子以及层间阴离子具有较好的可调控性，因此LDHs作为吸附剂在污水处理领域有着较大的应用范围和开发潜力，MgAl-LDH是其中的代表。采用MgAl-LDH修饰单一半导体材料，对设计和制备拥有优异光催化性能的新型催化剂具有巨大的开发价值。
发明内容
本发明的目的在于提供一种MgAl-LDH/N-(BiO)2CO3复合材料的制备方法，所述的MgAl-LDH/N-(BiO)2CO3复合材料包括以下原料：柠檬酸铋铵、硝酸镁、硝酸铝，其制备方法有以下步骤：
(1)将柠檬酸铋铵加入去离子水中，超声30min，之后转移至聚四氟乙烯反应釜中，水热处理，之后用去离子水洗涤干燥；
(2)将步骤(1)产物加入50ml去离子水中，之后加入硝酸镁和硝酸铝，将混合溶液置于25℃水浴磁力搅拌器中剧烈搅拌，同时缓慢滴加2mol/L的NaOH溶液直至混合溶液pH值，并用蒸馏水洗涤3次，80℃条件下干燥24h，得到MgAl-LDH/N-(BiO)2CO3复合材料。
优选的，所述步骤(1)中，柠檬酸铋铵和去离子水的质量体积比为1g：(30-50)ml。
优选的，所述步骤(1)中，水热反应温度为160-200℃，反应时间为16-32h。
优选的，所述步骤(2)中，步骤(1)产物与硝酸镁和硝酸铝的质量比为1g：(2-4)g：(1-2)g。
优选的，所述步骤(2)中，光照时间为20-40min。
与现有技术相比，本发明具有的有益效果如下：
本发明提供了一种MgAl-LDH/N-(BiO)2CO3复合材料的制备方法，所述工艺非常简单，得到的MgAl-LDH/N-(BiO)2CO3复合材料具有优异的光催化性能，MgAl/(BiO)2CO3形成异质结结构，减小了带隙宽度，从而提高了光吸收范围，进而提高了光催化能力，提升了材料的光催化性能。通过N元素的掺杂，改变电子结构以及材料的能带结构提高了光催化性能，本发明制备的MgAl-LDH/N-(BiO)2CO3复合材料成本低、处理方法简单，能有效净化染料污水中的污染物。
本发明原料简单，易于获取，并且对环境友好。
附图说明
图1为本发明实施例1制备的MgAl-LDH/N-(BiO)2CO3复合材料的扫描电子显微镜(SEM)图。
图2为本发明实施例1制备的MgAl-LDH/N-(BiO)2CO3复合材料的透射电子显微镜(TEM)图。
具体实施方案
实施例1：
一种MgAl-LDH/N-(BiO)2CO3复合材料，具体包括以下制备步骤：
(1)将1.6g柠檬酸铋铵加入70ml去离子水中，超声30min，之后转移至聚四氟乙烯反应釜中，在180℃下水热反应24h，之后用去离子水洗涤干燥；
(2)将1g步骤(1)产物加入50ml去离子水中，之后加入3g硝酸镁和1.5g硝酸铝，将混合溶液置于25℃水浴磁力搅拌器中剧烈搅拌，同时缓慢滴加2mol/L的NaOH溶液直至混合溶液pH至10，并用蒸馏水洗涤3次,80℃条件下干燥24h,得到MgAl-LDH/N-(BiO)2CO3复合材料。
实施例2：
一种MgAl-LDH/N-(BiO)2CO3复合材料，具体包括以下制备步骤：
(1)将1.6g柠檬酸铋铵加入48ml去离子水中，超声30min，之后转移至聚四氟乙烯反应釜中，在160℃下水热反应16h，之后用去离子水洗涤干燥；
(2))将1g步骤(1)产物加入50ml去离子水中，之后加入2g硝酸镁和1g硝酸铝，将混合溶液置于25℃水浴磁力搅拌器中剧烈搅拌，同时缓慢滴加2mol/L的NaOH溶液直至混合溶液pH至10.5，并用蒸馏水洗涤3次,80℃条件下干燥24h,得到MgAl-LDH/N-(BiO)2CO3复合材料。
实施例3：
一种MgAl-LDH/N-(BiO)2CO3复合材料，具体包括以下制备步骤：
(1)将1.6g柠檬酸铋铵加入80ml去离子水中，超声30min，之后转移至聚四氟乙烯反应釜中，在200℃下水热反应36h，之后用去离子水洗涤干燥；
(2))将1g步骤(1)产物加入50ml去离子水中，之后加入4g硝酸镁和2g硝酸铝，将混合溶液置于25℃水浴磁力搅拌器中剧烈搅拌，同时缓慢滴加2mol/L的NaOH溶液直至混合溶液pH至10.2，并用蒸馏水洗涤3次,80℃条件下干燥24h,得到MgAl-LDH/N-(BiO)2CO3复合材料。
实施例4：
一种MgAl-LDH/N-(BiO)2CO3复合材料，具体包括以下制备步骤：
(1)将1.6g柠檬酸铋铵加入80ml去离子水中，超声30min，之后转移至聚四氟乙烯反应釜中，在200℃下水热反应36h，之后用去离子水洗涤干燥；
(2))将1g步骤(1)产物加入50ml去离子水中，之后加入3g硝酸镁和1.5g硝酸铝，将混合溶液置于25℃水浴磁力搅拌器中剧烈搅拌，同时缓慢滴加2mol/L的NaOH溶液直至混合溶液pH至10.5，并用蒸馏水洗涤3次,80℃条件下干燥24h,得到MgAl-LDH/N-(BiO)2CO3复合材料。
对比例1：
将3g硝酸镁和1.5g硝酸铝，将混合溶液置于25℃水浴磁力搅拌器中剧烈搅拌，同时缓慢滴加2mol/L的NaOH溶液直至混合溶液pH至10，并用蒸馏水洗涤3次，80℃条件下干燥24h,得到MgAl-LDH材料。
对比例2：
将1.6g柠檬酸铋铵加入80ml去离子水中，超声30min，之后转移至聚四氟乙烯反应釜中，在200℃下水热反应36h，之后用去离子水洗涤干燥。
分别取20mg实施例1-4和对比例1-2所制备的催化剂分散于100ml浓度为10mg/L的次甲基蓝，10mg/L甲基橙和10mg/L刚果红溶液中,在黑暗环境中剧烈搅拌30min以促使吸附平衡，之后整个装置置于250W的高压汞灯下照射90min，并通过滤光片滤掉紫外光获得可见光，每隔15min取5ml样品，离心分离催化剂与溶液,用紫外分光光度计测量溶液吸光度，由此计算去除率。
利用紫外分光光度计测量污染物的浓度，首先以去离子水作为参照，配置不同浓度的标准溶液，利用紫外分光光度计测定溶液浓度，将浓度-吸光度标准曲线在最佳波长下绘制备用，在接下来的实验过程中，吸附后的污染物浓度由吸光度标准曲线计算得出，如果遇到超出最大测试浓度的污染物溶液，则需要通过稀释到最大值以下再进行测量，尽量减小测量误差。
表1实施例与对比例对有机污染物处理结果
从实施例1-4对污水中次甲基蓝、刚果红以及甲基橙的去除率可以看出，实施例1-4制备的MgAl-LDH/N-(BiO)2CO3复合材料在加入90min后能去除溶液中90％以上的污染物，说明其具有非常优异的去除水中污染物的能力，说明了本发明所制备材料可用于污水处理，并且工作效率高，能很好的起到绿色治理污水的目的。从实施例1-4和对比例1-2对污水中不同污染物的去除率可以看出，相比MgAl-LDH材料和N-(BiO)2CO3材料，利用本发明制作的MgAl-LDH/N-(BiO)2CO3复合材料的性能要优异的多，证明了该复合材料的优越性。
Claims (6)
1.一种MgAl-LDH/N-(BiO)2CO3复合材料的制备方法，其特征在于，所述复合材料的制备方法包括以下步骤：
(1)将柠檬酸铋铵加入去离子水中，超声30min，之后转移至聚四氟乙烯反应釜中，水热处理，之后用去离子水洗涤干燥；
(2)将步骤(1)产物加入50ml去离子水中，之后加入硝酸镁和硝酸铝，将混合溶液置于25℃水浴磁力搅拌器中剧烈搅拌，同时缓慢滴加2mol/L的NaOH溶液调节混合溶液pH值，继续晶化，收集沉淀物,并用蒸馏水洗涤3次，至溶液呈中性，80℃条件下干燥24h,得到MgAl-LDH/N-(BiO)2CO3复合材料。
2.如权利要求1所述的一种MgAl-LDH/N-(BiO)2CO3复合材料的制备方法，其特征在于，所述步骤(1)中，柠檬酸铋铵和去离子水的质量体积比为1g：(30-50)ml。
3.如权利要求1所述的一种MgAl-LDH/N-(BiO)2CO3复合材料的制备方法，其特征在于，所述步骤(1)中，水热反应温度为160-200℃，反应时间为16-32h。
4.如权利要求1所述的一种MgAl-LDH/N-(BiO)2CO3复合材料的制备方法，其特征在于，所述步骤(2)中，步骤(1)产物与硝酸镁和硝酸铝的质量比为1g：(2-4)g：(1-2)g。
5.如权利要求1所述的一种MgAl-LDH/N-(BiO)2CO3复合材料的制备方法，其特征在于，所述步骤(2)中，调节pH至10-10.5。
6.如权利要求1-5任一项所述的一种MgAl-LDH/N-(BiO)2CO3复合材料的制备方法，其特征在于，所述复合材料的制备方法制备的复合材料应用于光催化降解染料污水中的污染物。
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