CN117385179A - 一种分离靶件中In和Cd的方法 - Google Patents
一种分离靶件中In和Cd的方法 Download PDFInfo
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Abstract
本发明公开了一种分离靶件中In和Cd的方法,属于同位素药物制备技术领域。本发明首先将靶件真空加热,蒸馏除去Cd和Zn的混合物,得到靶件基底,把所述Cd和Zn的混合物放入碱液内碱浸得到碱浸液,对所述碱浸液过滤,得到的滤渣为Cd,所述靶件基底中含In。然后将所述靶件基底放入酸液进行酸浸得到酸浸液,对所述酸浸液过滤,得到含In的滤液,所述酸液为有机酸或非氧化性无机酸。最后将所述滤液使用树脂吸附、萃取或蒸馏的方法纯化得到In。本发明通过对靶件真空加热,有效利用Cu、Cd、In、Zn的沸点差异的原理,直接将Cd和Zn的混合物除去,实现In和Cd的分离,分离效率高,且属于物理分离,对In和Cd的损失较少。
Description
技术领域
本发明属于同位素药物制备技术领域,具体涉及一种分离靶件中In和Cd的方法。
背景技术
111In的半衰期为2.83 d,通过电子俘获衰变能释放能量为173 keV和247kev的两种γ射线,可用作诊断用放射性同位素,111In标记放射性药物主要用于肿瘤显像。111In的生产方法主要有三种:(1)通过回旋加速器产生质子轰击112Cd获得,要求质子流的能量为16~22MeV;(2)通过回旋加速器产生质子轰击111Cd 获得,要求质子流的能量为4~15MeV;(3)通过α粒子击109Ag获得,要求α粒子流的能量为15~30 MeV。实际制备中,综合粒子流能量、成本等因素考虑,主要使用方法(1)和(2)。
111In制备时,首先将经同位素富集后的Cd镀在高纯铜箔上(Cd镀层厚度控制在20-100μm,铜箔厚度为10-15μm),即可制备成靶件。然后,利用回旋加速器产生质子,轰击靶件即可得到一定量的111In,得到的111In还在靶件上,需要将In与Cd分离。现有在靶件中分离In和Cd的常见工艺为:首先使靶件经HNO3与Fe3+溶解,再将游离的In3+与Fe3+共沉淀(硝酸过量,溶液中铁离子以Fe3+为主);过滤,得到滤饼与滤液,滤液用来重新回收Cd同位素;滤饼为Fe与In的沉淀物,使用HBr酸溶解滤饼;用萃取剂(如二异丙基醚,DIPE)萃取In数次,后用HCl反萃;蒸馏除去盐酸中的萃取剂,后用离子交换树脂吸附可得到纯化后的In。由于靶件中还有Cu和Zn元素,需要进一步处理,分离步骤较繁琐。综上可知,现有的工艺选择性差,除杂流程长,In、Cd同位素损失率高,成本较高。
发明内容
针对上述不足,本发明提供一种分离靶件中In和Cd的方法,该方法选择性好,分离流程少,In、Cd同位素损失率低,有效降低成本。
本发明保护一种分离靶件中In和Cd的方法,该方法包括如下步骤:
将靶件真空加热,蒸馏除去Cd和Zn的混合物,得到靶件基底,把所述Cd和Zn的混合物放入碱液内碱浸得到碱浸液,对所述碱浸液过滤,得到的滤渣为Cd,所述靶件基底中含In。
将所述靶件基底放入酸液进行酸浸得到酸浸液,对所述酸浸液过滤,得到含In的滤液,所述酸液为有机酸或非氧化性无机酸。
将所述滤液使用树脂吸附、萃取或蒸馏的方法纯化得到In。
进一步地,所述真空加热的次数为两次,分别为第一次真空加热和第二次真空加热,能将所述Cd和Zn的混合物彻底去除。
进一步地,所述第一次真空加热的真空度为10~30Pa,所述第一次真空加热的温度为700~900℃,所述第一次真空加热的时间为1~4 h。
进一步地,所述第二次真空加热的真空度为2~7Pa,所述第二次真空加热的温度与所述第一次真空加热的温度相同,所述第二次真空加热的时间为1~3 h。
进一步地,所述碱液为NaOH溶液或KOH溶液,所述碱液的浓度为2~3 mol/L,所述碱浸的加热温度为35~80℃,所述碱浸的时间为0.5~1h。
进一步地,所述有机酸为乙酸或草酸。所述非氧化性无机酸选自硫酸、盐酸和氢溴酸中的一种。
进一步地,所述酸液的体积浓度为30%~80%,所述酸浸的温度为70~95℃,所述酸浸的搅拌速率为200~600 r/min,所述酸浸的时间为1~6 h。
进一步地,所述酸浸时加入双氧水,所述酸浸时加入双氧水,所述加入双氧水的量为双氧水与酸的比摩尔比为0.05~0.2:1。
进一步地,所述树脂吸附步骤选择的树脂为阳离子交换树脂或螯合树脂。
进一步地,所述萃取步骤的萃取剂选自中性萃取剂、胺类萃取剂和酸性萃取剂中的一种。
有益效果:
本发明通过对靶件真空加热,有效利用Cu、Cd、In、Zn的沸点差异的原理,直接将Cd和Zn的混合物除去,实现In和Cd的分离,分离效率高,且属于物理分离,对In和Cd的损失较少。本发明通过将Cd和Zn的混合物碱浸,能对Cd和Zn高效溶解和分离,对Cd重新回收利用,降低成本。本发明通过对靶件基底酸浸,利用在酸中溶解的电位不同,而将In选择性的溶解在酸液中,实现In和Cu的分离。本发明能将Cu、Cd、In和Zn四种元素有效分离,同时还能将In和Cd高纯度回收利用,另外,本发明中的分离方法步骤简短,选择性高,有效降低损失率和成本。
附图说明
为了更清楚地说明本发明实施例或现有技术中的技术方案,下面将对实施例或现有技术描述中所需要使用的附图作简单地介绍,显而易见地,下面描述中的附图仅仅是本发明的一些实施例,对于本领域普通技术人员来讲,在不付出创造性劳动的前提下,还可以根据这些附图获得其他的附图。
其中:
图1为本发明一个实施例中分离靶件中In和Cd的方法流程图。
具体实施方式
下面将结合本发明实施例,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
参考图1,本发明保护一种分离靶件中In和Cd的方法,该方法包括如下步骤:
将靶件真空加热,真空加热可以选择使用微型蒸馏装置,该装置由石英、氧化锆、氧化镁等材料制成,且具有冷端,便于蒸馏出金属的冷凝蒸馏。真空加热除去Cd和Zn的混合物,得到靶件基底,把Cd和Zn的混合物放入碱液内碱浸得到碱浸液,对碱浸液过滤,得到的滤渣为Cd,靶件基底中含In。
将靶件基底放入酸液进行酸浸得到酸浸液,对酸浸液过滤,得到含In的滤液,酸液为有机酸或非氧化性无机酸。
将滤液使用树脂吸附、萃取或蒸馏的方法纯化得到In。
本发明通过对靶件真空加热,有效利用Cu、Cd、In、Zn的沸点差异的原理,直接将Cd和Zn的混合物除去,实现In和Cd的分离,分离效率高,且属于物理分离,对In和Cd的损失较少。本发明通过将Cd和Zn的混合物碱浸,能对Cd和Zn高效溶解和分离,对Cd重新回收利用,降低成本。本发明通过对靶件基底酸浸,利用在酸中溶解的电位不同,而将In选择性的溶解在酸液中,实现In和Cu的分离。本发明能将Cu、Cd、In和Zn四种元素有效分离,同时还能将In和Cd高纯度回收利用,另外,本发明中的分离方法步骤简短,选择性高,有效降低损失率和成本。
在一个具体实施例中,真空加热的次数为两次,分别为第一次真空加热和第二次真空加热,能将Cd和Zn的混合物彻底去除。
在一个具体实施例中,第一次真空加热的真空度为10~30Pa,第一次真空加热的温度为700~900℃,第一次真空加热的时间为1~4 h。
在一个具体实施例中,第二次真空加热的真空度为2~7Pa,第二次真空加热的温度与第一次真空加热的温度相同,第二次真空加热的时间为1~3 h。
在一个具体实施例中,碱液为NaOH溶液或KOH溶液,碱液的浓度为2~3 mol/L,碱浸的加热温度为35~80℃,碱浸的时间为0.5~1h。
在一个具体实施例中,有机酸为乙酸或草酸。非氧化性无机酸选自硫酸、盐酸和氢溴酸中的一种。
在一个具体实施例中,酸液的体积浓度为30%~80%,酸浸的温度为70~95℃,酸浸的搅拌速率为200~600 r/min,酸浸的时间为1~6 h。
在一个具体实施例中,酸浸时加入双氧水,所述酸浸时加入双氧水,所述加入双氧水的量为双氧水与酸的比摩尔比为0.05~0.2:1。双氧水能加快靶件的溶解。
在一个具体实施例中,树脂吸附步骤选择的树脂为阳离子交换树脂或螯合树脂。
在一个具体实施例中,萃取步骤的萃取剂选自萃取剂为TBP等中性萃取剂,N235等胺类萃取剂,P507等酸性萃取剂。
以下为具体实施例。
由于本发明涉及的分离方法为元素分离,非同位素分离,即同一元素的不同同位素与另一元素的不同同位素分离均适用于本发明的工艺,故可用非放射性同位素做模拟冷实验,以代替真实放射性同位素分离实验。
实施例1
本实施例冷实验靶件,使用的Cd镀层中Cd为纯度为5N的高纯Cd,并掺有100 ppm的In、5 ppm的Zn,Cd涂层厚度20 μm;使用的Cu箔为纯度为6N的高纯Cu,厚度为10 μm。靶件总重量为500 mg。
将上述靶件放置于高纯石英托盘中,再将托盘放置在真空蒸馏炉中;先将高纯Ar气(纯度>6N)通入真空蒸馏炉中10 min后,关闭气体阀门,将真空蒸馏炉腔体抽至真空度为5 Pa;重复通入Ar气,并抽真空至5 Pa,重复该步骤三次。再次通入氩气,使炉腔体内压力保持在20 Pa。通电加热至750℃,并保温2 h;抽真空,将炉腔体内压力保持在5 Pa,并保温1h,该步骤中,冷凝段用循环水冷却,收集得到Cd、Zn冷凝物。取出靶件,将靶件置于80%的乙酸溶液中,加热至80℃,搅拌速率为300 r/min,保持6 h。过滤,得到滤液为含In的盐溶液,将滤液通过Dowex 1*4型树脂柱三次,并用0.05 mol/L的盐酸进行洗脱,洗脱后的溶液即为高纯度的含In溶液,滤渣为铜箔。上述Cd、Zn冷凝物取出后,置于3 mol/L的NaOH溶液中,加热溶解1 h,过滤,滤渣为Cd金属,滤液为Zn的盐溶液。
经检测,所得的In溶液中杂质总含量小于30 ppm,Zn含量低于20 ppm,杂质Cd含量低于15 ppm,杂质Cu含量低于10 ppm;回收Cd化学纯度大于99.9%,Cd回收率大于95%。
实施例2
本实施例冷实验靶件,使用的Cd镀层中Cd为纯度为5N的高纯Cd,并掺有100 ppm的In、5 ppm的Zn,Cd涂层厚度20 μm;使用的Cu箔为纯度为6N的高纯Cu,厚度为10 μm。靶件总重量为650 mg。
将上述靶件放置于高纯石英托盘中,再将托盘放置在真空蒸馏炉中;先将高纯Ar气(纯度>6N)通入真空蒸馏炉中10 min后,关闭气体阀门,将真空蒸馏炉腔体抽至真空度为5 Pa;重复通入Ar气,并抽真空至5 Pa,重复该步骤三次。再次通入氩气,使炉腔体内压力保持在20 Pa。通电加热至800℃,并保温3 h;抽真空,将炉腔体内压力保持在2 Pa,并保温1h,该步骤中,冷凝段用循环水冷却,收集得到Cd、Zn冷凝物。取出靶件,保持加入时草酸浓度为30%,加热至95℃,搅拌速率为400 r/min,保持6 h。过滤,得到滤液为含In的盐溶液,滤渣为铜箔。将滤液通过螯合类树脂柱三次,并用0.05 mol/L的盐酸进行洗脱,洗脱后的溶液即为高纯度的含In溶液,滤渣为铜箔。上述Cd、Zn冷凝物取出后,置于3 mol/L的NaOH溶液中,加热溶解1 h,过滤,滤渣为Cd金属,滤液为Zn的盐溶液。
经检测,所得的In溶液中杂质总含量小于200 ppm,Zn含量低于1 ppm,杂质Cd含量低于100 ppm,杂质Cu含量低于20 ppm;回收Cd化学纯度大于99.9%,Cd回收率大于96%。
实施例3
本实施例冷实验靶件,使用的Cd镀层中Cd为纯度为5N的高纯Cd,并掺有100 ppm的In、5 ppm的Zn,Cd涂层厚度20 μm;使用的Cu箔为纯度为6N的高纯Cu,厚度为10 μm。靶件总重量为500 mg。
将上述靶件放置于高纯氧化锆托盘中,再将托盘放置在真空蒸馏炉中;先将高纯Ar气(纯度>6N)通入真空蒸馏炉中10 min后,关闭气体阀门,将真空蒸馏炉腔体抽至真空度为5 Pa;重复通入Ar气,并抽真空至5 Pa,重复该步骤三次。再次通入氩气,使炉腔体内压力保持在20 Pa。通电加热至800℃,并保温2 h;抽真空,将炉腔体内压力保持在5 Pa,并保温1h,该步骤中,冷凝段用循环水冷却,收集得到Cd、Zn冷凝物。取出靶件,将靶件置于70%的乙酸溶液中,并加入相对于乙酸提及为10%的浓度为15%的双氧水,加热至90℃,搅拌速率为500 r/min,保持3 h。过滤,得到滤液为含In的盐溶液,使用P507萃取剂萃取溶液中的铟三次,并使用 1 mol/L的HCl酸进行反萃,即可得到In的盐溶液,滤渣为铜箔。上述Cd、Zn冷凝物取出后,置于2 mol/L的KOH溶液中,加热溶解0.5 h,过滤,滤渣为Cd金属,滤液为Zn的盐溶液。
经检测,所得的In溶液中杂质总含量小于8 ppm,Zn含量低于10 ppm,杂质Cd含量低于3 ppm,杂质Cu含量低于2 ppm;回收Cd化学纯度大于99.9%,Cd回收率大于94%。
以上所揭露的仅为本发明较佳实施例而已,当然不能以此来限定本发明之权利范围,因此依本发明权利要求所作的等同变化,仍属本发明所涵盖的范围。
Claims (10)
1.一种分离靶件中In和Cd的方法,其特征在于,包括如下步骤:
将靶件真空加热,蒸馏除去Cd和Zn的混合物,得到靶件基底,把所述Cd和Zn的混合物放入碱液内碱浸得到碱浸液,对所述碱浸液过滤,得到的滤渣为Cd,所述靶件基底中含In;
将所述靶件基底放入酸液进行酸浸得到酸浸液,对所述酸浸液过滤,得到含In的滤液,所述酸液为有机酸或非氧化性无机酸;
将所述滤液使用树脂吸附、萃取或蒸馏的方法纯化得到In。
2.根据权利要求1所述的分离靶件中In和Cd的方法,其特征在于,所述真空加热的次数为两次,分别为第一次真空加热和第二次真空加热,能将所述Cd和Zn的混合物彻底去除。
3.根据权利要求2所述的分离靶件中In和Cd的方法,其特征在于,所述第一次真空加热的真空度为10~30Pa,所述第一次真空加热的温度为700~900℃,所述第一次真空加热的时间为1~4 h。
4.根据权利要求2所述的分离靶件中In和Cd的方法,其特征在于,所述第二次真空加热的真空度为2~7Pa,所述第二次真空加热的温度与所述第一次真空加热的温度相同,所述第二次真空加热的时间为1~3 h。
5.根据权利要求1所述的分离靶件中In和Cd的方法,其特征在于,所述碱液为NaOH溶液或KOH溶液,所述碱液的浓度为2~3 mol/L,所述碱浸的加热温度为35~80℃,所述碱浸的时间为0.5~1h。
6.根据权利要求1所述的分离靶件中In和Cd的方法,其特征在于,所述有机酸为乙酸或草酸;所述非氧化性无机酸选自硫酸、盐酸和氢溴酸中的一种。
7.根据权利要求1所述的分离靶件中In和Cd的方法,其特征在于,所述酸液的体积浓度为30%~80%,所述酸浸的温度为70~95℃,所述酸浸的搅拌速率为200~600 r/min,所述酸浸的时间为1~6 h。
8.根据权利要求1所述的分离靶件中In和Cd的方法,其特征在于,所述酸浸时加入双氧水,所述加入双氧水的量为双氧水与酸的比摩尔比为0.05~0.2:1。
9.根据权利要求1所述的分离靶件中In和Cd的方法,其特征在于,所述树脂吸附步骤选择的树脂为阳离子交换树脂或螯合树脂。
10.根据权利要求1所述的分离靶件中In和Cd的方法,其特征在于,所述萃取步骤的萃取剂选自中性萃取剂、胺类萃取剂和酸性萃取剂中的一种。
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