CN112812231B - 一种吸附土壤中Cd的材料 - Google Patents

一种吸附土壤中Cd的材料 Download PDF

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CN112812231B
CN112812231B CN202110186921.1A CN202110186921A CN112812231B CN 112812231 B CN112812231 B CN 112812231B CN 202110186921 A CN202110186921 A CN 202110186921A CN 112812231 B CN112812231 B CN 112812231B
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王晓景
何晋勇
张号
梁扬志
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Abstract

土壤和地下水重金属污染物来源广泛，包括电镀、电池、电解、采矿、冶炼、农药、医药、油漆、颜料、五金、机械、化妆品、陶瓷、化工等众多行业。吸附是常用的去除重金属的方法。然而现有的吸附材料普遍吸附容量较小，因此，需要一种能够大量吸附土壤溶液和水中的重金属的新材料。本申请属于污染修复/治理领域，公开了一种吸附水体或土壤溶液中重金属Cd2+的聚合物材料及其合成方法。

Description

一种吸附土壤中Cd的材料
技术领域
本申请属于污染修复/治理领域，公开了一种吸附水体或土壤溶液中重金属Cd2+的聚合物材料及其合成方法。
背景技术
土壤和地下水重金属污染物来源广泛，包括电镀、电池、电解、采矿、冶炼、农药、医药、油漆、颜料、五金、机械、化妆品、陶瓷、化工等众多行业。吸附是常用的去除重金属的方法。然而现有的吸附材料普遍吸附容量较小，因此，需要一种能够大量吸附土壤溶液和水中的重金属的新材料。
发明内容
本申请是一种高效快速吸附重金属Cd2+离子的新材料。
其结构式为：
。
其制备方法如下：
1) 在溴化1-丁基-3-甲基咪唑 [bmim]Br中，加入N-乙酰基-1,6-二氨基吡啶、丙烯醛、异氰环己烷，上述四组分摩尔比1.5:1:1:1，将所得混合物在室温搅拌3h。反应完成后，将反应混合物加纯水搅拌，过滤，固相用乙酸乙酯搅拌溶解，然后用饱和食盐水洗，取乙酸乙酯层用无水硫酸镁干燥，过滤，滤液真空浓缩至干，固相用乙酸乙酯/正己烷 (V;V=1:3)洗脱得到中间体。
）玻璃反应器中，加入乙酸乙酯，对二乙烯基苯和前述中间体，其中对二乙烯基苯和前述中间体摩尔比1:1，搅拌，将溶液以氮气脱气，然后加入偶氮二异丁腈引发剂，氮气流下，80℃加热搅拌24小时。冷却至室温，然后在乙醚中沉降，过滤，过滤得到的固体微粒使用乙醇洗涤3次。真空干燥，得到白色微粒产物。
3）上述100重量份白色微粒经加料口加入单螺杆挤出机中，控制口模温度 100℃，压力为 11 MPa。通过安装在挤出机机筒上的发泡剂注入口注入15重量份发泡剂液态二氧化碳。然后经直径 3 mm 的圆孔口模挤出、切粒、冷却得到产物发泡珠粒，产物用于吸附重金属Cd2+离子，具有较高的吸附容量。
具体实施方式
实施例1(制备实验)：
在溴化1-丁基-3-甲基咪唑 [bmim]Br（0.09 mmol，山东西亚化学科技有限公司，99%）中，加入N-乙酰基-1,6-二氨基吡啶（0.06 mol，上海麦克林生化科技有限公司，97%）、丙烯醛（0.06 mmol，山东喜玛供应链管理有限公司，99%）和异氰环己烷（0.06 mmol，江苏艾康生物医药研发有限公司，98%），将所得混合物在室温搅拌3h。反应完成后，将反应混合物加100 ml纯水搅拌，过滤，固相用150 mL乙酸乙酯搅拌溶解，然后用150 mL饱和食盐水洗，取乙酸乙酯层用无水硫酸镁干燥，过滤，滤液真空浓缩至干，固相用乙酸乙酯/正己烷 (V;V=1:3)洗脱得到中间体。产率79%。反应式如下：
。
中间体元素分析(％)计算值：C, 68.43; H, 7.43; N, 18.78; O, 5.36。测定值：C, 68.39; H, 7.41; N, 18.76; O, 5.44。IR(KBr，cm-1)：3250，3174，3082，3018，2930，2887，2848，1822，1632，1529，1464，1410，1325，982，912，723。
250ml玻璃反应器中，加入100mL乙酸乙酯，0.04mol对二乙烯基苯(DVB，98％，郑州杰克斯化工产品有限公司，使用前先用中性氧化铝过滤除去阻聚剂)和0.04 mol前述中间体，搅拌，将溶液以氮气脱气5分钟，然后加入0.15 g偶氮二异丁腈(AIBN)引发剂，氮气流下，80℃加热搅拌24小时。冷却至室温，然后在乙醚中沉降，过滤，过滤得到的固体微粒使用乙醇洗涤3次。真空干燥，得到白色微粒产物，产率86.9％。
上述100重量份白色微粒经加料口加入单螺杆挤出机中，控制口模温度 100℃，压力为 11 MPa。通过安装在挤出机机筒上的发泡剂注入口注入15重量份发泡剂液态二氧化碳。然后经直径 3 mm 的圆孔口模挤出、切粒、冷却得到产物发泡珠粒，收率97.1％，产物结构式如下。元素分析(％)计算值：C, 74.96; H, 8.39; N, 12.95; O, 3.70。测定值：C,74.90; H, 8.38; N, 12.98; O, 3.74。产物FTIR结果如附图1所示。
实施例2(Cd2+吸附实验)：
采集野外无污染土壤，为砂壤土，风干碾细后过2 mm筛。称取2 kg上述过筛的无污染土样，将CdCl2(优级纯）碾磨粉碎，加入土中配得0.5 g Cd/kg的土样，混合均匀，并按照GB/T 17141-1997《土壤质量铅镉的测定石墨炉原子吸收分光光度法》测得土中镉含量0.5±0.5 g Cd/kg土。然后称取1 kg上述含镉土样放入3 L锥形瓶中，然后加入1 L去离子水，最后加入1 g本申请产物发泡珠粒，室温下30 rpm振荡。60分钟后，停止震荡，手工取出全部发泡珠粒，风干发泡珠粒，然后按照HJ 786-2016《固体废物-铅、锌和镉的测定:火焰原子吸收分光光度法》检测风干的发泡珠粒的镉含量即吸附量，测得发泡珠粒对镉的吸附量为0.352 g镉/g珠粒。
附图说明：
附图1为本申请产物的FTIR结果。

Claims (1)

1.一种高效快速吸附重金属Cd2+离子的新材料，结构式如下：
Figure FDA0004125946900000011
其制备方法如下：在溴化1-丁基-3-甲基咪唑[Bmim]Br中，加入N-乙酰基-1，6-二氨基吡啶、丙烯醛、异氰环己烷，上述四组分摩尔比1.5:1:1:1，将所得混合物在室温搅拌3h；反应完成后，将反应混合物加纯水搅拌，过滤，固相用乙酸乙酯搅拌溶解，然后用饱和食盐水洗，取乙酸乙酯层用无水硫酸镁干燥，过滤，滤液真空浓缩至干，固相用乙酸乙酯/正己烷V:V＝1:3洗脱得到中间体；玻璃反应器中，加入乙酸乙酯，对二乙烯基苯和前述中间体，其中对二乙烯基苯和前述中间体摩尔比1:1，搅拌，将溶液以氮气脱气，然后加入偶氮二异丁腈引发剂，氮气流下，80℃加热搅拌24小时；冷却至室温，然后在乙醚中沉降，过滤，过滤得到的固体微粒使用乙醇洗涤3次；真空干燥，得到白色微粒产物；100重量份白色微粒经加料口加入单螺杆挤出机中，控制口模温度100℃，压力为11MPa；通过安装在挤出机机筒上的发泡剂注入口注入15重量份发泡剂液态二氧化碳；然后经直径3mm的圆孔口模挤出、切粒、冷却得到产物发泡珠粒。
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