CN108745298B - 一种Fe/Mn改性毛竹遗态复合材料的制备方法及其应用 - Google Patents
一种Fe/Mn改性毛竹遗态复合材料的制备方法及其应用 Download PDFInfo
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Abstract
本发明公开了一种Fe/Mn改性毛竹遗态复合材料的制备方法及其应用。将毛竹切割为块体，削去表层致密结构，干燥，置于稀氨水中浸煮做抽提预处理，随后洗净干燥。以铁锰复合盐溶液为前驱体溶液，将抽提后的毛竹浸没于前驱体溶液中，在55~65℃条件下搅拌并水浴保温5天，取出试样，在60~80℃条件下烘24小时后于马弗炉中碳化，冷却，研磨，过筛，即制得Fe/Mn改性毛竹遗态复合材料。该Fe/Mn改性毛竹遗态复合材料能够应用于对水中砷进行吸附分离。本发明的制备方法成本低廉，工艺简单，对于减少固废污染、促进废物再利用具有重要意义。本发明的Fe/Mn改性毛竹遗态复合材料对水中砷的去除率高，吸附过程完成后，能够通过外加磁力进行固液分离，重复利用。
Description
技术领域
本发明属于吸附材料制备技术领域，特别涉及一种Fe/Mn改性毛竹遗态复合材料的制备方法及其应用。
背景技术
由于现代工业的发展，化工废水的排放、化石燃料的燃烧及生活垃圾等人为污染源，以及地质侵蚀、风化等天然污染源导致大量重金属进入水体，使水体重金属污染成为世界范围内的环境问题。砷作为一种常见的重金属污染物，具有剧毒和致癌性，对生态系统和人类健康构成严重威胁。长期饮用高砷水，会引起黑脚病，神经痛，血管损伤，肝肿大等健康问题。因此，发明经济、有效、可靠的除砷技术至关重要。
废水中重金属的去除方法有：沉淀法，离子交换法，反渗透法和吸附法等多种方法。但是其许多价格昂贵，并具有一定的局限性（例如产生二次污染物，工艺复杂等）。吸附法以其成本低、操作方便、效率高、设备简单、材料易再生等优点而备受关注。其中，生物吸附法是一种高效环保去除重金属离子的吸附技术，而且生物吸附剂的来源丰富、品种多样且成本低廉，此外，解吸后的生物吸附剂可重复使用。因此，寻找各种天然、廉价和高效的吸附材料，开发环境友好型产品和技术将成为可持续发展的必然趋势。
植物遗态材料因其价格低廉、来源广泛且结构特性优异而成为一种备受关注的吸附剂，它是一种在自然界经亿万年遗传演变形成的完美独特本征结构基础上，通过人工改性制备出的既保留天然植物特殊结构，又具有人为赋予新特性的吸附材料。其天然分级多孔结构提供了精密完美的稳固改性负载体，可改善吸附过程的水力学条件，从而有效提高了新材料的比表面积利用率和抗冲刷破坏性。
目前，国内外研究者尝试以不同植物遗态（如棕榈、山核桃木、小麦秸秆等）为模板制备获得具有水质净化功能的植物遗态材料。我国盛产的竹材具有维管系统的梯纹导管、环纹孔、螺纹导管以及纤维管、纤维管壁上的纹孔等分级多孔独特结构，被认为是植物模板的适宜选择。其中，毛竹是我国特别是广西分布广泛的竹类植物之一，具有较高的经济价值。它具有不同尺度范围的有序多孔的特殊解剖结构，纹孔膜和纹孔塞的存在，使得纹孔不是一种天然的开孔，通过适宜浸煮剂的预处理可以方便地将木材中导管孔的浸填体组织去除，增加毛竹竹材内部结构的三维网络连通性，提高后期浸渍性能，同时提高产物的网络连通性，利于制备植物模板多孔吸附材料。
但是目前对毛竹的利用主要集中在制纸浆、农具、家具和日常生活用品，且主要利用毛竹主干，对毛竹根部以及分枝以上部分通常丢弃或作为柴火，这些部分作为可再生性废弃物资源，如果处理不当，不仅会造成资源浪费，更会形成污染，给环境保护带来压力，不利于生态环境的可持续发展。如果用遗态概念去开发利用这些材料，就会弥补科学研究在“废弃物”再利用方面的不足，改善不良的处理方式，可将其变废为宝，这也非常符合国家提出的资源再利用、环境更美好的可持续发展战略，为实现其再利用提供了一条新的科学有效的途径。
发明内容
本发明的目的是提供一种Fe/Mn改性毛竹遗态复合材料的制备方法及其应用。
本发明思路：以稀氨水为前期预处理抽提液，含铁锰的混合盐溶液为前驱体溶液进行材料的制备，通过工艺控制，制备出保留了毛竹天然结构形态的Fe/Mn改性毛竹遗态复合材料，对其物相、结构、成分组成、形貌特征等进行了表征，并将其应用于含砷废水的吸附除砷试验，实现了大量废弃毛竹的资源化利用。
本发明的Fe/Mn改性毛竹遗态复合材料的具体制备步骤为：
（1）将毛竹切块干燥，然后削去结构致密的表层结构，得到毛竹块备用。
（2）配制体积百分比浓度为5~8%的稀氨水作为毛竹预处理抽提液。
（3）以体积比为1:1的乙醇-超纯水混合溶液为溶剂，将硝酸铁和氯化锰按摩尔比为(100-n):n加入到溶剂中溶解制得总摩尔浓度为0.8~1.2 mol/L的铁锰复合盐前驱体溶液。
（4）将步骤（1）获得的毛竹块置于步骤（2）制得的毛竹预处理抽提液中，在95~105℃条件下浸煮6~8小时，完成抽提预处理。
（5）将步骤（4）获得的产物用超纯水洗净，并在80 ℃的烘箱内干燥24小时。
（6）按液固比为3~5:1，将步骤（5）获得的产物浸没于步骤（3）获得的铁锰复合盐前驱体溶液中，在55~65 ℃水浴条件下保温5天，期间不定时补充步骤（3）获得的铁锰复合盐前驱体溶液并搅拌以保证步骤（5）获得的产物始终处于被步骤（3）获得的铁锰复合盐前驱体溶液浸没的状态，且步骤（3）获得的铁锰复合盐前驱体溶液处于分散状态，从溶液中取出材料后，在60 ℃条件下烘干24小时。
（7）重复步骤（6）3次。
（8）将步骤（7）获得产物置于马弗炉中于600~800 ℃条件下焙烧3~6小时，自然冷却至室温。
（9）将步骤（8）获得的产物磨碎，过筛，即制得Fe/Mn改性毛竹遗态复合材料。
本发明步骤（3）中硝酸铁和氯化锰的摩尔比优选为9:1。
本发明步骤（8）中马弗炉的温度优选700 ℃。
上述制得的Fe/Mn改性毛竹遗态复合材料应用于对水中砷进行吸附分离。
本发明的优点在于：
本发明的制备方法成本低廉，工艺简单，对于减少固废污染、促进废物再利用具有重要意义。本发明的Fe/Mn改性毛竹遗态复合材料对水中砷的去除率高，吸附过程完成后，能够通过外加磁力进行固液分离，重复利用。
附图说明
图1为本发明实施例制得的Fe/Mn改性毛竹遗态复合材料的FT-IR谱图。
图2为本发明实施例制得的Fe/Mn改性毛竹遗态复合材料的X-射线衍射图谱。
图3为本发明实施例中Fe/Mn改性毛竹遗态复合材料对As(V)的去除效果图。
具体实施方式
实施例：
（1）将毛竹切块干燥，然后削去结构致密的表层结构，得到毛竹块备用。
（2）配备体积百分比浓度为5%的稀氨水作为毛竹预处理抽提液。
（3）以体积比为1:1的乙醇-超纯水混合溶液为溶剂，将硝酸铁和氯化锰按摩尔比为9:1加入到溶剂中溶解制得总摩尔浓度为1.2 mol/L的铁锰复合盐前驱体溶液。
（4）将步骤（1）获得的毛竹块置于步骤（2）制得的毛竹预处理抽提液中，在100 ℃条件下浸煮8小时，完成抽提预处理。
（5）将步骤（4）获得的产物用超纯水洗净，并在80 ℃的烘箱内干燥24小时。
（6）按液固比为3:1，将步骤（5）获得的产物浸没于步骤（3）获得的铁锰复合盐前驱体溶液中，在60 ℃水浴条件下保温5天，期间不定时补充步骤（3）获得的铁锰复合盐前驱体溶液并搅拌以保证步骤（5）获得的产物始终处于被步骤（3）获得的铁锰复合盐前驱体溶液浸没的状态，且步骤（3）获得的铁锰复合盐前驱体溶液处于分散状态，从溶液中取出材料后，在60 ℃条件下烘干24小时。
（7）重复步骤（6）3次。
（8）将步骤（7）获得产物置于马弗炉中于700 ℃条件下焙烧3小时，自然冷却至室温。
（9）将步骤（8）获得的产物磨碎，过100目筛，即制得Fe/Mn改性毛竹遗态复合材料。
将本实施例制得的 Fe/Mn改性毛竹遗态复合材料应用于对水中As（V）进行去除。
称取25 mg本实施例制得的Fe/Mn改性毛竹遗态复合材料置于50mL含As(V)浓度为25 mg/L的溶液中。在pH值分别为3、5和8，温度为25 ℃，转速为150 rpm的条件下，进行振荡反应24 h后，用0.45 μm的滤膜过滤，用原子荧光形态分析仪测定溶液中的剩余As(V)浓度以考察其吸附能力，结果如图3所示，可以看出，本实施例制备得到的Fe/Mn改性毛竹遗态复合材料在pH=5的条件下对As（V）具有良好的去除能力。
Claims (3)
1.一种Fe/Mn改性毛竹遗态复合材料的制备方法，其特征在于具体步骤为：
(1)将毛竹切块干燥，然后削去结构致密的表层结构，得到毛竹块备用；
(2)配制体积百分比浓度为5～8％的稀氨水作为毛竹预处理抽提液；
(3)以体积比为1:1的乙醇-超纯水混合溶液为溶剂，将硝酸铁和氯化锰按摩尔比为9:1加入到溶剂中溶解制得总摩尔浓度为0.8～1.2mol/L的铁锰复合盐前驱体溶液；
(4)将步骤(1)获得的毛竹块置于步骤(2)制得的毛竹预处理抽提液中，在95～105℃条件下浸煮8小时，完成抽提预处理；
(5)将步骤(4)获得的产物用超纯水洗净，并在80℃的烘箱内干燥24小时；
(6)按液固比为3～5:1，将步骤(5)获得的产物浸没于步骤(3)获得的铁锰复合盐前驱体溶液中，在55～65℃水浴条件下保温5天，期间不定时补充步骤(3)获得的铁锰复合盐前驱体溶液并搅拌以保证步骤(5)获得的产物始终处于被步骤(3)获得的铁锰复合盐前驱体溶液浸没的状态，且步骤(3)获得的铁锰复合盐前驱体溶液处于分散状态，从溶液中取出材料后，在60℃条件下烘干24小时；
(7)重复步骤(6)3次；
(8)将步骤(7)获得产物置于马弗炉中于600～800℃条件下焙烧3～6小时，自然冷却至室温；
(9)将步骤(8)获得的产物磨碎，过筛，即制得Fe/Mn改性毛竹遗态复合材料。
2.根据权利要求1所述的Fe/Mn改性毛竹遗态复合材料的制备方法，其特征在于步骤(8)中马弗炉的温度为700℃。
3.一种如权利要求1、2中所述方法制备的Fe/Mn改性毛竹遗态复合材料的应用，其特征在于该Fe/Mn改性毛竹遗态复合材料应用于对水中砷吸附分离。
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