CN113231030A - 一种磁性蓝藻生物炭及其制备方法和应用 - Google Patents
一种磁性蓝藻生物炭及其制备方法和应用 Download PDFInfo
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Abstract
本发明公开了一种磁性蓝藻生物炭及其制备方法和应用,将蓝藻进行冷冻干燥、研磨过筛处理,得到蓝藻生物质;将Fe2O3与蓝藻生物质混合,置于烘箱中干燥处理,得到中间产物;将中间产物置于管式炉内,于惰性气氛保护下进行碳化,冷却至室温后研磨过筛,得到磁性蓝藻生物炭。本发明采用蓝藻水华作为生物炭原料,减轻了有害水华的处理处置问题,同时也一定程度降低了合成生物炭材料的成本;并且增强了催化剂性能和材料稳定性,提高了生物炭的回收利用率。
Description
技术领域
本发明涉及废水处理领域,特别是涉及一种磁性蓝藻生物炭及其制备方法和应用。
背景技术
目前,我国淡水水体富营养化日趋严重,66%以上的湖泊和水库处于富营养化水平,一些大型湖泊都先后爆发了严重的蓝藻水华,聚集在水面上散发出浓重的臭味,形成蓝绿色的浮沫,影响水生生态及人类健康。因此,蓝藻水华的资源化利用已成为亟待解决的难题。
生物炭是指在缺氧条件下将生物质通过热化学过程(比如热解、水热碳化或烘焙)得到的富含碳的产品。其制备原料来源非常广泛,如各种农林废弃物、工业及城市生活中的有机废弃物等。藻类生物质因其具有分布范围广泛、生长及成熟期快、N、P、K等无机成分和脂类物质含量高等特点,被认为是一种很有前景的制备生物炭的原料。
而现有技术中的生物炭多用于重金属或者有机物的吸附剂,而制备成催化剂降解污染物的蓝藻生物炭研究相对较少,且生物炭的回收利用情况也不乐观。
发明内容
发明目的:本发明的目的是提供一种磁性蓝藻生物炭及其制备方法和应用,以蓝藻为生物质原料制备生物炭,并获得了优异的降解效果和回收利用效率。
技术方案:本发明所述的一种磁性蓝藻生物炭的制备方法,其包括以下步骤:
(1)将蓝藻进行冷冻干燥、研磨过筛处理,得到蓝藻生物质;
(2)将Fe2O3与蓝藻生物质混合,置于烘箱中干燥处理,得到中间产物;
(3)将中间产物置于管式炉内,于惰性气氛保护下进行碳化,冷却至室温后研磨过筛,得到磁性蓝藻生物炭。
其中,步骤(1)中,将蓝藻冷冻干燥处理得到块状蓝藻生物质,将块状蓝藻生物质过60目筛;
上述步骤(2)中,Fe2O3的加入量占蓝藻生物质质量的2-10wt%;干燥处理温度为60-80℃,干燥时间为24-36h,有利于污泥完全干燥,形成较稳定的大分子颗粒。
上述步骤(3)中,碳化温度为400-800℃,碳化时间为2-4h;惰性气氛为N2、Ar或NH3等气氛;碳化的升温速率为2-10℃/min,并将冷却产物经研磨处理后过80目筛。
其中,所述惰性气氛的流速为150-200mL/min;
本发明还提供了一种上述制备方法得到的磁性蓝藻生物炭在降解废水中的应用。
优选地,所述废水为有机染料,如橙黄G溶液、亚甲基蓝或酸性橙。
发明原理:现有技术中没有研究将蓝藻生物炭用于活化过氧化氢或过硫酸盐去降解难降解有机污染物。而本发明将打捞的蓝藻藻泥进行冷冻干燥,得块状的蓝藻生物质,之后用研钵对其进行研磨,过80目筛;将所述Fe2O3与蓝藻生物质在适当比例(w/w)2-10%混合,放入60-80℃烘箱干燥,得中间产物;将上述中间产物放入管式炉,在惰性气氛N2/Ar/NH3保护下进行碳化,碳化温度为400-800℃,碳化时间为1-4h,冷却至室温后研磨过60目筛,得磁性蓝藻生物炭。
目前生物炭多采用比较繁杂的制备步骤和过程,且许多用的都是稀有的贵金属给生物炭的应用增加了时间成本和经济成本;并且所用的贵金属大多会在水体中溶出对水体有二次污染。本发明选取从太湖打捞的蓝藻为生物质原料,通过与Fe2O3混合的方式进行一次碳化后实现磁性物质负载,得到具有高效催化降解污染物的改性蓝藻生物炭,获得了协同增效的技术效果,填补了生物炭降解有机污染物的空白。同时铁离子不但能促进污染物降解,同时对环境也相对友好。
有益效果:
本发明提供了一种磁性蓝藻生物炭的制备方法,以蓝藻为生物质原料制备生物炭,解决了我国打捞的蓝藻水华难处理的问题,实现了有害蓝藻的资源化利用,通过蓝藻生物质前驱体和Fe2O3进行充分混合后,进行一次碳化,使磁性氧化铁成功负载在蓝藻生物炭上,增强蓝藻生物炭的催化性能和材料稳定性,实现了难降解有机染料的高效降解,并且提高其回收利用效率,填补了本领域的空白。
一方面,采用的蓝藻水华作为生物炭原料,减轻了有害水华的处理处置问题,同时也一定程度降低了合成生物炭材料的成本;另一方面,磁性蓝藻生物炭能够增强催化剂性能和材料稳定性,提高了生物炭的回收利用率。
附图说明
图1是磁性蓝藻生物炭制备流程示意图。
图2是磁性蓝藻生物炭降解污染物效果图。
具体实施方式
下面结合实施例对本发明进一步地详细描述。
如图1所示为磁性蓝藻生物炭制备流程图,首先将打捞的蓝藻藻泥进行冷冻干燥,得块状的蓝藻生物质。之后用研钵对其进行研磨,过筛;再将所述适当比例的Fe2O3与蓝藻生物质混合,放入烘箱干燥,得中间产物;将上述中间产物放入管式炉,在惰性气氛保护下进行碳化,冷却至室温后研磨过筛,得磁性蓝藻生物炭。
实施例1
一种磁性蓝藻生物炭的制备方法,包括以下步骤:
(1)将太湖打捞的蓝藻藻泥进行冷冻干燥,得块状的蓝藻生物质。之后用研钵对其进行研磨,过60目筛。
(2)将所述Fe2O3与蓝藻生物质(w/w)为2%进行混合,放入80℃烘箱干燥24h,得中间产物。
(3)将上述中间产物放入管式炉,以5℃/min的速率程序升温至600℃,停留2h,全程通氮气以保证缺氧环境冷却至室温后研磨过80目筛,得磁性蓝藻生物炭。
将制得的磁性蓝藻生物炭材料用于含染料——橙黄G的废水处理,具体步骤如下:
在100mL 20mg/L的橙黄G溶液中加入0.4g/L生物炭,密封后置于恒温振荡器中以110r/min转速在25℃条件下振荡进行30min吸附平衡实验,发现吸附效果不到2%几乎可以忽略。之后再将10mmol/L过硫酸钠投加到烧杯中,在设定时间取样,样品经0.45μm孔径滤膜过滤后采用紫外-可见分光光度计在478nm波长条件下测定,在60min后橙黄G的降解效率高达97%。
实施例2
一种磁性蓝藻生物炭的制备方法,包括以下步骤:
(1)将打捞的蓝藻藻泥进行冷冻干燥,得块状的蓝藻生物质。之后用研钵对其进行研磨,过60目筛。
(2)将所述Fe2O3与蓝藻生物质(w/w)为5%进行混合,放入80℃烘箱干燥24h,得中间产物。
(3)将上述中间产物放入管式炉,以5℃/min的速率程序升温至500℃,停留2h,全程通氮气以保证缺氧环境冷却至室温后研磨过80目筛,得磁性蓝藻生物炭。
将制得的磁性蓝藻生物炭材料用于含染料——亚甲基蓝的废水处理,具体步骤如下:
在50mL浓度为0.04M的KH2PO4缓冲溶液中加入2.5mg亚甲基蓝粉末使其浓度为50mg/L,然后通过添加5%H2SO4将pH调节至3。然后在溶液中加入0.5g生物炭,并使其在恒温振荡器中以25℃和150rpm的状态进行30min吸附平衡实验,发现吸附效果不到1%,几乎可以忽略。之后再投加100mmol/LH2O2于烧杯中,在不同的反应时间取样,样品通过0.45-μm膜过滤后采用紫外-可见分光光度计在664nm波长条件下测定,在1h后亚甲基蓝的降解效率高达92.4%。
实施例3
一种磁性蓝藻生物炭的制备方法,包括以下步骤:
(1)将打捞的蓝藻藻泥进行冷冻干燥,得块状的蓝藻生物质。之后用研钵对其进行研磨,过60目筛。
(2)将所述Fe2O3与蓝藻生物质(w/w)为10%进行混合,放入80℃烘箱干燥36h,得中间产物。
(3)将上述中间产物放入管式炉,以5℃/min的速率程序升温至700℃,停留1h,全程通氮气以保证缺氧环境冷却至室温后研磨过80目筛,得磁性蓝藻生物炭。
将制得的磁性蓝藻生物炭材料用于含染料——酸性橙的废水处理,具体步骤如下:
在50mL浓度为0.04M的KH2PO4缓冲溶液中加入2.5mg酸性橙粉末使其浓度为50mg/L,然后通过添加5%H2SO4将pH调节至3。然后在溶液中加入0.5g生物炭,实验在恒温振荡器中以25℃和150rpm的状态下进行30min吸附平衡实验,发现吸附效果不到1%,几乎可以忽略。之后再投加100mmol/LH2O2在烧杯中,于不同反应时间取样,用0.45-μm滤膜过滤后采用紫外-可见分光光度计在484nm波长条件下测定,在1h后酸性橙的降解效率高达87.6%。
如图2所示磁性蓝藻生物炭降解污染物效果图,可以看出该磁性蓝藻生物炭吸附效果不明显,几乎可以忽略。但其对于水体中多种难降解污染物均具有显著的降解效果,能够将其转化为无毒害小分子物质或者是二氧化碳和水,扩大了其应用范围,甚至为同步去除水环境中不同难降解污染物提供了有益启示。
Claims (10)
1.一种磁性蓝藻生物炭的制备方法,其特征在于:包括以下步骤:
(1)将蓝藻进行冷冻干燥、研磨过筛处理,得到蓝藻生物质;
(2)将Fe2O3与蓝藻生物质混合,置于烘箱中干燥处理,得到中间产物;
(3)将中间产物置于管式炉内,于惰性气氛保护下进行碳化,冷却至室温后研磨过筛,得到磁性蓝藻生物炭。
2.根据权利要求1所述的磁性蓝藻生物炭的制备方法,其特征在于:步骤(2)中,Fe2O3的加入量占蓝藻生物质质量的2-10wt%。
3.根据权利要求1所述的磁性蓝藻生物炭的制备方法,其特征在于:步骤(3)中,碳化温度为400-800℃,碳化时间为2-4h。
4.根据权利要求1所述的磁性蓝藻生物炭的制备方法,其特征在于:步骤(2)中,干燥处理温度为60-80℃,干燥时间为24-36h。
5.根据权利要求1所述的磁性蓝藻生物炭的制备方法,其特征在于:惰性气氛为N2、Ar或NH3。
6.根据权利要求1所述的磁性蓝藻生物炭的制备方法,其特征在于:步骤(1)中,将蓝藻冷冻干燥处理得到块状蓝藻生物质,将块状蓝藻生物质过60目筛;步骤(3)中,将冷却产物经研磨处理后过80目筛。
7.根据权利要求3所述的磁性蓝藻生物炭的制备方法,其特征在于:碳化的升温速率为2-10℃/min。
8.一种根据权利要求1~7任一项所述制备方法得到的磁性蓝藻生物炭。
9.根据权利要求8所述的磁性蓝藻生物炭在降解废水中的应用。
10.根据权利要求9所述的应用,其特征在于:所述废水为有机染料。
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