CN105817212A - 一种用沉积菱铁矿制备Fe/C复合多孔结构材料的方法 - Google Patents

一种用沉积菱铁矿制备Fe/C复合多孔结构材料的方法 Download PDF

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CN105817212A
CN105817212A CN201610326853.3A CN201610326853A CN105817212A CN 105817212 A CN105817212 A CN 105817212A CN 201610326853 A CN201610326853 A CN 201610326853A CN 105817212 A CN105817212 A CN 105817212A
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刘海波
陈天虎
邹雪华
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Hefei University of Technology
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Abstract

本发明公开了一种用沉积菱铁矿制备Fe/C复合多孔结构材料的方法，其特征在于：其是以低品位沉积菱铁矿和生物质粉体为原料，经混合、成型后，再在还原气氛下650～900℃热解和还原反应得到，主要物相为生物质炭和零价铁。本发明的Fe/C复合多孔结构材料具有高开放孔隙率、高磁化率、高吸附性和高生物化学活性，是具有生物活性和吸附性能的廉价生物载体材料，在微污染水净化中的应用具有很大前景，特别适合用于富营养化水体同步脱氮处理中。

Description

一种用沉积菱铁矿制备Fe/C复合多孔结构材料的方法
一、技术领域
本发明涉及低品位菱铁矿矿石和生物质资源化利用，属于矿物加工、生物质利用和环境工程材料领域。
二、背景技术
菱铁矿是分布广泛的一种碳酸盐矿物，晶体化学式为FeCO3。菱铁矿矿石常常在一些金属矿山作为伴生矿开采。高品位菱铁矿常常通过焙烧得到氧化铁用于炼铁，低品位菱铁矿通常情况下没有得到利用，常常在矿石开采中作为废石抛弃，既占用了土地，又破坏了环境。
我国菱铁矿资源丰富位居世界前列，已探明储量18.34亿吨，占铁矿石探明储量的14％。主要分布于云南、陕西、甘肃、青海、新疆、安徽等。一方面需要用经济合理的选冶技术开发利用菱铁矿；另一方面，必须对低品位菱铁矿资源进行非传统的开发利用。
我国每年生产各种秸秆大约10亿吨，农林产品及以生物质为原料的工业企业也产生数以亿吨计的加工残余物。随着农村经济发展和生活水平提高，导致秸秆在全国范围内大量过剩。每到收获季节，秸秆焚烧造成了严重的大气污染，同时也存在严重的火灾隐患和航空飞行安全问题。对秸秆等农产品废弃物进行资源化利用已经成为全国各地政府环境综合治理的当务之急。
生物质能源化利用有如下几种途径；热解气化、热解液化、直接燃烧、成型燃烧、成型碳化等。热解气化目前遇到热解气中焦油净化的难题；热解液化存在制得的液体燃料热值低、成分复杂的问题；直接燃烧存在锅炉积碳的问题。目前成型燃烧和成型碳化受到广泛关注。
三、发明内容
本发明是为避免上述现有技术所存在的问题，提供一种用沉积菱铁矿制备Fe/C复合多孔结构材料的方法，旨在同时实现低品位沉积菱铁矿和生物质的再利用。
本发明解决技术问题，采用如下技术方案：
本发明用沉积菱铁矿制备Fe/C复合多孔结构材料的方法，其特征在于：
将低品位沉积菱铁矿粉体和生物质粉体按照质量比1:0.5～15混合造粒，然后在还原气氛下经650～900℃热解和还原焙烧15～60min，再在无氧气氛下自然冷却至室温，即获得以生物质炭和零价铁为主要物相的Fe/C复合多孔结构材料。
其中：所述的低品位沉积菱铁矿的矿物组成主要包括：菱铁矿、黏土矿物和石英，铁的品位在30-55％；
所述的生物质为：各类农作物秸秆，木材加工废弃物锯末、刨花，庭院和绿化修整的枯枝树叶，或农产品加工产生的固体残渣。
本发明用沉积菱铁矿制备Fe/C复合多孔结构材料的方法，具体是按如下步骤进行：
(1)将低品位沉积菱铁矿矿石破碎、筛分，获得粒径不大于0.1mm的沉积菱铁矿粉体；将生物质破碎成粒径不大于5mm的生物质粉体；
(2)将沉积菱铁矿粉体和生物质粉体按照质量比1:0.5～15混合均匀，获得混合料；
(3)用成型机把所述混合料成型为直径4-12mm的棒状颗粒物；
(4)将所述棒状颗粒物在还原气氛下于650～900℃热解和还原焙烧15～60min，再在无氧气氛下自然冷却至室温，即获得以生物质炭和零价铁为主要物相的Fe/C复合多孔结构材料。
本发明用沉积菱铁矿矿石和生物质制备Fe/C复合多孔结构材料，其有益效果体现在以下几个方面：
1、沉积菱铁矿矿石和生物质粉体混合物挤出成型，生物质在挤出成型的胚料中具有粘结作用，使成型胚料具有较高的颗粒强度，无需添加粘结剂；在还原气氛下650～900℃热解和还原反应过程中，沉积菱铁矿矿石中作为杂质组分的粘土矿物等与生物质中的钾钠化学反应，具有增强烧结、提高颗粒强度的作用。
2、在还原气氛下生物质的热解气化，一方面可以提高材料的孔隙率和比表面积，获得多孔结构的材料，另一方面热解还原气体H2、CO、挥发性有机物与沉积菱铁矿矿石中铁反应转变为零价铁。生物质既是材料的致孔剂，又是铁的还原剂，还是形成生物炭的前驱体。
3、选择沉积菱铁矿矿石，既利用了低品位铁矿资源，又利用了沉积菱铁矿矿石资源的矿物学特性。经研究发现，菱铁矿矿石中的主要矿物菱铁矿在还原气氛下热分解转变为具有纳米孔结构的零价铁材料。还原产物零价铁具有较低的结晶度和较高的反应活性。
4、低品位沉积菱铁矿矿石中的化学氧不仅具有增强生物质热解气化的作用，还具有催化生物质热解气化过程中焦油裂解的作用，可以消除热解气体中的焦油。
5、低品位沉积菱铁矿矿石粉体与生物质粉体混合物经过挤出成型、还原气氛下热解反应，不仅菱铁矿还原形成的零价铁与生物碳化形成的生物炭紧密复合，而且材料具有特定的粒径、开放的大孔空隙、孔隙体积大、强磁性、高比表面积、良好的吸附性和化学反应活性。
6、Fe/C复合多孔结构材料既具有高效吸附除磷作用，还具有吸附水中各类有机污染物的作用。同时其高开放孔隙率又可以使各类微生物在其颗粒外表面和内部附着，是具有生物活性的优良微生物载体材料，微生物在Fe/C复合多孔结构材料外表面和内部形成氧化还原分带，同时具有氧化氨氮和反硝化脱氮的作用，在微污染水净化中的应用具有很大前景，特别适合富营养化水体同步脱氮处理中应用。
四、附图说明
图1为实施例1所制备的Fe/C复合多孔结构材料的粉末X射线衍射图谱，显示其中主要物相为单质铁；
图2为实施例1所制备的Fe/C复合多孔结构材料SEM图像，可以看出菱铁矿相变纳米铁的形貌特征。
五、具体实施方式
实施例1
本实施例按如下步骤制备Fe/C复合多孔结构材料：
(1)将铁品位47.3％的低品位沉积菱铁矿矿石破碎、过0.1mm筛，获得沉积菱铁矿粉体；将油菜秸秆破碎、过1mm筛，获得秸秆粉体；
(2)按照质量比1:3称取沉积菱铁矿粉体和秸秆粉体并拌合均匀，获得混合料；
(3)把上述混合料加入螺杆挤出成型机料斗内，挤出成型为直径5mm的棒状颗粒物；
(4)将成型的棒状颗粒物在管式炉中氢气气氛下于750℃焙烧30min，然后在无氧气氛下自然冷却至室温，即获得以生物质炭和零价铁为主要物相的Fe/C复合多孔结构材料。
图1为本实施例所制备的Fe/C复合多孔结构材料粉末的X射线衍射图谱，表明原始样品中的杂质石英保持不变，菱铁矿被生物质还原为单质铁。产物中单质铁含量为56％，生物炭的含量为17％。
图2为本实施例所制备Fe/C复合多孔结构材料的SEM图像，可以看出菱铁矿相变形成纳米铁的形貌特征。
实施例2
本实施例按如下步骤制备Fe/C复合多孔结构材料：
(1)将铁品位47.3％的低品位沉积菱铁矿矿石破碎、过0.1mm筛，获得沉积菱铁矿粉体；将木材加工的锯屑破碎、过1mm筛，获得生物质粉体；
(2)按照质量比1:5称取沉积菱铁矿粉体和生物质粉体并拌合均匀，获得混合料；
(3)把上述混合料加入螺杆挤出成型机料斗内，挤出成型为直径5mm的棒状颗粒物；
(4)将成型的棒状颗粒物在管式炉中氢气气氛下于850℃焙烧25min，然后在无氧气氛下自然冷却至室温，即获得以生物质炭和零价铁为主要物相的Fe/C复合多孔结构材料。
经XRD分析，结果表明原始样品中的杂质石英保持不变，菱铁矿被生物质还原为单质铁。经测试，产物孔隙体积比为68％，磁化率为9920SI、比表面积为79.8m2/g。

Claims (5)

1.一种用沉积菱铁矿制备Fe/C复合多孔结构材料的方法，其特征在于：
将低品位沉积菱铁矿粉体和生物质粉体按照质量比1:0.5～15混合造粒，然后在还原气氛下经650～900℃热解和还原焙烧15～60min，再在无氧气氛下自然冷却至室温，即获得以生物质炭和零价铁为主要物相的Fe/C复合多孔结构材料。
2.根据权利要求1所述的方法，其特征在于：
所述生物质为：农作物秸秆，木材加工废弃物锯末、刨花，庭院和绿化修整的枯枝树叶，或农产品加工产生的固体残渣。
3.根据权利要求1所述的方法，其特征在于：所述低品位沉积菱铁矿中铁的品位在30-55％。
4.根据权利要求1所述的方法，其特征在于，具体是按如下步骤进行：
(1)将低品位沉积菱铁矿矿石破碎、筛分，获得粒径不大于0.1mm的沉积菱铁矿粉体；将生物质破碎成粒径不大于5mm的生物质粉体；
(2)将沉积菱铁矿粉体和生物质粉体按照质量比1:0.5～15混合均匀，获得混合料；
(3)用成型机把所述混合料成型为直径4-12mm的棒状颗粒物；
(4)将所述棒状颗粒物在还原气氛下于650～900℃热解和还原焙烧15～60min，再在无氧气氛下自然冷却至室温，即获得以生物质炭和零价铁为主要物相的Fe/C复合多孔结构材料。
5.根据权利要求1或4所述的，其特征在于：所述还原气氛为含有氢气或一氧化碳的气氛。
CN201610326853.3A 2016-05-13 2016-05-13 一种用沉积菱铁矿制备Fe/C复合多孔结构材料的方法 Active CN105817212B (zh)

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CN114272896A (zh) * 2021-12-23 2022-04-05 中南大学 一种介导草酸去除六价铬和染料的铁基生物炭制备及应用

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