CN113209942A - 一种纤维素基重金属复合吸附材料及制备方法 - Google Patents
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Abstract
本发明公开了一种纤维素基重金属复合吸附材料及制备方法，所述制备方法包括以下步骤：采用NaOH和尿素的混合溶液溶解纤维素，然后在凝固浴中再生成具有三维网状结构的纤维素小球、纤维或者其他形状的宏观材料，然后采用吸附沉淀法，负载铁氧化物或者铁氢氧化物，即得到体积不可逆缩减的纤维素基重金属复合吸附材料。本发明吸附材料制备工艺简单，无毒，生产成本低；吸附材料可用于从水体中快速去除重金属离子污染物，尤其是对砷、铬等重金属离子，具有优异的吸附性能，去除率高，吸附饱和干燥后，其体积不可逆的缩减为原来的1/10以下，大大降低后续处理的费用。
Description
技术领域
本发明涉及水处理技术领域，具体是一种纤维素基重金属复合吸附材料及制备方法。
背景技术
经济高效的水净化技术，一直是人们追求的目标。由于地理原因或地质原因，部分地区的地下水或者地表水，存在着明显的重金属污染。另外，随着人类社会工业化的进程，自然水体面临着严重金属污染的风险。重金属离子毒性大，在低浓度时就表现出明显的毒性，而且能在生物有机体中累积，通过食物链和饮用水进入人体或者动物体内，引起一系列不良反应甚至疾病。因此，分离移除水体中的重金属离子，对于环境保护和人类健康有着至关重要的作用。目前，用于水体重金属处理的方法主要有化学沉淀法、吸附法、离子交换法等等。吸附法适用场景广泛，操作简单，是应用最为广泛的水处理技术。但吸附饱和的材料，需要经过再生或者无害化处理，这种后续处理步骤，一般需要异位进行，运输费用会增加吸附法的成本。近年来，利用天然高分子材料作为吸附剂，吸附去除水体重金属受到越来越多研究人员 的关注，尤其是资源丰富、价廉、易得的天然纤维素为基体的吸附材料备受关注。
纤维素分子中含有大量羟基，对带有正电荷的重金属离子有良好的吸附能力。但水体中难于去除的重金属离子，如砷、铬等，均带负电荷。因此需要对纤维素进行改性或者以纤维素为基底，负载对砷、铬等有优异吸附性能的铁氧化物或铁氢氧化物材料，制备成复合吸附材料，得到高效复合吸附剂。
现有技术如授权公告号为CN201780087582.3的中国发明专利，公开了一种以微晶纤维素为基底，负载氢氧化铁的纤维素基粉体吸附剂及其制备方法。该方法制备的吸附剂，其尺寸在微纳米尺度，用于装填吸附柱时，水阻太大。而且由于纤维素没有形成三维网络互穿结构，孔隙度偏低，干燥后不会发生大的体积缩减。
发明内容
本发明就是为了解决现有技术中存在的问题，所提出了一种纤维素基重金属复合吸附材料及制备方法。
本发明采用了如下的技术方案。
一种纤维素基重金属复合吸附材料的制备方法，包括以下步骤：
S1.将尿素、NaOH和水按照质量比为7:12:81的比例混合获得尿素-NaOH混合溶液，将纤维素溶解在尿素-NaOH混合溶液中，搅拌得到质量分数为1-7.5% 的纤维素溶液；
S2.将步骤S1的纤维素溶液缓慢滴加到NaCl、HCl、HNO3或H2SO4溶液中，静置10-14h，得到纤维素小球；
S3.将步骤S2获得的纤维素小球用去离子水清洗后，浸没到0.1-0.3M铁盐溶液中10-14h；
S4. 将步骤S3获得的吸附铁盐后的纤维素小球进行抽滤，然后在含有氨水蒸汽的真空条件下，静置22-26h，用蒸馏水冲洗后，即得纤维素基重金属复合吸附材料。
进一步的，步骤S1中，所述纤维素选用α纤维素、微晶纤维素及其衍生物、纸浆纤维、棉纤维或富含纤维素的材料。
进一步的，所述纸浆纤维选用竹子、稻草、麦草、杨木、芦苇、桦木的碱法或硫酸盐法制浆并经过化学或生物漂白后的纸浆；棉纤维选用棉短绒或脱脂棉；所述富含纤维素的材料包括蒲草或废纸。
进一步的，步骤S3中，铁盐包括Fe2+或Fe3+盐中的一种或多种；所述Fe2+或Fe3+盐包括氯化物、硫酸盐、硝酸盐、醋酸盐。
进一步的，所述Fe2+或Fe3+盐选用氯化铁、硫酸亚铁、硝酸铁、醋酸铁或硫酸亚铁铵。
进一步的，步骤S2中，纤维素溶液以2-4 mL/min的速度滴加到NaCl、HCl、HNO3或H2SO4溶液中。
进一步的，步骤S2中，NaCl的浓度为8-12%；HCl、HNO3和H2SO4的浓度均为0.1-1 M。
一种上述纤维素基重金属复合吸附材料的制备方法制备获得的纤维素基重金属复合吸附材料。
进一步的，所述吸附材料为具有三维网络结构的球状、纤维状或块状。
本发明获得了如下有益效果。
本发明以纤维素为载体制备吸附剂，其原料来源广泛、价格低廉、环境友好，且制备方法简单、反应条件温和，设备要求低，便于规模化生产；
纤维素可以发生可逆的体积变化，负载铁氧化物、铁氢氧化物后，体积缩减过程不可逆。吸附饱和后，经干燥后，体积大幅缩减，有利于吸附剂使用后的运输，方便后续处理。
附图说明
图1为本发明纤维素小球负载氢氧化铁前后的扫描电镜图；
图2为本发明负载氢氧化铁的纤维素小球吸附As(III)的热力学曲线图；
图3为本发明纤维素小球干燥前后的对比图。
具体实施方式
以下参照实施例对本发明进行进一步的技术说明。
实施例1
称取7 g NaOH，12 g尿素，加入81 mL水溶解，配置总重量100 g的混合溶液。称取4g 棉纤维，加入上述溶液，剧烈搅拌，得到纤维素溶液。用注射器移取纤维素溶液，以3 mL/min的速度滴加到10 %的NaCl溶液中，再生成为具有三维网络结构的纤维素小球。静置12 h后，用去离子水冲洗，浸没到0.2 M 的FeCl3溶液中12 h，吸附铁离子到纤维素小球内部。取出后真空抽滤，去除多余的铁盐溶液。然后将吸附铁盐的纤维素小球，放到玻璃培养皿中，置于真空干燥器中，真空干燥器中用小烧杯盛放50 mL浓氨水溶液，干燥器密封后，静置24小时，将铁盐转变为铁氧化物或铁氢氧化物。最后将纤维素小球取出，用大量去离子水冲洗，即得到纤维素负载氢氧化铁的复合吸附材料。
实验结果如图1-3所示，图1（a.纤维素小球；b.负载氢氧化铁的纤维素小球）为纤维素小球负载氢氧化铁前后的扫描电镜照片，从图1可以看出，纤维素小球具有明显的孔隙结构，负载氢氧化铁之后，孔隙减小。图2为负载氢氧化铁的纤维素小球吸附As(III)的热力学曲线图，复合材料用于吸附含有As(III)的水，从图2可以看出，得到其最大饱和吸附量为237 mg/g。图3为纤维素小球干燥前后的光学照片，从图3可以看出，干燥后，其体积缩小为原来的5%。
Claims (9)
1.一种纤维素基重金属复合吸附材料的制备方法，其特征在于：包括以下步骤：
S1.将尿素、NaOH和水按照质量比为7:12:81的比例混合获得尿素-NaOH混合溶液，将纤维素溶解在尿素-NaOH混合溶液中，搅拌得到质量分数为1-7.5% 的纤维素溶液；
S2.将步骤S1的纤维素溶液缓慢滴加到NaCl、HCl、HNO3或H2SO4溶液中，静置10-14h，得到纤维素小球；
S3.将步骤S2获得的纤维素小球用去离子水清洗后，浸没到0.1-0.3M铁盐溶液中10-14h；
S4. 将步骤S3获得的吸附铁盐后的纤维素小球进行抽滤，然后在含有氨水蒸汽的真空条件下，静置22-26h，用蒸馏水冲洗后，即得纤维素基重金属复合吸附材料。
2.根据权利要求1所述的一种纤维素基重金属复合吸附材料的制备方法，其特征在于：步骤S1中，所述纤维素选用α纤维素、微晶纤维素及其衍生物、纸浆纤维、棉纤维或富含纤维素的材料。
3.根据权利要求2所述的一种纤维素基重金属复合吸附材料的制备方法，其特征在于：所述纸浆纤维选用竹子、稻草、麦草、杨木、芦苇、桦木的碱法或硫酸盐法制浆并经过化学或生物漂白后的纸浆；棉纤维选用棉短绒或脱脂棉；所述富含纤维素的材料包括蒲草或废纸。
4.根据权利要求1所述的一种纤维素基重金属复合吸附材料的制备方法，其特征在于：步骤S3中，铁盐包括Fe2+或Fe3+盐中的一种或多种；所述Fe2+或Fe3+盐包括氯化物、硫酸盐、硝酸盐、醋酸盐。
5.根据权利要求3所述的一种纤维素基重金属复合吸附材料的制备方法，其特征在于：所述Fe2+或Fe3+盐选用氯化铁、硫酸亚铁、硝酸铁、醋酸铁或硫酸亚铁铵。
6.根据权利要求1所述的一种纤维素基重金属复合吸附材料的制备方法，其特征在于：步骤S2中，纤维素溶液以2-4 mL/min的速度滴加到NaCl、HCl、HNO3或H2SO4溶液中。
7.根据权利要求1所述的一种纤维素基重金属复合吸附材料的制备方法，其特征在于：步骤S2中，NaCl的浓度为8-12%；HCl、HNO3和H2SO4的浓度均为0.1-1 M。
8.一种权利要求1-7任一所述的纤维素基重金属复合吸附材料的制备方法制备获得的纤维素基重金属复合吸附材料。
9.根据权利要求8所述的一种纤维素基重金属复合吸附材料，其特征在于：所述吸附材料为具有三维网络结构的球状、纤维状或块状。
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