CN116371367A - 一种基于含铀废水处理的无机有机杂化材料及其制备方法和应用 - Google Patents
一种基于含铀废水处理的无机有机杂化材料及其制备方法和应用 Download PDFInfo
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Abstract
本发明涉及一种基于含铀废水处理的无机有机杂化材料及其制备方法和应用,属于吸附材料领域。采用水热法制备出具有开放骨架结构的无机有机钒氧层状杂化材料,对铀具有优异的离子交换性能,表现为离子交换速率快、吸附容量高、分配系数高、pH适用范围广等特点。本发明的吸附材料解决了传统吸附材料吸附动力学慢、选择性差、pH适用范围窄的缺点,拓展了吸附材料的应用环境。
Description
发明领域
本发明涉及含铀废水的离子交换型材料的制备及应用,属于吸附材料领域。
背景技术
矿物开采、加工处理过程中产生的含有高水平天然放射性核素的废物的数量巨大,需要采取不同的管理方式。通常,铀矿冶的废石、尾矿中放射性核素主要以地表水和地下水为载体迁移到生态环境中,具有隐蔽性强、滞留时间长、污染物迁移途径复杂等特点,给人类生存带来了严重威胁。开发匹配用于处理含铀放射性废水的技术迫在眉睫。目前的吸附材料pH适用范围窄,吸铀动力学差,选择性能力不足,制约着吸附材料的规模化应用。
发明内容
为了解决上述问题,本发明提出一种基于含铀废水处理的无机有机钒氧层状杂化材料及其制备方法和应用。本发明制备的钒氧层状化合物对铀具有优异的离子交换性能,表现为离子交换速率快、吸附容量高、分配系数高、pH适用范围广等特点。本发明是对目前离子交换型材料处理放射性核素的重要革新。
本发明的目的之一是提供一种基于含铀废水处理的无机有机杂化材料,以解决吸附材料对废水中铀去除效果不理想的问题。所述所述无机有机杂化材料的化学式为[(CH3)2NH2]V3O7,空间群为P21。
本发明还提供了一种所述无机有机钒氧层状杂化材料的制备方法,包括以下步骤:
(5)将步骤(4)的反应物去除上清液,置于离心管中,加入丙酮,离心洗涤3次,加入去离子水离心洗涤3次,获得黑色固体,并将黑色固体置于80 ℃的烘箱中,干燥12 h,获得无机有机钒氧层状杂化材料。
优选的,所述步骤(1)中五氧化二钒、一水氢氧化锂、去离子水的摩尔比为1:1.2:110。
优选的,步骤(2)中,所述澄清溶液与N,N-二甲基甲酰胺的体积比为8~12:1。
优选的,步骤(3)中,pH的调节范围为4.5~6。
优选的,步骤(4)中,水热反应的温度为180~200℃。
进一步的,所述无机有机杂化材料的空间群为P21。
本发明的有益效果是:
本发明制备的无机有机层状杂化材料,具有开放的层状骨架结构,骨架结构中的有机胺离子[CH3NH3]+可与铀发生离子交换,饱和吸附容量为156mg/g,最大分配系数为kd U=6.06×106mL/g,离子响应速率小于20min,pH适用范围为3~9。采用2mol/L的KCl溶液可对铀进行洗脱,洗脱后晶体结构保持不变。
附图说明
图1为本发明实施案例1制备的无机有机钒氧层状杂化材料的晶体结构图。
图2为本发明实施案例1制备的无机有机钒氧层状杂化材料的XRD图谱。
图3为本发明实施案例1制备的无机有机钒氧层状杂化材料的Raman图谱。
图4为本发明实施案例1制备的无机有机钒氧层状杂化材料离子交换后的的扫描图。
图5为本发明实施案例1制备的无机有机钒氧层状杂化材料离子交换后的能谱图。
图6本发明实施案例1制备的无机有机钒氧层状杂化材料的吸附容量曲线。
图7本发明实施案例1制备的无机有机钒氧层状杂化材料的吸附前后的XRD图谱。
具体实施方式
下面将结合本发明实施例,对本发明的技术方案进行清楚地阐述。应理解,这些实施例仅用于说明本发明而不用于限制本发明的范围。
实施例1
(1)称取五氧化二钒3.64g,一水氢氧化锂1.68g,置于40mL的去离子水中,磁力搅拌4h后溶解,获得黄色澄清溶液。
(2)在步骤(1)所得的澄清溶液中滴加4mL的N,N-二甲基甲酰胺,磁力搅拌2h,获得黄绿色溶液。
(3)将步骤(2)所得的溶液,采用醋酸调节pH至5,磁力搅拌1h,获得紫红色澄清溶液。
(4)将步骤(3)所得溶液转移至装有100mL聚四氟乙烯的反应釜中,置于的烘箱中,在190℃的条件下反应4天。
(5)将步骤(4)的反应物去除上清液,置于100mL的离心管中,加入20ml丙酮,离心洗涤3次,加入去离子水离心洗涤3次,获得黑色固体。并将黑色固体置于80℃的烘箱中,干燥12h,获得无机有机钒氧层状杂化材料。
本实施案例使用模拟放射性含铀废水的铀浓度为40ppm,pH值为6.0。吸附性能测试中,投料比为1:1000(),铀的饱和吸附容量为156mg/g。离子分配系数为kd U=6.06×106mL/g,离子响应速率小于20min。采用2mol/L的KCl溶液可以完成对铀的洗脱,洗脱后晶体结构保持不变。
实施例2
(1)称取五氧化二钒5.46、一水氢氧化锂2.52g,置于60mL的去离子水中,磁力搅拌4h后溶解,获得黄色澄清溶液。
(2)在步骤(1)所得的澄清溶液中滴加5mL的N,N-二甲基甲酰胺,磁力搅拌2h,获得黄绿色溶液。
(3)将步骤(2)所得的溶液,采用醋酸调节pH至6,磁力搅拌1h,获得紫红色澄清溶液。
(4)将步骤(3)所得的溶液转移至装有100mL的聚四氟乙烯的反应釜中,置于的烘箱中,在185℃的条件下反应4天。
(5)将步骤(4)中反应物去除上清液,置于100mL的离心管中,加入50ml丙酮,离心洗涤3次,加入去离子水离心洗涤3次,获得黑色固体。并将黑色固体置于80℃的烘箱中,干燥12h,获得无机有机钒氧层状杂化材料。
本实施案例使用模拟放射性含铀废水的铀浓度为40ppm,pH值为8.0。吸附性能测试中,投料比为1:100(体积比),铀的饱和吸附容量为132mg/g。离子分配系数为kd U=5.06×106mL/g,离子响应速率小于35min。采用2mol/L的KCl溶液可以完成对铀的洗脱,洗脱后晶体结构保持不变。
Claims (7)
1.一种基于含铀废水处理的无机有机杂化材料,其特征在于,所述无机有机杂化材料的化学式为[(CH3)2NH2]V3O7。
2.根据权利要求1所述的无机有机杂化材料,其特征在于,所述无机有机杂化材料的制备方法,包括以下步骤:
(1)称取五氧化二钒、一水氢氧化锂置于去离子水中,磁力搅拌4h后溶解,获得黄色澄清溶液;
(2)在步骤(1)所得的澄清溶液中滴加N,N-二甲基甲酰胺,磁力搅拌2h,获得黄绿色溶液;
(3)将步骤(2)所得的溶液,采用醋酸调节pH至弱酸性后,磁力搅拌1h,获得紫红色澄清溶液;
(4)将步骤(3)所得溶液转移至装有聚四氟乙烯内胆的反应釜中,置于烘箱中,反应4天;
(5)将步骤(4)的反应物去除上清液,置于离心管中,加入丙酮,离心洗涤3次,加入去离子水离心洗涤3次,获得黑色固体,并将黑色固体置于80℃的烘箱中,干燥12h,获得无机有机钒氧层状杂化材料。
3.根据权利要求2所述的无机有机杂化材料,其特征在于,所述步骤(1)中五氧化二钒、一水氢氧化锂、去离子水的摩尔比为1:1.2:110。
4.根据权利要求2所述的无机有机杂化材料,其特征在于,所述步骤(2)中,所述澄清溶液与N,N-二甲基甲酰胺的体积比为8~12:1。
5.根据权利要求2所述的无机有机杂化材料,其特征在于,所述步骤(3)中pH的调节范围为4.5~6。
6.根据权利要求2所述的无机有机杂化材料,其特征在于,所述步骤(4)中的水热反应温度为180~200℃。
7.根据权利要求1-6任一项所述的无机有机杂化材料,其特征在于,所述无机有机杂化材料的空间群为P21。
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