CN116809020A - 一种去除水体中重金属的磁化改性吸附剂的制备方法 - Google Patents
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Abstract
本发明公开了一种去除水体中重金属的磁化改性吸附剂的制备方法，A对颗粒活性炭进行预处理；对预处理后所述颗粒活性炭进行酸化处理；对酸化处理后的所述颗粒活性炭采用化学共沉淀法制备酸化磁性颗粒活性炭；对酸化改性磁性颗粒活性炭干燥处理后得到吸附剂。本发明对磁性颗粒活性炭的合成过程进行了优化，基于传统的活性炭吸附剂进行磁化改性处理，合成制备一种具有磁性且吸附性能较好的磁性吸附材料。
Description
技术领域
本发明属于重金属处理技术领域，尤其是涉及一种去除水体中重金属的磁化改性吸附剂的制备方法。
背景技术
重金属废水是对环境污染最严重、对人类危害最大的工业废水之一，重金属废水的排放会对自然界中动植物的生长及人体健康造成较为严重的威胁，重金属可通过食物链在生物体内富集，破坏生物机体，引发多种疾病。因此如何对重金属废水进行更加有效的治理，已成为人们迫切需要解决的问题。因此需要一种去除水体中重金属的磁化改性吸附剂的制备方法。
发明内容
本发明的目的是针对上述问题，提供一种去除水体中重金属的磁化改性吸附剂的制备方法。
为达到上述目的，本发明提供如下技术方案：
本发明包括如下步骤：
A对颗粒活性炭进行预处理；
B对预处理后所述颗粒活性炭进行酸化处理；
C对酸化处理后的所述颗粒活性炭采用化学共沉淀法制备酸化磁性颗粒活性炭；
D对酸化改性磁性颗粒活性炭干燥处理后得到吸附剂。
进一步地，所述酸化的方法包括将所述颗粒活性炭加入到体积比为3:1的H2SO4-HNO3混酸溶液并混合均匀后60℃水浴回流1h静置冷却后用去离子水冲洗至表面呈中性。
进一步地，所述颗粒活性炭的预处理步骤包括：
步骤一，对颗粒活性炭过20-40目筛进行初筛；
步骤二，对所述颗粒活性炭浸渍混合与酸性溶液混合浸泡24h后冲洗至中性；
步骤三，将颗粒活性炭和去离子水按照体积比为1:5煮沸后搅拌5h后过滤；
步骤四，对过滤后的所述颗粒活性炭进行干燥处理。
进一步地，所述酸性溶液为体积分数为2%的HCl溶液 。
进一步地，所述干燥处理的方法包括在120℃的条件下常压干燥8h。
进一步地，所述磁性颗粒活性炭的制备方法包括
a FeCl3 ∙ 6H2O和FeSO4 ∙7H2O按照mol比2：1溶解在100ml蒸馏水后得到混合溶液；
所述混合溶液与所述颗粒活性炭按照mol比1：（1-5）在N2气条件在进行加热搅拌；
b温度升温至70℃滴加碱性溶液将PH调整至9~10后，在N2气条件在进行继续搅拌1h；
c将所述混合液室温陈化24h后用去离子冲洗至中性后烘干得到所述改性磁性颗粒活性炭。
现有技术相比，本发明提供了一种去除水体中重金属的磁化改性吸附剂的制备方法，具备以下有益效果：
本发明对磁性颗粒活性炭的合成过程进行了优化，基于传统的活性炭吸附剂进行磁化改性处理，合成制备一种具有磁性且吸附性能较好的磁性吸附材料。
附图说明
图1为本发明去除水体中重金属的磁化改性吸附剂的制备方法的流程示意图；
图2为本发明磁性颗粒活性炭的合成示意图；
图3为本发明酸化改性磁性颗粒活性炭的制备流程示意图；
具体实施方式
以下实施例仅处于说明性目的，而不是想要限制本发明的范围。
如图1所示，本发明包括如下步骤：
1.1颗粒活性炭的预处理
本实验按照如下步骤对颗粒活性炭进行预处理：
首先将实验用颗粒活性炭过20-40目筛，来固定实验过程中使用的颗粒活性炭尺寸大小。
其次称取一定量经过筛选的颗粒活性炭倒入1000 ml烧杯中，用去离子水对其进行冲洗、搅拌，浸泡在体积分数为2%的HCl溶液中浸泡24h后，用去离子水冲洗至中性。
在烧杯中加入去离子水，控制固液比为1:5以上。将烧杯放入电热套中进行加热煮沸。
将煮沸后的固液混合物进行机械搅拌5h后过滤。将(3) (4)步骤重复进行3次。
用去离子水反复冲洗经过煮沸处理后的颗粒活性炭，至滤液为中性。
将处理后的颗粒活性炭放入鼓风干燥烘箱中，在120℃的条件下常压干燥8h，记作GAC。
1.2. 磁性颗粒活性炭的合成
如图2所示，本发明采用化学共沉淀法制备磁性颗粒活性炭复合材料本实验按照如下步骤制备磁性颗粒活性炭复合材料：
称取FeCl3 ∙ 6H2O 7.8g 、FeSO4 ∙7H2O 3.8g即以摩尔比为2:1的比例溶解在100ml脱气蒸馏水中。加入一定质量的经过2.2.1所述方法处理后的颗粒活性炭至混合溶液中并在氮气氛围下进行机械搅拌。
当温度达到70℃时，向溶液中逐滴滴加 5M NaOH至溶液pH=9~10（每次加入约50ml），在这个pH下溶液从黄棕色变成黑色。滴加结束后继续在氮气的氛围下持续搅拌一小时。
搅拌结束后，将混合液室温陈化24h后用蒸馏水、无水乙醇反复冲洗至中性。
将剩余材料进行烘干，保存。
1.3 酸化改性磁性颗粒活性炭的制备如图3所示，酸化改性磁性颗粒活性炭的制备步骤如下：
称取10g经过1.1方法预处理后的颗粒活性炭，加入到体积比为3:1的H2SO4-HNO3混酸溶液中并混合均匀；
在60℃水浴回流1h，静置冷却后用去离子水冲洗至表面呈中性；
将处理后的颗粒活性炭放入鼓风烘箱中，在120℃的条件下常压干燥8h，记作N-GAC。
将经过酸化处理后的颗粒活性炭N-GAC按照1.2所述的化学共沉淀法来合成酸化改性磁性颗粒活性炭。
将材料进行干燥封闭保存，并记作NGAC-Fe3O4。
本发明针对目前普遍存在的重金属废水污染问题，以铬离子和铜离子为对象，进行了新型磁化改性吸附剂吸附去除水体中重金属的研究。研究中基于传统的活性炭吸附剂进行磁化改性处理性，合成制备一种具有磁性且吸附性能较好的磁性吸附材料。利用该吸附剂对含有铜、铬废水进行处理，研究不同条件对含铬含铜废水去除性能的影响，分析了磁性活性炭对含铬含铜废水的去除效果及作用机理，并对磁性颗粒活性炭的合成过程及对废水的处理过程进行了优化，以期为含重金属废水处理提供相应的理论与技术指导。
以上所述仅为本发明的较佳实施例，并不用以限制本发明，凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。
Claims (6)
1.一种去除水体中重金属的磁化改性吸附剂的制备方法，其特征在于：包括如下步骤：
A对颗粒活性炭进行预处理；
B对预处理后所述颗粒活性炭进行酸化处理；
C对酸化处理后的所述颗粒活性炭采用化学共沉淀法制备酸化磁性颗粒活性炭；
D对酸化改性磁性颗粒活性炭干燥处理后得到吸附剂。
2.根据权利要求1所述的一种去除水体中重金属的磁化改性吸附剂的制备方法，其特征在于：所述酸化的方法包括将所述颗粒活性炭加入到体积比为3:1的H2SO4-HNO3混酸溶液并混合均匀后60℃水浴回流1h静置冷却后用去离子水冲洗至表面呈中性。
3.根据权利要求1所述的一种去除水体中重金属的磁化改性吸附剂的制备方法，其特征在于：所述颗粒活性炭的预处理步骤包括：
步骤一，对颗粒活性炭过20-40目筛进行初筛；
步骤二，对所述颗粒活性炭浸渍混合与酸性溶液混合浸泡24h后冲洗至中性；
步骤三，将颗粒活性炭和去离子水按照体积比为1:5煮沸后搅拌5h后过滤；
步骤四，对过滤后的所述颗粒活性炭进行干燥处理。
4.根据权利要求3所述的一种去除水体中重金属的磁化改性吸附剂的制备方法，其特征在于：所述酸性溶液为体积分数为2%的HCl溶液 。
5.根据权利要求1或者3所述的一种去除水体中重金属的磁化改性吸附剂的制备方法，其特征在于：所述干燥处理的方法包括在120℃的条件下常压干燥8h。
6.根据权利要求1所述的一种去除水体中重金属的磁化改性吸附剂的制备方法，其特征在于：所述磁性颗粒活性炭的制备方法包括
a FeCl3 ∙ 6H2O和FeSO4 ∙7H2O按照mol比2：1溶解在100ml蒸馏水后得到混合溶液；
所述混合溶液与所述颗粒活性炭按照mol比1：（1-5）在N2气条件在进行加热搅拌；
b温度升温至70℃滴加碱性溶液将PH调整至9~10后，在N2气条件在进行继续搅拌1h；
c将所述混合液室温陈化24h后用去离子冲洗至中性后烘干得到所述改性磁性颗粒活性炭。
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| CN107469769A (zh) * | 2017-09-06 | 2017-12-15 | 河海大学 | 一种磁性吸附材料的制备方法及其应用 |
| CN109261124A (zh) * | 2018-10-30 | 2019-01-25 | 成都市水泷头化工科技有限公司 | 一种去除水中重金属离子的活性炭吸附剂及制备方法 |
| CN110538630A (zh) * | 2019-08-27 | 2019-12-06 | 华南农业大学 | 一种耐酸型油茶壳基磁性活性炭及其制备方法 |
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| CN107469769A (zh) * | 2017-09-06 | 2017-12-15 | 河海大学 | 一种磁性吸附材料的制备方法及其应用 |
| CN109261124A (zh) * | 2018-10-30 | 2019-01-25 | 成都市水泷头化工科技有限公司 | 一种去除水中重金属离子的活性炭吸附剂及制备方法 |
| CN110538630A (zh) * | 2019-08-27 | 2019-12-06 | 华南农业大学 | 一种耐酸型油茶壳基磁性活性炭及其制备方法 |
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