CN114917882A - 一种高效提钪微球及其制备方法和应用 - Google Patents
一种高效提钪微球及其制备方法和应用 Download PDFInfo
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- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/265—Synthetic macromolecular compounds modified or post-treated polymers
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- B01J20/28021—Hollow particles, e.g. hollow spheres, microspheres or cenospheres
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Abstract
本发明涉及湿法冶金领域,公开了一种高效提钪微球及其制备方法和应用,制备方法包括如下步骤,在100份水中加入1‑5份均质剂,0.1‑2份助剂,搅拌,加入5‑30份活性组分,2‑10份塑球组分、搅拌后升温至60℃加入0.5‑3份引发剂,反应4小时,加入0.5‑2份固化剂,待微球形成,升温至80℃进行固化,待固化完成后即得尺寸均一的提钪微球。将提钪微球装柱,加入含钪料液进行循环吸附,对吸附完成的提钪微球进行洗脱,得到富钪溶液,蒸发结晶得到氯化钪产品,钪综合回收率可达85%以上,氯化钪产品纯度高达99%以上。本发明绿色环保,工艺流程简单,对钪离子的交换速率快、吸附率高、吸附选择性好,可实现钪回收的产业化。
Description
技术领域
本发明属于湿法冶金领域,尤其涉及一种高效提钪微球及其制备方法和应用。
背景技术
钪是一种过渡金属元素,它的元素符号是Sc,原子序数是21,是一种质软、银白色的金属。常跟稀土矿石混合存在,比如黑稀金矿。在一些锡、钨矿中也含有钪,在钪钇石中含量较高。钪因其自身特殊物理、化学性质,已用于制备铝钪合金、燃料电池、钪钠卤灯、示踪剂、激光晶体等产品,在特种钢铁、有色合金、高性能陶瓷、催化剂等领域有着广阔的应用前景。
目前,钪的提取方法有溶剂萃取法、离子交换法、沉淀法、液膜萃取法、升华法等等。溶剂萃取法的应用非常广泛,在湿法冶金、化工、医药等工业生产中都有溶剂萃取方法的使用。溶剂萃取法具有分离效果好、分离效率高、金属回收率高、设备简单易于生产。离子交换就是利用离子交换剂功能团中的阳离子或阴离子与溶液中同性离子进行可逆交换反应的方法。采用离子交换法可以从水溶液中提取有价金属或是净化溶液。离子交换法处理不了浓溶液,因为离子交换树脂容量有限。但其没有萃取法中萃取剂的夹带、乳化、溶解及有机溶剂的气味问题。
自20世纪70年代以来,我国科技工作者根据我国钪资源条件提出并研发了多种钪提取工艺,取得了突破性进展。钪提取涉及多个过程,涉及原料富集、浸出、除杂、制取粗氧化钪,再经过纯化得到纯氧化钪。一般钪的提取运用的是湿法冶金技术,如从氯化烟尘中提钪,先用水或是酸浸出烟尘,之后用萃取剂萃取回收钪。虽然钪提取技术有了很大提高,但就目前而言还存在成本高、回收率低和冶金废液难处理等技术问题。故研制一种高效绿色的提钪材料就显得尤为重要。
发明内容
本发明基于现有提钪技术的现状,特提出一种高效提钪微球及其制备方法和应用,以改善提钪过程中的污染高、收率低、能耗大的问题。
本发明提出了一种高效提钪微球,制备方法包括如下步骤,在100份水中加入1-5份均质剂,0.1-2份助剂,搅拌,加入5-30份活性组分,2-10份塑球组分、搅拌后升温至60℃加入0.5-3份引发剂,反应4小时后,加入0.5-2份固化剂,待微球形成,升温至80℃进行固化,待固化完成后即得尺寸均一的提钪微球。
优选地,上述的一种高效提钪微球,所述的活性组分为二(2-乙基己基)磷酸、2-乙基己基膦酸单(2-乙基己基)酯、二(2-乙基己基)膦酸、异丙基膦酸单(1-己基-4-乙基)辛基酯、二(2,4,4-三甲基戊基)膦酸、二(2,4,4-三甲基戊基)硫代膦酸、二(2,4,4-三甲基戊基)二硫代膦酸中的一种或两种复配。
优选地,上述的一种高效提钪微球,所述的均质剂为十二烷基苯磺酸钠、十二烷基磺酸钠、吐温系列、司班系列中的一种或两种以上的混合。
优选地,上述的一种高效提钪微球,所述的助剂为[Cnmim][ReO4]或[CnPy][ReO4],其中,n=2-8。
优选地,上述的一种高效提钪微球,所述的引发剂为叔丁基过氧化氢、过硫酸钾、偶氮二异丁腈、过氧化甲乙酮中的一种或两种以上的混合。
优选地,上述的一种高效提钪微球,所述的固化剂为聚酰胺、叔胺盐、二乙基氨基丙胺、双氰胺中的一种或两种以上的混合。
优选地,上述的一种高效提钪微球,所述的塑球组分为苯乙烯、脲醛树脂预聚物、甲基丙烯酸甲酯、酚醛树脂预聚物中的一种或两种以上的混合。
一种高效提钪微球在吸附钪中的应用,将上述的提钪微球装柱,加入含钪料液进行循环吸附,使用洗脱剂对吸附完成的提钪微球进行洗脱,从而得到富钪溶液,蒸发结晶得到氯化钪。
优选地,上述的一种高效提钪微球在吸附钪中的应用,所述的洗脱剂为5-15wt%的钪捕获剂。
优选地,上述的一种高效提钪微球在吸附钪中的应用,所述的钪捕获剂为硫酸、硝酸、盐酸中的一种或两种的组合。
本发明的有益效果是:本发明针对现有提钪技术存在的各种弊端,发明一种高效提钪微球的制备方法。常规方法需要长时间的蒸发浓缩或是萃取存在污染环境的有机溶剂。本发明的工艺流程简单,易于大规模生产,化工材料常见且消耗低,能有效地降低提钪成本,产品纯度高,钪的总回收率高达85%以上,所用试剂环境友好,具有明显的社会效益和经济效益。
具体实施方式
下面以具体的实施例进一步说明本发明的内容,但不应理解为对本发明的限制,在不背离本发明精神和实质的情况下,对本发明方法、步骤或者条件等所做修改或替换,均应涵盖在本发明的权利要求范围当中。
实施例1一种高效提钪微球及应用
1、提钪微球的制备:在反应釜中加入100份的水,然后加入2份均质剂十二烷基磺酸钠和0.5份助剂[C5mim][ReO4],搅拌30分钟后,加入10份活性组分二(2-乙基己基)磷酸,酚醛树脂预聚物4份、搅拌10分钟后升温至60℃加入1份引发剂过氧化甲乙酮,反应4小时后,加入固化剂二乙基氨基丙胺1份,待微球形成,然后升温至70℃进行固化,待固化完成后收集产品,即得尺寸均一的提钪微球。
2、装柱吸附:将提钪微球装入离子交换柱内,含钪料液作为流动相,进行过柱吸附工艺,同出口液体流速控制在8BV/h;
3、解吸:向装有完成吸附的提钪微球中加入5wt%的盐酸洗脱剂,控制流速为10BV/h。
4、蒸发结晶:将富钪洗脱液在80℃下蒸发浓缩、静置结晶,沉淀母液返回吸附工艺;将晶体过滤后重结晶提纯,获得氯化钪产品。
5、检测:吸附后含钪料液使用电感耦合等离子光谱仪检测钪元素含量为23.77mg/L,产品纯度99.27%。
实施例2一种高效提钪微球及应用
1、提钪微球的制备:在反应釜中加入100份的水,然后加入3份均质剂十二烷基磺酸钠和1份助剂[C5Py][ReO4],搅拌30分钟后,加入15份活性组分二(2-乙基己基)膦酸,塑球组分脲醛树脂预聚物6份、搅拌10分钟后升温至60℃加入1.5份引发剂过氧化甲乙酮,反应4小时后,加入固化剂二乙基氨基丙胺1份,待微球形成,然后升温至75℃进行固化,待固化完成后收集产品,即得尺寸均一的提钪微球。
2、装柱吸附:将提钪微球装入离子交换柱内,含钪料液作为流动相,进行过柱吸附工艺,同出口液体流速控制在8BV/h;
3、解吸:向装有完成吸附的提钪微球中加入7wt%的盐酸洗脱剂,控制流速为10BV/h。
4、蒸发结晶:将富钪洗脱液在80℃下蒸发浓缩、静置结晶,沉淀母液返回吸附工艺;将晶体过滤后重结晶提纯,获得氯化钪产品。
5、检测:吸附后含钪料液使用电感耦合等离子光谱仪检测钪元素含量为36.34mg/L,产品纯度99.48%。
实施例3一种高效提钪微球及应用
1、提钪微球的制备:在反应釜中加入100份的水,然后加入1份均质剂吐温-20和司班-80(比例1:1),1.5份助剂[C6mim][ReO4],搅拌30分钟后,加25份活性组分二(2,4,4-三甲基戊基)硫代膦酸,塑球组分苯乙烯10份、搅拌10分钟后升温至60℃加入2份引发剂过氧化甲乙酮,反应4小时后,加入固化剂二乙基氨基丙胺1.5份,待微球形成,然后升温至80℃进行固化,待固化完成后收集产品,即得尺寸均一的提钪微球。
2、装柱吸附:将提钪微球装入离子交换柱内,含钪料液作为流动相,进行过柱吸附工艺,同出口液体流速控制在8BV/h;
3、解吸:向装有完成吸附的提钪微球中加入10wt%的盐酸洗脱剂,控制流速为10BV/h。
4、蒸发结晶:将富钪洗脱液在80℃下蒸发浓缩、静置结晶,沉淀母液返回吸附工艺;将晶体过滤后重结晶提纯,获得氯化钪产品。
5、检测:吸附后含钪料液使用电感耦合等离子光谱仪检测钪元素含量为21.87mg/L,产品纯度99.63%。
吸附后含钪料液中钪元素的含量以及氯化钪产品纯度见表1:
表1.吸附后含钪料液中钪元素的含量以及氯化钪产品纯度
Claims (10)
1.一种高效提钪微球,其特征在于:制备方法包括如下步骤,在100份水中加入1-5份均质剂,0.1-2份助剂,搅拌,加入5-30份活性组分,2-10份塑球组分、搅拌后升温至60℃加入0.5-3份引发剂,反应4小时后,加入0.5-2份固化剂,待微球形成,升温至70-80℃进行固化,待固化完成后即得尺寸均一的提钪微球。
2.根据权利要求1所述的一种高效提钪微球,其特征在于:所述的活性组分为二(2-乙基己基)磷酸、2-乙基己基膦酸单(2-乙基己基)酯、二(2-乙基己基)膦酸、异丙基膦酸单(1-己基-4-乙基)辛基酯、二(2,4,4-三甲基戊基)膦酸、二(2,4,4-三甲基戊基)硫代膦酸、二(2,4,4-三甲基戊基)二硫代膦酸中的一种或两种复配。
3.根据权利要求1所述的一种高效提钪微球,其特征在于:所述的均质剂为十二烷基苯磺酸钠、十二烷基磺酸钠、吐温系列、司班系列中的一种或两种以上的混合。
4.根据权利要求1所述的一种高效提钪微球,其特征在于:所述的助剂为[Cnmim][ReO4]或[CnPy][ReO4],其中,n=2-8。
5.根据权利要求1所述的一种高效提钪微球,其特征在于:所述的引发剂为叔丁基过氧化氢、过硫酸钾、偶氮二异丁腈、过氧化甲乙酮中的一种或两种以上的混合。
6.根据权利要求1所述的一种高效提钪微球,其特征在于:所述的固化剂为聚酰胺、叔胺盐、二乙基氨基丙胺、双氰胺中的一种或两种以上的混合。
7.根据权利要求1所述的一种高效提钪微球,其特征在于:所述的塑球组分为苯乙烯、脲醛树脂预聚物、甲基丙烯酸甲酯、酚醛树脂预聚物中的一种或两种以上的混合。
8.一种高效提钪微球在吸附钪中的应用,其特征在于:将权利要求1-7任一项所述的提钪微球装柱,加入含钪料液进行循环吸附,使用洗脱剂对吸附完成的提钪微球进行洗脱,从而得到富钪溶液,蒸发结晶得到氯化钪。
9.根据权利要求1所述的一种高效提钪微球在吸附钪中的应用,其特征在于:所述的洗脱剂为5-15wt%的钪捕获剂。
10.根据权利要求9所述的一种高效提钪微球在吸附钪中的应用,其特征在于:所述的钪捕获剂为硫酸、硝酸、盐酸中的一种或两种的组合。
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