CN110813228A - 一种铁锰复合除铬材料及其制备方法 - Google Patents
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Abstract
本发明涉及一种铁锰复合除铬材料及其制备方法，属于环境材料技术领域。本发明在加热和还原气体氛围的调控下，将铁、锰矿物按照一定的比例混合均匀，制备出高吸附量的铁锰复合材料能够固化水体以及土壤中的重金属铬Cr(VI)，具有吸附容量高、pH适应范围广、稳定性强、具有较强的氧化还原活性、绿色环保且长时间内有强效持久的固化作用等特点。该新型除铬材料制备方法简单、绿色经济，在含Cr(VI)废水的净化处理以及Cr(VI)污染土壤的修复方面具有广阔的应用前景。
Description
技术领域
本发明属于环境功能材料领域，特别涉及一种铁锰复合除铬材料及其制备方法。
背景技术
铬(Cr)广泛应用于纺织印染、制革、电镀业、木材防腐等工业过程中。由于铬的溶解性、持久性和生物富集性，在地下水、地表水和土壤中经常检测到铬。Cr在环境中有多种氧化态，其中最常见和稳定的形式是Cr(III)和Cr(VI)种，两者表现出截然不同的性质。例如，包括HCrO4和Cr2O7 2-在内的Cr(VI)是可溶性的，在水中高度流动，Cr(VI)是毒性最大的重金属之一，可引起呕吐、肺充血、肝损伤和呼吸系统疾病。相比之下，Cr(III)在自然水生环境中毒性要小得多，这是由于Cr(OH)3或CrxFe1-x(OH)3等不溶性物种的形成所致。因此，Cr(VI)被美国环境保护署(USEPA)确定为最优先的危险污染物，其在中国地表水和废水中的强制排放限值分别为0.05和0.5 mg/L。因此，如何有效地从水环境中去除Cr(VI)是一个巨大的挑战。
目前从水中去除Cr (VI)的常用方法有吸附法、沉淀法、离子交换法、还原法、电解法和络合法。然而，这些方法也有一些缺点；事实上，它们的发展受到复杂过程和高成本的阻碍。因此，有必要寻找一种廉价、简便、有效的去除废水中铬(VI)的方法。
本发明在加热和还原气体氛围的调控下，将铁、锰矿物按照一定的比例混合均匀，制备出高吸附量的铁锰复合材料能够选择性吸附去除水中的重金属铬Cr(VI),具有吸附容量高、pH适应范围广、稳定性强、具有较强的氧化还原活性、绿色环保且长时间内有强效持久的固化作用等优良特性。该新型除铬材料制备方法简单、绿色经济，在含Cr(VI)废水的净化处理以及Cr(VI)污染土壤的修复方面具有广阔的应用前景。
发明内容
为解决上述问题，本发明的目的在于提供一种吸附容量高、pH适应范围广、稳定性强、具有较强的氧化还原活性的铁锰复合除铬材料及其制备方法。
为达到上述目的，本发明提供以下的技术方案：
一种铁锰复合除铬材料及其制备方法，所制备的复合材料包括高温热还原的黄铁矿和菱锰矿。
一种铁锰复合除铬材料及其制备方法，包括以下步骤：
（1）分别将天然黄铁矿与菱锰矿进行初步破碎，破碎粒径为0.5~1 cm，再分别将矿物研磨成细粉状，过325目筛，再将黄铁矿与菱锰矿按一定质量比（1-3）:（1-3）研磨混匀，得到铁锰矿物复合体；
（2）将铁锰矿物复合体置于以氢气为还原气氛，氩气为保护气的氛围中500℃焙烧1-2h，控制气体流速为100-450 mL/min，升温速率为10-50 ℃/min。自然降温过程，收集焙烧后的粉末，进行称重；
（3）将制备的的固体材料置于厌氧环境中研磨成细粉，即获得铁锰复合除铬材料。
由于采用上述方案，本发明的有益效果是：
1.本发明产品制备原料为纯天然黄铁矿和菱锰矿，价格低廉，制备方法简单可行，生产周期短，易实现工业化生产；
2.本发明制得的铁锰复合除铬材料，具有吸附容量高、pH适应范围广、稳定性强、具有较强的氧化还原活性、绿色环保且长时间内有强效持久的固化作用等优良特性能够对重金属Cr(VI)污染的土壤和水体起到很显著地修复效果，且该材料具有磁性，容易回收再利用。
附图说明
图1是本发明实施例1中复合材料质比1:1的除铬反应前后的扫描电镜图及能谱分析图谱；
图2是本发明实施例1和实施例2中不同初始浓度对复合材料质量配比1:1和1:2吸附容量的影响；
图3是本发明实施例1和实施例2不同初始浓度对下复合材料质量配比1:1和1:2的去除率；
图4是不同pH下复合材料质量配比为2:1的Cr(VI)固化去除效果，显示了复合材料的高pH适应范围。
具体实施方式
以下将结合说明书附图和具体实施例对本发明进一步说明，而不是对本发明的限定。
实施例1
本发明的铁锰复合除铬材料处理水体中的重金属离子Cr(VI),包括以下步骤：
分别将天然黄铁矿与菱锰矿进行初步破碎，破碎粒径为0.5 cm，再分别将矿物研磨成细粉状，过325目筛，再将黄铁矿与菱锰矿按质量比1:1研磨混匀，得到铁锰矿物复合体；将铁锰矿物复合体置于以氢气为还原气氛，氩气为保护气的氛围中500℃焙烧2h，控制气体流速为150 mL/min，升温速率为20℃/min。自然降温，收集焙烧后的粉末状复合材料，即获得铁锰复合除铬材料。取0.05g该复合材料，分别置于初始浓度为30/80/150/250/350/450/550 mg/L总体系为20mL含Cr(VI)水溶液中，调节pH为6，反应24h后，用DPCI法测得溶液剩余Cr（VI）浓度，并计算最终的去除百分比，结果显示去除率分别为100%、100%、87.3%、59.8%、53.28%、45.61%、42.14%。
实施例2
本发明的铁锰复合除铬材料处理水体中的重金属离子Cr(VI),包括以下步骤：
分别将天然黄铁矿与菱锰矿进行初步破碎，破碎粒径为0.5cm，再分别将矿物研磨成细粉状，过325目筛，再将黄铁矿与菱锰矿按质量比1:2研磨混匀，得到铁锰矿物复合体；将铁锰矿物复合体置于以氢气为还原气氛，氩气为保护气的氛围中500℃焙烧2h，控制气体流速为150 mL/min，升温速率为20℃/min。自然降温过程，收集焙烧后的粉末状复合材料，即获得铁锰复合除铬材料。取0.05g该复合材料，分别置于初始浓度为30/80/150/250/350/450/550 mg/L总体系为20mL含Cr(VI)水溶液中，调节pH为6，反应24h后，用DPCI法测得溶液剩余Cr（VI）浓度，并计算最终的去除百分比，结果显示去除率分别为100%、100%、84.03%、59.59%、49.86%、44.56%、39.49%。
实施例3
本发明的铁锰复合除铬材料处理土壤中的重金属离子Cr(VI),包括以下步骤：
分别将天然黄铁矿与菱锰矿进行初步破碎，破碎粒径为0.5 cm，再分别将矿物研磨成细粉状，过325目筛，再将黄铁矿与菱锰矿按质量比1:1研磨混匀，得到铁锰矿物复合体；将铁锰矿物复合体置于以氢气为还原气氛，氩气为保护气的氛围中500℃焙烧2h，控制气体流速为150 mL/min，升温速率为20℃/min。自然降温过程，收集焙烧后的粉末状复合材料，获得的铁锰复合除铬材料。2.5g/kg的浓度均匀加入150mg/kg的Cr（VI）污染的土壤样品中，并将土壤保持一定的湿度，分别反应24小时后测土壤中浸出液中Cr（VI）的含量，并计算Cr（VI）的去除率。结果显示去除率在百分之87%以上，
实施例4
本发明的铁锰复合除铬材料处理土壤中的重金属离子Cr(VI),包括以下步骤：
分别将天然黄铁矿与菱锰矿进行初步破碎，破碎粒径为0.5 cm，再分别将矿物研磨成细粉状，过325目筛，再将黄铁矿与菱锰矿按质量比1:1研磨混匀，得到铁锰矿物复合体；将铁锰矿物复合体置于以氢气为还原气氛，氩气为保护气的氛围中500℃焙烧2h，控制气体流速为150 mL/min，升温速率为20℃/min。自然降温过程，收集焙烧后的粉末状复合材料，获得的铁锰复合除铬材料。2.5g/kg的浓度均匀加入300mg/kg的Cr（VI）污染的土壤样品中，并将土壤保持一定的湿度，分别反应24小时后测土壤中浸出液中Cr（VI）的含量，并计算Cr（VI）的去除率。结果显示去除率在百分之70%以上。
以上仅是本发明的优选实施方式，本发明的保护范围并不仅局限于上述实施例，与本发明构思无实质性差异的各种工艺方案均在本发明的保护范围。
Claims (5)
1.一种铁锰复合除铬材料及其制备方法，其特征在于在加热和还原气体氛围的调控下，将铁、锰矿物按照一定的比例混合，制备出高氧化还原活性的铁锰复合材料。
2.按照权利要求1所述的一种铁锰复合除铬材料及其制备方法，其特征在于将所制备的高氧化还原活性的铁锰复合材料作为除铬材料。
3.根据权利要求1所述的一种铁锰复合除铬材料及其制备方法，其特征在于，所述的铁、锰矿物分别为天然黄铁矿和菱锰矿，均研磨成细粉并且过325目。
4.根据权利要求1所述的一种铁锰复合除铬材料及其制备方法，其特征在于制备方法为：
将铁矿与锰矿按质量比（1-3）:（1-3）混合均匀，至于还原气体为还原氛围和惰性气体为保护气的氛围，下高温焙烧1-2小时；自然冷却至室温，即可获得铁锰复合材料，厌氧氛围下保存。
5.根据权利要求1所述的一种铁锰复合除铬材料及其制备方法，其特征在于，步骤（1）所述，焙烧过程中以H2提供还原性气氛，Ar作为保护气制造严格厌氧环境，气体流速分别控制在150-450mL/min，焙烧温度为500℃，升温速率控制在10-50℃/min。
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