CN108854948A - 一种同步去除放射性水中锶和铯的沸石改性方法 - Google Patents
一种同步去除放射性水中锶和铯的沸石改性方法 Download PDFInfo
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Abstract
本发明公开了一种同步去除放射性水中锶和铯的沸石改性方法,所述方法步骤如下:1)先用蒸馏水对待改性天然沸石进行3~5次冲洗,然后烘干备用;2)将步骤1)所得的沸石加入NaOH溶液中,然后放入摇床中恒温震荡,最后用蒸馏水对沸石冲洗5~7次,烘干备用;3)将步骤2)所得的沸石加入Cu(NO3)2溶液中,然后放入摇床中恒温震荡,最后用蒸馏水对沸石冲洗5~7次,烘干备用;4)将步骤3)所得的沸石加入K4Fe(CN)6溶液中,然后放入摇床中恒温震荡,最后用蒸馏水对沸石冲洗5~7次,烘干得到改性沸石颗粒。本发明的方法能够使改性后的沸石同时具有高效去除放射性水中锶和铯的效果,提高了沸石的吸附容量和选择吸附性。
Description
技术领域
本发明属于水处理技术领域,涉及一种沸石改性方法,具体涉及一种同步去除放射性水中锶和铯的沸石改性方法。
背景技术
随着科学技术的发展,核电占总能源的比例越来越高,但是随之而来的放射性污染也越来越严重。虽然核电站污水都是经过处理达标后才排放,但是排放的污水中会不可避免的含有少量的低浓度低放射性物质,90Sr和137Cs作为铀反应的主要产物,也是这些低浓度低放射性物质的主要成分。从目前来看,对含锶、铯放射性水进行处理的方法有化学沉淀法、离子交换法、吸附法、蒸发法、萃取法、生物法和膜法等,在这些处理方法的研究中,离子交换法是近年来最主要的研究方向。
在众多的无机离子交换剂中,沸石的稳定性好,交换容量高,材料低价易得,是处理低放射性水行之有效的方法之一。据相关专利文献报道,亚铁氰根(分子式为Fe(CN)6 4-)具有极高的化学稳定性,并且由于它对Cs和Sr有较强的结合能力,因此能够使金属亚铁氰化物对Cs和Sr有很强的选择吸附能力。然而因为它们存在粉末稠度问题,直接将这些吸附剂应用到固定柱模式下不可行。但是可以将亚铁氰化物负载到其他一些多孔载体上实现吸附柱应用,如硅胶、活性炭、聚氨酯(PU)泡沫、沸石和离子交换树脂等。
发明内容
为了克服现有沸石改性方法的不足,本发明提供了一种同步去除放射性水中锶和铯的沸石改性方法,该方法能够使改性后的沸石同时具有高效去除放射性水中锶和铯的效果,不仅提高了沸石的吸附容量和选择吸附性,而且可以简化现有去除锶和铯的工艺设备,对提升放射性水处理效果具有十分重要的意义。
本发明的目的是通过以下技术方案实现的:
一种同步去除放射性水中锶和铯的沸石改性方法,如图1所示,包括如下步骤:
1)先用蒸馏水对待改性天然沸石进行3~5次冲洗,然后烘干备用;
2)将步骤1)所得的沸石加入NaOH溶液中,然后放入摇床中恒温震荡,最后用蒸馏水对沸石冲洗5~7次,烘干备用;
3)将步骤2)所得的沸石加入Cu(NO3)2溶液中,然后放入摇床中恒温震荡,最后用蒸馏水对沸石冲洗5~7次,烘干备用;
4)将步骤3)所得的沸石加入K4Fe(CN)6溶液中,然后放入摇床中恒温震荡,最后用蒸馏水对沸石冲洗5~7次,烘干得到改性沸石颗粒。
优选地,所述步骤1)中,待改性天然沸石的粒径为300~500μm。
优选地,所述步骤1)中,烘干温度为60~70℃,烘干时间为4~8h。
优选地,所述步骤2)中,NaOH溶液的浓度为0.1~2mol/L,震荡温度为25~40℃,震荡时间为4~8小时,摇床转速为60~120rpm,烘干温度为80~100℃,烘干时间为10~14h。
优选地,所述步骤3)中,Cu(NO3)2溶液的浓度为0.05~0.2mol/L,震荡温度为20~35℃,震荡时间为2~6小时,摇床转速为100~160rpm,烘干温度为80~100℃,烘干时间为10~14h。
优选地,所述步骤4)中,K4Fe(CN)6溶液的浓度为0.02~0.1mol/L,震荡温度为20~35℃,震荡时间为2~6小时,摇床转速为100~160rpm,烘干温度为80~100℃,烘干时间为10~14h。
优选地,所述步骤4)中,改性沸石颗粒的粒径为300~500μm。
本发明所制备的改性沸石对放射性水中锶和铯的去除效果很好,研究结果表明:在放射性水中锶浓度为10mg/L、铯浓度为10mg/L,改性沸石投加量为2g/L,25℃,磁力搅拌吸附时间为2h的条件下,锶和铯的剩余浓度分别为0.3~0.6mg/L、0.2~0.5mg/L。此外,该改性沸石还具有良好的再生效果。
本发明方法的改性原理如下:
天然沸石本身具有强吸附、强离子交换性、耐高温腐蚀等特性,但其吸附对象局限性大,离子交换容量较低。用亚铁氰化物改性沸石来去除废水中的锶和铯是一种比较新的处理方法。以过渡金属的亚铁氰化物和钛硅酸盐为代表的无机离子交换剂来去除放射性废水中锶和铯的效果很好,但是这些吸附剂的尺寸太小,不易沉淀,会造成固液分离困难,不利于柱式操作,而且对后续处理的要求较高。制备出的亚铁氰化铜由于颗粒尺寸较小,因此发生了团聚现象,影响处理效果。用沸石作为载体来负载亚铁氰化物可以有效地改善这些问题,能够用于柱状处理,简化处理流程,改善团聚现象,使亚铁氰化物分布均匀,提高处理效果。而且沸石本身作为一种无机离子交换剂,具有很强的化学稳定性和热力学稳定性,对锶和铯也具有一定的去除效果。所以从理论上来说,用亚铁氰化物来改性沸石可以对锶和铯的去除有比较好的效果。
本发明具有如下优点:
1、本发明的制备方法简单且环保,在充分考虑沸石的反复利用问题上,降低了在实际工程运用中的成本。
2、沸石颗粒较大,能够用于柱状处理,简化处理流程。
3、沸石成本低,因该沸石颗粒球不易随着出水流失,可回收再进行吸附脱附,有效利用率高,大大降低了材料成本。
4、相较于一般沸石,本发明所制备的改性沸石对放射性水中锶和铯的吸附能力得到了大大的提升,对锶和铯的去除效果很好,将其用于锶铯污染物的静态吸附实验和动态吸附试验,验证了该改性材料的高效吸附性,为改性沸石同步去除锶和铯的研究应用奠定了良好的基础。
附图说明
图1为本发明同步去除放射性水中锶和铯的沸石改性工艺流程图。
具体实施方式
下面结合附图对本发明的技术方案作进一步的说明,但并不局限如此,凡是对本发明技术方案进行修改或者等同替换,而不脱离本发明技术方案的精神和范围,均应涵盖在本发明的保护范围中。
实施例1
本实施例提供了一种同步去除放射性水中锶和铯的沸石改性方法,所述方法具体步骤如下:
1)先用蒸馏水将适量粒径为400μm的待改性天然沸石进行5次冲洗,然后60℃烘干8h;
2)将步骤1)所得的沸石加入0.5mol/L NaOH溶液中,放入摇床中恒温30℃震荡6h,摇床转数为100rpm,然后用蒸馏水对沸石冲洗6次,90℃烘干12h,备用;
3)将步骤2)所得的沸石加入0.1mol/L Cu(NO3)2溶液中然后,放入摇床中恒温25℃震荡4h,摇床转数为140rpm,最后用蒸馏水对沸石冲洗7次,100℃烘干12h,备用;
4))将步骤3)所得的沸石加入0.05mol/L K4Fe(CN)6溶液中,然后放入摇床中恒温25℃震荡4h,摇床转数为140rpm,最后用蒸馏水对沸石冲洗7次,100℃烘干12h,得到改性沸石颗粒。
本实施例制备得到的改性后沸石的粒径为400μm,对放射性水中锶和铯的去除效果很好,在放射性水中锶浓度为10mg/L、铯浓度为10mg/L,改性沸石投加量为2g/L,25℃,磁力搅拌吸附时间为2h的条件下,锶和铯的剩余浓度分别为0.38mg/L、0.35mg/L,去除率高达96.2%和96.5%。
实施例2
本实施例提供了一种同步去除放射性水中锶和铯的沸石改性方法,所述方法具体步骤如下:
1)先用蒸馏水将适量粒径为300μm的待改性天然沸石进行4次冲洗,然后70℃烘干8h;
2)将步骤1)所得的沸石加入1mol/L NaOH溶液中,然后放入摇床中恒温35℃震荡5h,摇床转数为90rpm,最后用蒸馏水对沸石冲洗7次,80℃烘干12h,备用;
3)将步骤2)所得的沸石加入0.2mol/L Cu(NO3)2溶液中,然后放入摇床中恒温25℃震荡4h,摇床转数为130rpm,最后用蒸馏水对沸石冲洗7次,90℃烘干12h,备用;
4)将步骤3)所得的沸石加入0.1mol/L K4Fe(CN)6溶液中,然后放入摇床中恒温25℃震荡4h,摇床转数为130rpm,最后用蒸馏水对沸石冲洗7次,90℃烘干12h,得到改性沸石颗粒。
本实施例制备得到的改性后沸石的粒径为500μm,对放射性水中锶和铯的去除效果很好,在放射性水中锶浓度为10mg/L、铯浓度为10mg/L,改性沸石投加量为2g/L,25℃,磁力搅拌吸附时间为2h的条件下,锶和铯的剩余浓度分别为0.36mg/L、0.34mg/L,去除率高达96.4%和96.6%。
实施例3
本实施例提供了一种同步去除放射性水中锶和铯的沸石改性方法,所述方法具体步骤如下:
1)先用蒸馏水对适量粒径为500μm的待改性天然沸石进行6次冲洗,然后然后80℃烘干8h;
2)将步骤1)所得的沸石加入0.8mol/L NaOH溶液中,然后放入摇床中恒温30℃震荡6h,摇床转数为80rpm,最后用蒸馏水对沸石冲洗7次,85℃烘干12h,备用;
3)将步骤2)所得的沸石加入0.15mol/L Cu(NO3)2溶液中,然后放入摇床中恒温25℃震荡4h,摇床转数为140rpm,最后用蒸馏水对沸石冲洗7次,95℃烘干12h,备用;
4)将步骤3)所得的沸石加入0.075mol/L K4Fe(CN)6溶液中,然后放入摇床中恒温25℃震荡4h,摇床转数为150rpm,最后用蒸馏水对沸石冲洗7次,95℃烘干12h,得到改性沸石颗粒。
本实施例制备得到的改性后沸石的粒径为500μm,对放射性水中锶和铯的去除效果很好,在放射性水中锶浓度为10mg/L、铯浓度为10mg/L,改性沸石投加量为2g/L,25℃,磁力搅拌吸附时间为2h的条件下,锶和铯的剩余浓度分别为0.40mg/L、0.38mg/L,去除率高达96.0%和96.2%。
Claims (7)
1.一种同步去除放射性水中锶和铯的沸石改性方法,其特征在于所述方法步骤如下:
1)先用蒸馏水对待改性天然沸石进行3~5次冲洗,然后烘干备用;
2)将步骤1)所得的沸石加入NaOH溶液中,然后放入摇床中恒温震荡,最后用蒸馏水对沸石冲洗5~7次,烘干备用;
3)将步骤2)所得的沸石加入Cu(NO3)2溶液中,然后放入摇床中恒温震荡,最后用蒸馏水对沸石冲洗5~7次,烘干备用;
4)将步骤3)所得的沸石加入K4Fe(CN)6溶液中,然后放入摇床中恒温震荡,最后用蒸馏水对沸石冲洗5~7次,烘干得到改性沸石颗粒。
2.根据权利要求1所述的同步去除放射性水中锶和铯的沸石改性方法,其特征在于所述步骤1)中,待改性天然沸石的粒径为300~500μm。
3.根据权利要求1所述的同步去除放射性水中锶和铯的沸石改性方法,其特征在于所述步骤1)中,烘干温度为60~70℃,烘干时间为4~8h。
4.根据权利要求1所述的同步去除放射性水中锶和铯的沸石改性方法,其特征在于所述步骤2)中,NaOH溶液的浓度为0.1~2mol/L,震荡温度为25~40℃,震荡时间为4~8小时,摇床转速为60~120rpm,烘干温度为80~100℃,烘干时间为10~14h。
5.根据权利要求1所述的同步去除放射性水中锶和铯的沸石改性方法,其特征在于所述步骤3)中,Cu(NO3)2溶液的浓度为0.05~0.2mol/L,震荡温度为20~35℃,震荡时间为2~6小时,摇床转速为100~160rpm,烘干温度为80~100℃,烘干时间为10~14h。
6.根据权利要求1所述的同步去除放射性水中锶和铯的沸石改性方法,其特征在于所述步骤4)中,K4Fe(CN)6溶液的浓度为0.02~0.1mol/L,震荡温度为20~35℃,震荡时间为2~6小时,摇床转速为100~160rpm,烘干温度为80~100℃,烘干时间为10~14h。
7.根据权利要求1所述的同步去除放射性水中锶和铯的沸石改性方法,其特征在于所述步骤4)中,改性沸石颗粒的粒径为300~500μm。
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