CN106832391B - 一种抑制浸渍树脂萃取剂流失的方法 - Google Patents

一种抑制浸渍树脂萃取剂流失的方法 Download PDF

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CN106832391B
CN106832391B CN201710068479.6A CN201710068479A CN106832391B CN 106832391 B CN106832391 B CN 106832391B CN 201710068479 A CN201710068479 A CN 201710068479A CN 106832391 B CN106832391 B CN 106832391B
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王俊莲
谢美英
刘新宇
王化军
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Abstract

本发明提供一种抑制浸渍树脂萃取剂流失的方法，属于材料制备技术领域。该方法在浸渍树脂制备过程中加入低分子量直链聚合物或低交联度的聚合物，使萃取剂和聚合物在有机溶剂中充分溶解混匀，在旋转蒸发除去溶剂的过程中，萃取剂和聚合物交叉吸附到大孔树脂基底表面，聚合物链像“绳子”一样将萃取剂“绑在”大孔树脂基底上，增强了萃取剂的稳定性。该方法可有效抑制萃取剂的流失，制备过程属于物理过程，操作非常简单。

Description

一种抑制浸渍树脂萃取剂流失的方法
技术领域
本发明涉及材料制备技术领域，特别是指一种抑制浸渍树脂萃取剂流失的方法。
背景技术
浸渍树脂的制备方法简单，高效，经济，支撑基底和萃取剂的性能可分别调控、任意匹配，且萃取剂吸附在基底的表面，便于金属离子与萃取剂接触，萃取达平衡时间相对较短，被广泛应用于稀有金属、贵金属、有色金属、稀土元素的提取、分离和回收。
然而，浸渍树脂是依靠萃取剂与支撑基底之间的范德华作用力相结合，该作用力较弱，萃取剂容易流失，造成浸渍树脂萃取容量降低，循环使用性能差。增强浸渍树脂稳定性的方法通常有两种：一种是用热水或是有机溶剂洗涤浸渍树脂，将浸渍树脂表面与大孔树脂基底作用力较弱的萃取剂分子洗掉，这种方法虽然降低了浸渍树脂使用过程中萃取剂的流失，增强了浸渍树脂的稳定性，但总体上还是造成了萃取剂的浪费；另外一种方法是利用交联反应在浸渍树脂的表面包裹一层亲水性薄膜，使萃取剂被束缚在薄膜里，该方法可有效抑制萃取剂的流失，但会降低浸渍树脂的饱和负载量，水相中的离子要穿过包裹的亲水性薄膜才能与浸渍树脂表面的萃取剂结合，延长了萃取达平衡时间，且包裹PVA交联反应属于化学反应过程，增加了制备步骤。
发明内容
本发明要解决的技术问题是提供一种抑制浸渍树脂萃取剂流失的方法，其核心是在浸渍树脂制备过程中加入低分子量直链聚合物或低交联度的聚合物，使萃取剂和聚合物在有机溶剂中充分溶解混匀，在旋转蒸发除去溶剂的过程中，萃取剂和聚合物交叉吸附到大孔树脂基底表面，聚合物链像“绳子”一样将萃取剂“绑在”大孔树脂基底上，增强了萃取剂的稳定性。
该方法在浸渍树脂制备过程中加入低分子量直链聚合物或低交联度的聚合物，具体步骤如下：
(1)将萃取剂溶于有机溶剂中，加入低分子量直链聚合物或低交联度的聚合物，超声振荡或加热使低分子量直链聚合物或低交联度的聚合物溶解；
(2)加入具有多孔结构的聚合物支撑基底，浸渍1-48h；
(3)用旋转蒸发仪将有机溶剂去除。
其中，萃取剂为二(2-乙基己基)磷酸酯(P204)、2-乙基己基磷酸-2-乙基己基酯(P507)、二(2,4,4’-三甲基戊基)次膦酸(Cyanex 272)、Cyanex 572、二(2,3-二甲基丁基)次膦酸、二(2-乙基己基)次膦酸、(2,3-二甲基丁基)(2,4,4’-三甲基戊基)次膦酸、磷酸三丁酯、三正辛基氧膦、Cyanex 923、二(2,4,4’-三甲基戊基)二硫代膦酸(Cyanex 301)、二(2,4,4’-三甲基戊基)一硫代膦酸(Cyanex 302)、N,N,N’,N’-四(2-乙基己基)二乙醇酰胺、四乙基二乙醇酰胺、3-羟基-2-萘甲酸、8-羟基喹啉及其二卤代衍生物、双硫腙、水杨酸、2-羟基-5-壬基苯甲醛肟、5,8-二乙基-7-羟基-十二烷基-6-铜肟(LIX63)、LIX 54、CyphosIL101、仲辛基苯氧基乙酸中的一种或一种以上。
有机溶剂为乙醇、异丙醇、正丁醇、丙酮、甲乙酮、N,N-二甲基甲酰胺、四氢呋喃、1,4-二氧六环、甲苯、二甲苯、苯、氯仿、二氯甲烷、正己烷、环己烷、正辛烷、石油醚、二甲亚砜中、2-甲氧基乙醇的一种或一种以上。
低分子量直链聚合物或低交联度的聚合物为以苯乙烯、甲基丙烯酸、甲基丙烯酸甲酯、甲基丙烯酸乙酯、甲基丙烯酸羟乙酯、甲基丙烯酸丙酯、甲基丙烯酸丁酯、丙烯酸、丙烯酸甲酯、丙烯酸乙酯、丙烯酸羟乙酯、丙烯酸丙酯、丙烯酸羟丙酯、丙烯酸丁酯、丙烯酸异丁酯、丙烯酸叔丁酯、丙烯酸异辛酯、4-乙烯基吡啶、丙烯腈、丙烯酰胺中的一种或一种以上为单体制备的重均分子量介于5000-55000之间的直链聚合物，或以上述烯烃为单体，以二乙烯基苯、二甲基丙烯酸乙二醇酯、N,N’-亚甲基双丙烯酰胺中的一种或一种以上为交联剂，制备的重均分子量介于5000-55000之间且交联度小于10％的聚合物。
步骤(2)中的具有多孔结构的聚合物支撑基底为苯乙烯-二乙烯基苯聚合物颗粒、丙烯酸酯聚合物颗粒、甲基丙烯酸酯聚合物颗粒、酚醛树脂颗粒、丙烯酰胺聚合物颗粒，如XAD-2、XAD-4、XAD-7HP、XAD-8、XAD-16、XAD-1180、XAD-2000、XAD-2010、XAD-761、HZ830、HPD800、Diaion HP2MG、Chromosorb-W。
步骤(1)中有机溶剂质量为萃取剂质量的1-50倍，低分子量直链聚合物或低交联度的聚合物质量为萃取剂质量的0.1-10％，步骤(2)中具有多孔结构的聚合物支撑基底质量为萃取剂质量的0.5-3倍。
本发明的上述技术方案的有益效果如下：
该方法不仅可有效抑制萃取剂的流失，且操作非常简单，与浸渍树脂的制备过程融为一体，无需另外的操作，还可通过改变加入的低分子量直链聚合物或低交联度聚合物的量和性质来调节浸渍树脂的性能，如稳定性、亲疏水性等。
具体实施方式
为使本发明要解决的技术问题、技术方案和优点更加清楚，下面将结合具体实施例进行详细描述。
本发明提供一种抑制浸渍树脂萃取剂流失的方法。
实施例1
(1)向250mL单口烧瓶中加入80mL乙醇、5g Cyanex 572、0.05g重均分子量26769、多分散系数为1.26、交联度为2％的苯乙烯-二乙烯基苯聚合物，超声振荡使其溶解。
(2)加入5g大孔树脂支撑物基底XAD-16，浸渍24h，使大孔树脂充分溶胀。
(3)用旋转蒸发仪除去乙醇，得到萃取剂不易流失的浸渍树脂。
实施例2
(1)向250mL单口烧瓶中加入120mL丙酮、10g LIX 63、0.5g重均分子量38962、多分散系数为1.17，甲基丙烯酸甲酯-丙烯酸丁酯共聚物，超声振荡使其溶解。
(2)加入15g大孔树脂支撑物基底XAD-7HP，浸渍42h，使大孔树脂充分溶胀。
(3)用旋转蒸发仪除去丙酮，得到稳定性得到强化的浸渍树脂。
实施例3
(1)向250mL单口烧瓶中加入150mL二甲苯、6g水杨酸、0.2g重均分子量8037、多分散系数为1.15、交联度8％丙烯酸甲酯-甲基丙烯酸丁酯-二甲基丙烯酸乙二醇酯共聚物，加热到60℃使其溶解。
(2)加入10g大孔树脂支撑物基底Diaion HP2MG，浸渍35h，使大孔树脂充分溶胀。
(3)用旋转蒸发仪除去二甲苯，得到负载水杨酸的稳定性得到强化的浸渍树脂。
以上所述是本发明的优选实施方式，应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明所述原理的前提下，还可以做出若干改进和润饰，这些改进和润饰也应视为本发明的保护范围。

Claims (4)

1.一种抑制浸渍树脂萃取剂流失的方法，其特征在于：在浸渍树脂制备过程中加入低分子量直链聚合物或低交联度的聚合物，具体步骤如下：
(1)将萃取剂溶于有机溶剂中，加入低分子量直链聚合物或低交联度的聚合物，超声振荡或加热使低分子量直链聚合物或低交联度的聚合物溶解；
(2)加入具有多孔结构的聚合物支撑基底，浸渍1-48h；
(3)用旋转蒸发仪将有机溶剂去除；
所述步骤(1)中的低分子量直链聚合物或低交联度的聚合物为以苯乙烯、甲基丙烯酸、甲基丙烯酸甲酯、甲基丙烯酸乙酯、甲基丙烯酸羟乙酯、甲基丙烯酸丙酯、甲基丙烯酸丁酯、丙烯酸、丙烯酸甲酯、丙烯酸乙酯、丙烯酸羟乙酯、丙烯酸丙酯、丙烯酸羟丙酯、丙烯酸丁酯、丙烯酸异丁酯、丙烯酸叔丁酯、丙烯酸异辛酯、4-乙烯基吡啶、丙烯腈、丙烯酰胺中的一种以上为单体制备的重均分子量介于5000-55000之间的直链聚合物，或以上述烯烃为单体，以二乙烯基苯、二甲基丙烯酸乙二醇酯、N,N’-亚甲基双丙烯酰胺中的一种以上为交联剂，制备的重均分子量介于5000-55000之间且交联度小于10％的聚合物；
所述步骤(1)中有机溶剂质量为萃取剂质量的1-50倍，所述的低分子量直链聚合物或低交联度的聚合物质量为萃取剂质量的0.1-10％，所述步骤(2)中具有多孔结构的聚合物支撑基底质量为萃取剂质量的0.5-3倍。
2.根据权利要求1所述的抑制浸渍树脂萃取剂流失的方法，其特征在于：所述步骤(1)中萃取剂为二(2-乙基己基)磷酸酯(P204)、2-乙基己基磷酸-2-乙基己基酯(P507)、二(2,4,4’-三甲基戊基)次膦酸(Cyanex 272)、Cyanex 572、二(2,3-二甲基丁基)次膦酸、二(2-乙基己基)次膦酸、(2,3-二甲基丁基)(2,4,4’-三甲基戊基)次膦酸、磷酸三丁酯、三正辛基氧膦、Cyanex 923、二(2,4,4’-三甲基戊基)二硫代膦酸(Cyanex 301)、二(2,4,4’-三甲基戊基)一硫代膦酸(Cyanex 302)、N,N,N’,N’-四(2-乙基己基)二乙醇酰胺、四乙基二乙醇酰胺、3-羟基-2-萘甲酸、8-羟基喹啉及其二卤代衍生物、双硫腙、水杨酸、2-羟基-5-壬基苯甲醛肟、5,8-二乙基-7-羟基-十二烷基-6-铜肟(LIX63)、LIX54、CyphosIL101、仲辛基苯氧基乙酸中的一种以上。
3.根据权利要求1所述的抑制浸渍树脂萃取剂流失的方法，其特征在于：所述步骤(1)中的有机溶剂为乙醇、异丙醇、正丁醇、丙酮、甲乙酮、N,N-二甲基甲酰胺、四氢呋喃、1,4-二氧六环、甲苯、二甲苯、苯、氯仿、二氯甲烷、正己烷、环己烷、正辛烷、石油醚、二甲亚砜、2-甲氧基乙醇中 的一种以上。
4.根据权利要求1所述的抑制浸渍树脂萃取剂流失的方法，其特征在于：所述步骤(2)中的具有多孔结构的聚合物支撑基底为苯乙烯-二乙烯基苯聚合物颗粒、丙烯酸酯聚合物颗粒、甲基丙烯酸酯聚合物颗粒、酚醛树脂颗粒、丙烯酰胺聚合物颗粒。
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