CN108160048A - 高稳定性除铯吸附剂的规模化制备方法及其产品与应用 - Google Patents
高稳定性除铯吸附剂的规模化制备方法及其产品与应用 Download PDFInfo
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- CN108160048A CN108160048A CN201810008565.2A CN201810008565A CN108160048A CN 108160048 A CN108160048 A CN 108160048A CN 201810008565 A CN201810008565 A CN 201810008565A CN 108160048 A CN108160048 A CN 108160048A
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- Prior art keywords
- adsorbent
- ferrocyanide
- particulate form
- inorganic oxide
- transition metal
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- 239000003463 adsorbent Substances 0.000 title claims abstract description 209
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- 229910052792 caesium Inorganic materials 0.000 title abstract description 41
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 title abstract description 40
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 50
- 229910052723 transition metal Inorganic materials 0.000 claims abstract description 37
- 229910052809 inorganic oxide Inorganic materials 0.000 claims abstract description 36
- 150000003624 transition metals Chemical class 0.000 claims abstract description 27
- 150000002500 ions Chemical class 0.000 claims abstract description 21
- 230000002285 radioactive effect Effects 0.000 claims abstract description 19
- 229910001417 caesium ion Inorganic materials 0.000 claims abstract description 17
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- 230000002745 absorbent Effects 0.000 claims abstract description 15
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- 238000002386 leaching Methods 0.000 claims abstract description 11
- 150000004767 nitrides Chemical class 0.000 claims abstract description 9
- 238000005253 cladding Methods 0.000 claims abstract description 8
- 239000002861 polymer material Substances 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 51
- 239000000243 solution Substances 0.000 claims description 51
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- 239000002243 precursor Substances 0.000 claims description 23
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- -1 transition metal salt Chemical class 0.000 claims description 10
- 229930006000 Sucrose Natural products 0.000 claims description 9
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- 239000002253 acid Substances 0.000 claims description 7
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 6
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- 239000000661 sodium alginate Substances 0.000 claims description 6
- 235000010413 sodium alginate Nutrition 0.000 claims description 6
- 229940005550 sodium alginate Drugs 0.000 claims description 6
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims description 5
- 150000007513 acids Chemical class 0.000 claims description 3
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- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 2
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- XOGGUFAVLNCTRS-UHFFFAOYSA-N tetrapotassium;iron(2+);hexacyanide Chemical compound [K+].[K+].[K+].[K+].[Fe+2].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] XOGGUFAVLNCTRS-UHFFFAOYSA-N 0.000 description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
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- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 description 6
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- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 5
- 239000011230 binding agent Substances 0.000 description 5
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 5
- 239000004327 boric acid Substances 0.000 description 5
- 229910052796 boron Inorganic materials 0.000 description 5
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- 239000012530 fluid Substances 0.000 description 5
- 239000002052 molecular layer Substances 0.000 description 5
- 230000009467 reduction Effects 0.000 description 5
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 4
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 229910052708 sodium Inorganic materials 0.000 description 4
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- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 4
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 3
- 235000013162 Cocos nucifera Nutrition 0.000 description 3
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- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 description 3
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- PANJMBIFGCKWBY-UHFFFAOYSA-N iron tricyanide Chemical compound N#C[Fe](C#N)C#N PANJMBIFGCKWBY-UHFFFAOYSA-N 0.000 description 3
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 3
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- GTSHREYGKSITGK-UHFFFAOYSA-N sodium ferrocyanide Chemical compound [Na+].[Na+].[Na+].[Na+].[Fe+2].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] GTSHREYGKSITGK-UHFFFAOYSA-N 0.000 description 3
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- DCYOBGZUOMKFPA-UHFFFAOYSA-N iron(2+);iron(3+);octadecacyanide Chemical compound [Fe+2].[Fe+2].[Fe+2].[Fe+3].[Fe+3].[Fe+3].[Fe+3].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] DCYOBGZUOMKFPA-UHFFFAOYSA-N 0.000 description 2
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- 238000000643 oven drying Methods 0.000 description 2
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- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical group O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
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- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明涉及高稳定性除铯吸附剂的规模化制备方法及其产品与应用。具体地,本发明涉及一种颗粒态无机氧化物或活性炭负载型过渡金属稳定的亚铁氰化物吸附剂,其包含:颗粒态的无机氧化物载体或者颗粒态的活性炭载体;包覆所述无机氧化物或活性炭载体的过渡金属稳定的亚铁氰化物层;以及包覆所述过渡金属稳定的亚铁氰化物层的高分子材料层。该吸附剂具有高压碎强度和低离子浸出率。本发明还涉及该吸附剂的制备方法及其在去除放射性同位素Cs离子和去除稳定性同位素Cs离子的应用,以及去除放射性同位素Rb离子和去除稳定性同位素Rb离子的应用。
Description
技术领域
本发明涉及无机材料领域,特别涉及一种稳定性高的除铯吸附剂的规模化制备方法及其产品与应用,该吸附剂同时对铷也有良好的吸附性能。
背景技术
按照中国核电中长期发展规划目标,到2020年,中国大陆运行核电装机容量将达到5800万千瓦,在建3000万千瓦左右;到2030年要全面实现建设核电强国目标。面对核能事业发展新形势新挑战,中国迫切需要在放射性废物处理、核应急技术、放射性流出物排放标准等方面大力发展。
放射性液体的高效及时处理,是建立核安全纵深防御体系亟待解决的重要问题之一,因此迫切需要开展废液应急处理新技术、新装备与新材料的研发和储备,在核电站内建立起多层次的废液处理处置技术保障。第一个层次是核电站正常运行过程中,放射性核素的实际消除。该项技术主要针对核电站正常运行过程中放射性废物的去除,在保障处理工艺稳定性、有效性的同时实现废物小量化。第二个层次是当电站发生燃料破损等问题时,在废液中核素范围宽、形态多样的情况下,及时开展场内废液应急处理。该项技术能够及时、快速、高效去除污染,防止放射性物质外泄。第三个层次是纵深防御体系的最后一道防线,即在发生超设计基准事故的极端情况下,迅速启动场外核应急处理,最大限度限制核事故对环境的影响。
相比较于离子交换树脂,无机离子吸附剂对主要痕量核素Cs、Sr、Co、Ag、I等的选择性高,可以从高盐量的放射性废水中高效地去除目标核素离子,能快速大幅度降低废液的放射性活度,并且受共存非放离子的影响小,因此其使用寿命长,产生少量的固体废物。此外,大量的放射性元素富集在小体积的固态无机离子交换剂中,使得辐射防护变得相对容易。相比于吸附产生的废树脂,无机吸附技术产生的放射性废弃物热稳定性和化学稳定性好、耐辐照性能强,不易被辐射分解或生物分解,便于后期的处理处置,并且在地下处置场长期储存过程中,更具长期安全性。进一步,基于无机吸附技术的废液深度净化装置结构简单,具备有效、选择性强、小型化、模块化、可移动性强的技术特点,对现场服务条件要求低,非常适合于核电厂放射性废液成分较为复杂且现场布置空间有限的特殊要求。
基于无机吸附剂高效、快速和选择性高的应用特点,无机吸附技术在核电站事故废液处理中起到了关键作用。以日本福岛事故废液的处理为最典型的案例,从最初放射性废水处理系统的建立,到后来运行过程中的逐步完善,一直保持了无机吸附+膜技术耦合的工艺路线,采用无机吸附工艺选择性去除主要核素Cs-134和Cs-137,大幅度降低废水的放射性水平,降低后续工艺的辐射防护要求,进一步采用膜工艺能够广谱性去除水中的放射性核素。据福岛提供的水质监测结果,经过Cs吸附、反渗透的工艺流程处理后,水样的放射性水平从最初的107-108Bq/L的水平(事故发生后的初期高于此水平)降低到了103-104Bq/L的水平。无机吸附剂在核电站正常运行工况下也获得了较多的应用,例如:芬兰Loviisa和匈牙利Paks电站采用除铯吸附剂对核电站蒸发器废液进一步减容;苏格兰敦雷电站采用无机吸附剂从1500吨Na冷却堆废液和57吨Na/K冷却堆高含盐量废液中选择性去除Cs-134和Cs-137;英国Bradwell Magnox电站在核设施退役过程采用无机吸附剂对燃料元件碎片酸性溶解液进行处理;日本原子能研究所(JAERI)采用无机吸附剂在浓硝酸溶解废液中去除Pu/Cs/Sr;以及美国Savannah River和Callaway核电站、英国Sellafield以及芬兰Olkiluoto核电站均采用无机吸附剂对乏燃料储存池废液处理。
在过去的几十年间,用于除铯的无机吸附剂的研究不是太多,主要包括例如焦磷酸氧锆(中国原子能科学研究院的中国发明专利CN106342077B);由非金属矿物经过相应的处理复合而成的无机复合吸附剂(核工业北京地质研究院的中国发明专利CN103691393B);磁性铯选择性吸附剂(日本捷恩智株式会社的中国发明专利CN104054136和中国原子能科学研究院的中国发明专利CN1129922C);以及本课题组研制成功的亚铁氰化物系列除铯无机吸附剂,其对核电站应急放射性废水的处理具有良好的性能,并获得多项中国国家专利授权,例如CN100469435C、CN101279249B、CN102836693B等。
我国正在建设的AP1000反应堆中设计采用无机吸附剂对工艺水中的Cs-134和Cs-137进行选择性的去除。工艺水主要包括核电站正常运行情况下的堆芯冷却水、核燃料储存池冷却水等,我国大多数在运行的核电站采用核级水过滤器与离子交换除盐床的工艺进行去除,其中除盐床的前后分别设有不同过滤精度的过滤器,前过滤器用于去除废液中的颗粒物,保护除盐床运行,而后过滤器主要是去除除盐床产生的废弃树脂颗粒,保障出水的洁净度。电站的运行对工艺水的水质要求非常高,例如要求工艺水具有极低的电导率和离子浓度以抑制金属腐蚀和保障反应堆的安全运行,并且要求工艺水具有极低的浊度,以保障工艺水处理过程中过滤器不易被堵塞,延长过滤器的使用寿命,减少固体废物量。在AP1000的工艺水处理设计中,采用絮凝结合活性炭过滤技术去除废液中的胶体,接着采用无机吸附剂去除主要核素Cs-134和Cs-137,进而采用离子交换树脂去除其他核素。这样的去除工艺其设计目标旨在提高核素处理效果,并减少放射性废树脂的产生量。目前,AP1000设计采用的无机吸附剂为沸石,在使用中存在吸附速度慢和容易粉化导致水质浊度和电导率升高的现象。
鉴于以上情况,提供能够在核电站正常运行工况下从工艺水中高效去除铯离子的高强度、高稳定性的无机吸附剂仍是目前亟待解决的问题之一。
发明内容
本发明的一个目的在于:提供一种高强度、高稳定性的颗粒态除铯吸附剂,并实现其在核电站正常运行工况下从工艺水中高效去除Cs-134和Cs-137。
本发明的发明人经大量实验,出乎意料地发现,通过洗涤除去颗粒态无机氧化物或者活性炭负载型过渡金属稳定的亚铁氰化物吸附剂的表面上结合松散的固相颗粒和该吸附剂中的可溶性离子之后,在其上包覆高分子材料层,可以获得具有机械稳定性和低离子渗出率的除铯吸附剂。
一方面,本发明提供了一种颗粒态无机氧化物或者颗粒态活性炭负载型过渡金属稳定的亚铁氰化物吸附剂,其包含:颗粒态的无机氧化物或者颗粒态的活性炭作为载体;包覆所述无机氧化物或活性炭载体的过渡金属稳定的亚铁氰化物层;以及包覆所述过渡金属稳定的亚铁氰化物层的高分子材料层。
优选地,所述高分子材料包括海藻酸钠、壳聚糖、数均分子量介于2000-6000之间的聚乙二醇、聚乙烯醇、蔗糖或其任意组合。
优选地,根据本发明的吸附剂具有2-100N/particle的压碎强度。
优选地,根据本发明的吸附剂具有这样的离子浸出特性,以至于所述吸附剂在10的液固比下浸泡24小时后,所得浸出液的浊度小于10mg/L。
优选地,根据本发明的吸附剂具有这样的离子浸出特性,以至于所述吸附剂在10的液固比下浸泡24小时后,所得浸出液的电导率小于15mg/L。
由此获得的吸附剂能够在核电站正常运行工况下从工艺水中高效去除Cs-134和Cs-137。这种吸附剂不仅可以应用于AP1000型反应堆,也可以应用于国内外各种堆型的压水堆核电站,以降低主要核素Cs-134和Cs-137的排放,减少离子交换树脂的用量,实现废物小量化的目标。而且,由此得到的吸附剂对放射性废液中存在的同族核素Rb-88和Rb-89也有良好的吸附性能。
另一方面,本发明还涉及上述颗粒态无机氧化物或者颗粒态活性炭负载型过渡金属稳定的亚铁氰化物吸附剂的制备方法,包括:
1)提供初级吸附剂;
2)用去离子水洗涤步骤1)的初级吸附剂,直到洗涤液的电导率为25.0μs/cm或更低且浊度为30mg/L或更低;以及
3)用高分子材料包覆经洗涤的初级吸附剂,优选在酸或碱的存在下,从而得到经包覆的初级吸附剂;以及
4)可选地,用去离子水洗涤步骤3)的经包覆的初级吸附剂,直到洗涤液的电导率为20.0μs/cm或更低且浊度为20mg/L或更低,
从而得到所述颗粒态无机氧化物或者颗粒态活性炭负载型过渡金属稳定的亚铁氰化物吸附剂。
优选地,根据本发明的一个实施方式,提供初级吸附剂的步骤包括,将颗粒态无机氧化物或者颗粒态活性炭载体浸渍在亚铁氰化物的水溶液中2-48小时,从而得到负载有亚铁氰化物的前体A,然后将前体A与过渡金属盐的水溶液混合,并在100-150℃的温度下反应2-24小时。
优选地,根据本发明的一个实施方式,提供初级吸附剂的步骤包括,将颗粒态无机氧化物或者颗粒态活性炭载体浸渍在过渡金属盐的水溶液中2-48小时,从而得到负载有过渡金属盐的前体B,然后将前体B与亚铁氰化物的水溶液混合,并在100-150℃的温度下反应2-24小时。
在本发明的一个具体实施方式中,根据本发明的吸附剂是通过包括如下的步骤制备的:
(1)亚铁氰化物的负载:首先在1号反应釜中加入纯水并加热到80-100℃,在其中加入可溶性亚铁氰化物,使之溶解;其次在反应釜中加入颗粒态无机氧化物载体或者颗粒态活性炭载体,浸渍2-48h,之后进行固液相分离并干燥,获得负载有亚铁氰化物的前体A;
(2)制备过渡金属稳定的亚铁氰化物吸附剂:首先在2号反应釜中加入纯水并加热到80-100℃,在其中加入可溶性过渡金属盐,使之溶解;其次将步骤(1)中获得的负载有亚铁氰化物的前体A加入反应釜,搅拌均匀后,将反应釜密封,并将反应温度设置在100-150℃下反应2-24h,反应结束后进行固液相分离,获得初级的除铯吸附剂B;
(3)吸附剂的清洗:采用去离子水对步骤(2)中获得的初级除铯吸附剂B进行清洗,优选进行10小时或更长,直到洗涤液的电导率为25.0μs/cm或更低且浊度为30.0mg/L或更低,之后将获得的吸附剂干燥,优选采用恒温烘箱或真空烘箱在60-120℃的干燥温度下进行干燥,记为二级吸附剂C;
(4)吸附剂包覆:通过如下在步骤(3)获得的二级吸附剂C表面包覆高分子材料层:将具有粘结作用的高分子材料溶解在纯水中配制成一定浓度的溶液;将二级吸附剂C加入到溶液体系中;根据高分子材料的不同,在搅拌的过程中滴加酸或碱溶液;将混合物搅拌1-10h之后,进行固液相分离,从而获得三级吸附剂D。
(5)吸附剂的清洗:采用去离子水对步骤(4)中获得的三级除铯吸附剂D进行清洗,优选进行10小时或更长,直到洗涤液的电导率为20.0μs/cm或更低且浊度为20mg/L或更低,之后进行固液相分离,并将吸附剂干燥,优选采用恒温烘箱或真空烘箱在60-120℃的干燥温度下进行干燥,获得最终的除铯吸附剂E。
进一步,根据本发明,采用的亚铁氰化物是可溶的,包括亚铁氰化钾和亚铁氰化钠。优选地,可溶性亚铁氰化物的水溶液浓度为10~50wt%。
进一步,根据本发明,颗粒态无机氧化物载体包括硅胶小球、氧化铝小球、氧化钛小球、氧化锆小球、分子筛小球。优选地,小球的颗粒度为0.5~5mm,其压碎强度为2-150N/particle。
进一步,根据本发明,颗粒态活性炭载体可以是煤基碳,或者是椰壳炭、果壳碳等。优选地,活性炭颗粒的颗粒度约为0.5~5mm,其压碎强度为2-150N/particle。
进一步,根据本发明,过渡金属盐是可溶的,包括硫酸铜、硝酸铜、氯化铜、硫酸亚铁、硝酸铁、硝酸镍、硫酸镍、氯化锌、硫酸锌、醋酸锌、硝酸钴、氯化钴、氧氯化锆、硫酸锰、或其任意组合。优选地,上述可溶性盐的水溶液的浓度为10~60wt%。
进一步,根据本发明,采用的高分子材料包括海藻酸钠、壳聚糖、聚乙二醇(2000-6000)、聚乙烯醇、蔗糖或其组合。优选地,上述高分子材料被配制成浓度为1~20wt%的水溶液。
进一步,根据本发明,滴加的酸为盐酸、硫酸、醋酸或其任意组合。优选地,酸的浓度为0.01~1mol/L。
进一步,根据本发明,滴加的碱为氢氧化钠、碳酸钠、碳酸氢钠、氨水或其任意组合。优选地,碱的浓度为0.01~1mol/L;
由上述制备方法制备所得的系列颗粒负载型亚铁氰化物吸附剂,也在本发明的保护范围之内。
本发明的发明人惊讶地发现,根据本发明的颗粒态无机氧化物或颗粒态活性炭负载型过渡金属稳定的亚铁氰化物吸附剂具有结构稳定、吸附性能高的特点。这种吸附剂由于可以吸附放射性和/或稳定性同位素Cs离子,也可以吸附放射性和/或稳定性同位素Rb离子,因此具有广阔的应用前景。例如,可以通过吸附作用用于实现分离和/或去除或提取放射性或稳定同位素Cs离子,也可以用于分离和/或去除或提取放射性或稳定同位素Rb离子的应用。因此,上述根据本发明的颗粒态无机氧化物或者颗粒态活性炭负载型过渡金属稳定的亚铁氰化物吸附剂在去除放射性同位素Cs离子和去除稳定同位素Cs离子的应用,以及去除放射性同位素Rb离子和去除稳定同位素Rb离子的应用,也在本发明的保护范围之内。
本发明的发明人认识到,对采用无机氧化物或活性炭为载体,并且在载体表面上具有一系列过渡金属稳定的亚铁氰化物层(采用浸渍和高温水热两步反应来实现)的初级吸附剂进行水洗过程,可以去除在初级吸附剂的表面上结合松散的部分固相颗粒,并使该初级吸附剂中的可溶性离子充分释放,使经洗涤的初级吸附剂具有良好的机械强度和较低的离子浸出特性。进一步地,在经洗涤的初级吸附剂表面进行高分子层包覆,可以进一步提高吸附剂的机械强度,从而获得优选具有2-100N/particle的压碎强度和极低离子浸出特性的吸附剂。
具体实施方式
下面结合具体实施方式对本发明作进一步阐述,但本发明并不限于以下实施例。所述方法如无特别说明均为常规方法,所述原材料及检测所用标准化学试剂如无特别说明均能从公开商业途径而得。
在以下的实施例中,吸附剂分别进行了静态吸附和固定床吸附反应柱性能试验测定,吸附前后Cs+离子的浓度采用等离子体质谱(ICP-MS)来测定,吸附剂性能采用分配系数Kd和去污系数DF来表示。
静态吸附测定中,一定量的吸附剂加入到50mL的离心管中,置于恒温摇床上摇动48h~72h,测定吸附前后的Cs+离子浓度,吸附剂性能采用分配系数Kd和去污系数DF来表示。吸附分配系数Kd(mL/g)如下式1所示,其中C0和Ct分别为被吸附离子的初始浓度以及达到吸附平衡后浓度,F为被处理溶液体积(mL)与吸附剂质量(mg)之比。去污系数如下式2所示,为被吸附离子的进水浓度与达到吸附平衡后的出水浓度的比值。一般吸附分配系数说明了吸附材料本身的特性,Kd值在105以上的说明吸附剂的性能良好;去污系数的大小不仅与材料本身的吸附特性相关,也与吸附剂的用量相关,该值越大说明污染物去除得越干净。
Kd=(Co–Ct)×F×1000/Ct (1)
动态吸附性能采用固定床吸附反应柱进行,测试柱高度10cm,直径1.5cm,水流量为20BV/h。采用去污系数DF来表示吸附柱对Cs+的去污效果。
根据本发明的吸附剂的压碎强度是通过如下测定的。吸附剂的压碎强度采用国产的压碎强度仪进行测定,仪器型号为:YHKC-2A型颗粒强度测试仪。测定中,随机选取60-100颗吸附剂颗粒,测定时逐一将颗粒放在压锤正下方中心位置,旋转手柄,使压锤下落,当接近颗粒时,缓慢旋转,使压锤慢慢接触,当听到颗粒破碎的声音时,仪器上给出压碎时刻加载在颗粒上的力为多少牛顿。根据本发明的吸附剂的离子浸出特征是通过如下测定的:首先将吸附剂浸泡在10倍体积的纯水中,采用搅拌器进行搅拌,或采用摇床进行摇动,一定时间后,分别采用浊度计HACH 2100N和电导率仪DDSJ-308A测定浸泡液体的浊度和电导率。浊度计采用的精度为0.001mg/L,电导率仪采用的精度为0.01μs/cm。
实施例1:硅胶负载型吸附剂制备与除铯性能
优选出机械强度较高的硅胶Si-1,颗粒度为0.5-2.0mm,在其上制备亚铁氰化铜钾吸附剂,步骤如下:
(1)铜盐的负载:首先在1号反应釜中加入纯水并加热到80-100℃,在其中加入硫酸铜,使之溶解形成浓度为10-50%的溶液;其次在反应釜中加入硅胶颗粒Si-1为载体,浸渍2-48h,之后进行固液相分离并干燥,获得负载有硫酸铜的前体Si-1-A。
(2)制备过渡金属稳定的亚铁氰化物吸附剂:首先在2号反应釜中加入纯水并加热到80-100℃,在其中加入亚铁氰化钠,使之溶解并形成浓度为10-50%的溶液;其次将步骤(1)中获得的负载有硫酸铜的前体Si-1-A加入反应釜,搅拌均匀后,将反应釜密封,并将反应温度设置在100℃下反应24h,反应结束后进行固液相分离,获得初级的除铯吸附剂Si-1-B。
(3)吸附剂的清洗:采用纯净水对步骤(2)中获得的初级除铯吸附剂Si-1-B进行清洗,每次清洗所用的水体积为吸附剂体积的10倍,直到连续搅拌24h后的洗涤液中电导率为22.8μs/cm,浊度降低为17.8mg/L,之后将获得的吸附剂干燥,记为二级吸附剂Si-1-C。
(4)吸附剂包覆:在步骤(3)获得的二级吸附剂Si-1-C表面包覆高分子层,方法是采用壳聚糖为粘结剂,首先将壳聚糖溶解在纯水中配制成浓度为2~10wt%的溶液,将二级吸附剂Si-1-C加入到溶液体系中,在搅拌1h后,逐渐往体系中加入1.0M的氢氧化钠溶液,直到溶液中pH值达到10-11,继续搅拌并反应5-10h后,固液相分离,获得三级吸附剂Si-1-D。
(5)吸附剂的清洗:采用纯净水对步骤(4)中获得的三级除铯吸附剂Si-1-D进行清洗,每次清洗所用的水体积为吸附剂体积的10倍,直到连续搅拌24h后的洗涤液的浊度小于20mg/L,电导率小于20μs/cm,之后固液相分离,并将吸附剂采用真空干燥,获得最终的硅胶负载型亚铁氰化铜钾除铯吸附剂。
经测定,吸附剂的压碎强度为12~14N/particle,在液固比为10的条件下浸泡24h后,液体中浊度为6mg/L,电导率为11μs/cm,溶液中COD浓度为1.5mg/L。采用静态吸附方法测定吸附性能中,溶液初始Cs离子浓度为10mg/L,共存的硼酸浓度为以硼计500mg/L,测试液体积为50mL,吸附剂质量为10mg的条件下,对Cs的去污系数DF值为26.2,相当于Cs的去除率大于95%。
实施例2:氧化铝负载型吸附剂制备与铯去除性能
优选出机械强度较高的氧化铝小球Al-1,颗粒度为0.5-2.0mm,在其上制备亚铁氰化锌钾吸附剂,步骤如下:
(1)亚铁氰化物的负载:首先在1号反应釜中加入纯水并加热到80-100℃,在其中加入亚铁氰化钾,使之溶解形成浓度为10-50%的溶液;其次在反应釜中加入氧化铝小球Al-1为载体,浸渍2-48h,之后进行固液相分离并在恒温烘箱内干燥,获得负载有亚铁氰化物的前体Al-1-A。
(2)制备过渡金属稳定的亚铁氰化物吸附剂:首先在2号反应釜中加入纯水并加热到80-100℃,在其中加入醋酸锌,使之溶解并形成浓度为10-50%的溶液;其次将步骤(1)中获得的负载有亚铁氰化物的前体Al-1-A加入反应釜,搅拌均匀后,将反应釜密封,并将反应温度设置在100℃下反应8-16h,反应结束后进行固液相分离,获得初级的除铯吸附剂Al-1-B。
(3)吸附剂的清洗:采用纯净水对步骤(2)中获得的初级除铯吸附剂Al-1-B进行清洗,每次清洗所用的水体积为吸附剂体积的10倍,直到连续搅拌24h后的洗涤液中电导率为18.2μs/cm,浊度降低为21.3mg/L,之后将获得的吸附剂干燥,记为二级吸附剂Al-1-C。
(4)吸附剂包覆:在步骤(3)获得的二级吸附剂Al-1-C表面包覆高分子层,方法是分别采用聚乙烯醇、聚乙二醇(6000)为粘结剂,首先分别将聚乙烯醇、聚乙二醇溶解在纯水中配制成溶液,聚乙烯醇溶液浓度为1~10wt%,聚乙二醇(6000)的浓度为5~30%。将二级吸附剂Al-1-C加入到溶液体系中,液固比为10:1;继续搅拌并反应2-10h后,固液相分离,获得三级吸附剂Al-1-D。
(5)吸附剂的清洗:采用纯净水对步骤(4)中获得的三级除铯吸附剂Al-1-D进行清洗,每次清洗所用的水体积为吸附剂体积的10倍,直到连续搅拌24h后的洗涤液的浊度小于20mg/L,电导率小于20μs/cm,之后固液相分离,并将吸附剂采用真空干燥,获得最终的氧化铝负载型亚铁氰化锌钾除铯吸附剂。
经测定,吸附剂的压碎强度为3~9N/particle,在液固比为10的条件下浸泡24h后,液体中浊度为3mg/L,电导率为7μs/cm,溶液中COD浓度为2.7mg/L。采用静态吸附方法测定吸附性能中,溶液初始Cs离子浓度为10mg/L,共存的硼酸浓度为以硼计500mg/L,测试液体积为50mL,吸附剂质量为10mg的条件下,对Cs的去污系数DF值为23.2,相当于Cs的去除率大于95%。
进一步采用固定床小吸附柱进行动态测定,吸附柱高度10cm,直径1.5cm,吸附剂装满整个吸附柱,处理水流量为20BV/h,其中Cs的初始浓度为10mg/L。测定结果表明,吸附剂在处理水量达到3870BV时,对Cs的去污系数还可以达到330。
实施例3:氧化钛负载型吸附剂制备与性能
优选出机械强度较高的氧化钛小球Ti-1,颗粒度为0.5-2.0mm,在其上制备亚铁氰化钴钾吸附剂,步骤如下:
(1)亚铁氰化物的负载:首先在1号反应釜中加入纯水并加热到80-100℃,在其中加入亚铁氰化钾,使之溶解形成浓度为10-50%的溶液;其次在反应釜中加入氧化钛小球Ti-1为载体,浸渍2-48h,之后进行固液相分离并在恒温烘箱内干燥,获得负载有亚铁氰化物的前体Ti-1-A。
(2)制备过渡金属稳定的亚铁氰化物吸附剂:首先在2号反应釜中加入纯水并加热到80-100℃,在其中加入硝酸钴,使之溶解并形成浓度为10-50%的溶液;其次将步骤(1)中获得的负载有亚铁氰化物的前体Ti-1-A加入反应釜,搅拌均匀后,将反应釜密封,并将反应温度设置在100℃下反应4-12h,反应结束后进行固液相分离,获得初级的除铯吸附剂Ti-1-B。
(3)吸附剂的清洗:采用纯净水对步骤(2)中获得的初级除铯吸附剂Ti-1-B进行清洗,每次清洗所用的水体积为吸附剂体积的10倍,直到连续搅拌24h后的洗涤液中电导率为22.4μs/cm,浊度降低为15.8mg/L,之后将获得的吸附剂干燥,记为二级吸附剂Ti-1-C。
(4)吸附剂包覆:在步骤(3)获得的二级吸附剂Al-1-C表面包覆高分子层,方法是分别采用聚乙烯醇+蔗糖、聚乙二醇+蔗糖(6000)为粘结剂,首先分别将聚乙烯醇、聚乙二醇溶解在纯水中配制成溶液,聚乙烯醇溶液浓度为1~10wt%,聚乙二醇(6000)的浓度为5~30%;其次在溶液中加入蔗糖使之溶解,并控制蔗糖与聚乙烯醇或聚乙二醇浓度的1~4倍。将二级吸附剂Ti-1-C加入到溶液体系中,液固比为10:1;继续搅拌并反应2-10h后,固液相分离,获得三级吸附剂Ti-1-D。
(5)吸附剂的清洗:采用纯净水对步骤(4)中获得的三级除铯吸附剂Al-1-D进行清洗,每次清洗所用的水体积为吸附剂体积的10倍,直到连续搅拌24h后的洗涤液的浊度小于20mg/L,电导率小于20μs/cm,之后固液相分离,并将吸附剂采用真空干燥,获得最终的氧化铝负载型亚铁氰化锌钾除铯吸附剂。
经测定,吸附剂的压碎强度为3~9N/particle,在液固比为10的条件下浸泡24h后,液体中浊度为2mg/L,电导率为6μs/cm,溶液中COD浓度为1.6mg/L。采用静态吸附方法测定吸附性能中,溶液初始Cs离子浓度为10mg/L,共存的硼酸浓度为以硼计500mg/L,测试液体积为50mL,吸附剂质量为10mg的条件下,对Cs的去污系数DF值为26.7,相当于Cs的去除率大于95%。
进一步采用固定床小吸附柱进行动态测定,吸附柱高度10cm,直径1.5cm,吸附剂装满整个吸附柱,处理水流量为20BV/h,其中Cs的初始浓度为10mg/L。测定结果表明,吸附剂在处理水量达到4213BV时,对Cs的去污系数还可以达到310。
实施例4:氧化锆负载型吸附剂制备与铷、铯吸附性能
优选出具有单斜晶相的氧化锆小球Zr-1作为吸附剂载体,小球颗粒度为0.5-2.0mm,具有很高的机械强度,压碎强度大于30N/particle,在其上制备亚铁氰化铁(III)钾吸附剂,步骤如下:
(1)亚铁氰化物的负载:首先在1号反应釜中加入纯水并加热到80-100℃,在其中加入亚铁氰化钠,使之溶解形成浓度为10-50%的溶液;其次在反应釜中加入氧化锆小球Zr-1为载体,浸渍10-48h,之后进行固液相分离并在恒温烘箱内干燥,获得负载有亚铁氰化物的前体Zr-1-A。
(2)制备过渡金属稳定的亚铁氰化物吸附剂:首先在2号反应釜中加入纯水并加热到80-100℃,在其中加入硝酸铁,使之溶解并形成浓度为10-50%的溶液;其次将步骤(1)中获得的负载有亚铁氰化物的前体Zr-1-A加入反应釜,搅拌均匀后,将反应釜密封,并将反应温度设置在120℃下反应10-24h,反应结束后进行固液相分离,获得初级的除铯吸附剂Zr-1-B。
(3)吸附剂的清洗:采用纯净水对步骤(2)中获得的初级除铯吸附剂Zr-1-B进行清洗,每次清洗所用的水体积为吸附剂体积的10倍,直到连续搅拌24h后的洗涤液中电导率为15.6μs/cm,浊度降低为25.8mg/L,之后将获得的吸附剂干燥,记为二级吸附剂Zr-1-C。
(4)吸附剂包覆:在步骤(3)获得的二级吸附剂Zr-1-C表面包覆高分子层,方法是采用海藻酸钠为粘结剂,首先将海藻酸钠溶解在纯水中配制成溶液,浓度为1~10wt%。将二级吸附剂Zr-1-C加入到溶液体系中,液固比为10:1;搅拌1h后滴加1M的盐酸溶液直到pH值为4~5,继续搅拌并反应2-10h后,固液相分离,获得三级吸附剂Zr-1-D。
(5)吸附剂的清洗:采用纯净水对步骤(4)中获得的三级除铯吸附剂Zr-1-D进行清洗,每次清洗所用的水体积为吸附剂体积的10倍,直到连续搅拌24h后的洗涤液的浊度小于20mg/L,电导率小于20μs/cm,之后固液相分离,并将吸附剂采用真空干燥,获得最终的氧化锆负载型亚铁氰化铁钾(普鲁士蓝)除铯吸附剂。
经测定,吸附剂的压碎强度为41N/particle,在液固比为10的条件下浸泡24h后,液体中浊度为7mg/L,电导率为12μs/cm,溶液中COD浓度为1.9mg/L。
采用静态吸附方法测定铯和锂、钠、钾、铷的竞争吸附性能,测试液体积为50mL,吸附剂的质量为10mg。测试液中以硼计的硼酸浓度为500ppm,Cs的初始浓度为10mg/L;共存的锂、钠、钾、铷离子采用两个浓度,分别相当于与10mg/L的Cs相同摩尔比。实验中测定在共存离子的竞争徐状态下,吸附剂对Cs的吸附性能变化。在单独Cs+存在的情况下,吸附剂对Cs的去污系数为23.2,在相同摩尔数的Li+、Na+、K+、Rb+的竞争吸附下,对Cs的去污系数分别为21.6、11.3、9.2和9.4。
从实验数据可见,本发明研制的负载型亚铁氰化物系列吸附剂对第一主族的离子都有一定的吸附特性,主要是Na+、K+、Rb+与Cs+之间有一定的竞争关系,但对Li的吸附性能很差,因此核电站工艺废液中存在的LiOH,不会影响到核素Cs的吸附去除性能。一般的,在核电站工艺废液中同时存在放射性核素Rb+,因此本发明研制的负载型亚铁氰化物系列吸附剂可以同时去除工艺水中的Rb-88、Rb-89和Cs-134与Cs-137。
实施例4:活性炭负载型吸附剂制备及其铯吸附性能
优选出颗粒度为0.5-2.0mm椰壳活性炭颗粒作为载体,经纯水清洗,直到pH为中性,电导率<20μS/cm,之后,活性炭颗粒烘干,作为吸附剂载体。测定可知所选择的活性炭颗粒具有较高的机械强度,压碎强度大于20N/particle,在其上制备亚铁氰化镍(II)钾吸附剂,步骤如下:
(1)亚铁氰化物的负载:首先在1号反应釜中加入纯水并加热到80-100℃,在其中加入亚铁氰化钾,使之溶解形成浓度为10-50%的溶液;其次在反应釜中加入活性炭颗粒为载体,浸渍10-48h,之后进行固液相分离并在恒温烘箱内干燥,获得负载有亚铁氰化物的前体GAC-1-A。
(2)制备过渡金属稳定的亚铁氰化物吸附剂:首先在2号反应釜中加入纯水并加热到80-100℃,在其中加入硫酸镍,使之溶解并形成浓度为10-50%的溶液;其次将步骤(1)中获得的负载有亚铁氰化物的前体GAC-1-A加入反应釜,搅拌均匀后,将反应釜密封,并将反应温度设置在120℃下反应10-24h,反应结束后进行固液相分离,获得初级的除铯吸附剂GAC-1-B。
(3)吸附剂的清洗:采用纯净水对步骤(2)中获得的初级除铯吸附剂GAC-1-B进行清洗,每次清洗所用的水体积为吸附剂体积的10倍,直到连续搅拌24h后的洗涤液中电导率<20μs/cm,浊度降低<20mg/L,之后将获得的吸附剂干燥,记为二级吸附剂GAC-1-C。
(4)吸附剂包覆:在步骤(3)获得的二级吸附剂GAC-1-C表面包覆高分子层,方法是聚乙烯醇为粘结剂,首先将聚乙烯醇溶解在纯水中配制成溶液,浓度为1~10wt%。将二级吸附剂GAC-1-C加入到溶液体系中,液固比为10:1;继续搅拌并反应2-10h后,固液相分离,获得三级吸附剂GAC-1-D。
(5)吸附剂的清洗:采用纯净水对步骤(4)中获得的三级除铯吸附剂GAC-1-D进行清洗,每次清洗所用的水体积为吸附剂体积的10倍,直到连续搅拌24h后的洗涤液的浊度小于20mg/L,电导率小于20μs/cm,之后固液相分离,并将吸附剂采用真空干燥,获得最终的颗粒活性炭负载型亚铁氰化镍钾除铯吸附剂。
经测定,吸附剂的压碎强度为32N/particle,在液固比为10的条件下浸泡24h后,液体中浊度为12mg/L,电导率为18μs/cm,溶液中COD浓度为1.4mg/L。
采用静态吸附方法测定铯吸附性能,测试液体积为40mL,吸附剂的质量为10mg。测试液中以硼计的硼酸浓度为1000ppm,Cs的初始浓度为10mg/L。实验中测定吸附剂对Cs的去污系数为48.3。
上面通过具体实施例的方式对本发明的各个方面进行了解释,但是本领域技术人员可以理解:本发明并不仅限于上面所描述的具体实施方式,本领域技术人员对本文所公开的各种具体技术手段、原料、工艺步骤等所做的等效替换和以及各种技术手段、原料、工艺步骤等的组合都在本发明的范围之内。
为了进一步举例说明本发明的某些方面,本发明还具体地提供了如下的一些非限制性实施方式:
1.一种颗粒态无机氧化物或活性炭负载型过渡金属稳定的亚铁氰化物吸附剂,其包含:颗粒态的无机氧化物载体,或者颗粒态的活性炭载体;包覆所述无机氧化物或活性炭载体的过渡金属稳定的亚铁氰化物层;以及包覆所述过渡金属稳定的亚铁氰化物层的高分子材料层。
2.如实施方式1所述的吸附剂,其中,所述高分子材料层包括海藻酸钠、壳聚糖、数均分子量介于2000-6000之间的聚乙二醇、聚乙烯醇、蔗糖或其任意组合。
3.如实施方式1或2所述的吸附剂,其具有2-100N/particle的压碎强度。
4.如实施方式1或2所述的吸附剂,其具有这样的离子浸出特性,以至于所述吸附剂在10的液固比下浸泡24小时后,所得液体的浊度为10mg/L或更低。
5.如实施方式1或2所述的吸附剂,其具有这样的离子浸出特性,以至于所述吸附剂在10的液固比下浸泡24小时后,所得液体的电导率为15μs/cm或更低。
6.用于制备颗粒态无机氧化物或活性炭负载型过渡金属稳定的亚铁氰化物吸附剂的方法,包括:
1)提供初级吸附剂;
2)用去离子水洗涤步骤1)的初级吸附剂,直到洗涤液的电导率为25.0μs/cm或更低且浊度为30mg/L或更低;
3)用高分子材料包覆经洗涤的初级吸附剂,从而得到经包覆的初级吸附剂;以及
4)可选地,用去离子水洗涤步骤3)的经包覆的初级吸附剂,直到洗涤液的电导率为20.0μs/cm或更低且浊度为20mg/L或更低,
从而得到所述颗粒态无机氧化物或者活性炭负载型过渡金属稳定的亚铁氰化物吸附剂。
7.根据实施方式6所述的方法,其中,提供初级吸附剂的步骤包括,将颗粒态无机氧化物或者颗粒态活性炭载体浸渍在亚铁氰化物的水溶液中2-48小时,从而得到负载有亚铁氰化物的前体A,然后将前体A与过渡金属盐的水溶液混合,并在100-150℃的温度下反应2-24小时。
8.根据实施方式6所述的方法,其中,提供初级吸附剂的步骤包括,将颗粒态无机氧化物或者颗粒态活性炭载体浸渍在过渡金属盐的水溶液中2-48小时,从而得到负载有过渡金属盐的前体B,然后将前体B与亚铁氰化物的水溶液混合,并在100-150℃的温度下反应2-24小时。
9.根据实施方式6-8中任意一项所述的方法,其中,所述高分子材料包括海藻酸钠、壳聚糖、聚乙二醇(2000-6000)、聚乙烯醇、蔗糖或其组合,优选被配制成浓度为1%~20wt%的水溶液。
10.根据实施方式6-8中任意一项所述的方法,其中,用高分子材料包覆经洗涤的初级吸附剂的步骤在酸或碱的存在下进行。
11.根据实施方式10所述的方法,其中,所述酸选自由盐酸、硫酸、醋酸或其组合组成的组,优选具有0.01-1mol/L的浓度;所述碱选自由氢氧化钠、碳酸钠、碳酸氢钠、氨水或其组合组成的组,优选具有0.01-1mol/L的浓度。
12.根据实施方式7-8中任意一项所述的方法,其中,所述颗粒态无机氧化物载体包括硅胶小球、氧化铝小球、氧化钛小球、氧化锆小球、分子筛小球或其组合,优选具有0.5到5mm的颗粒度,和/或2-150N/particle的压碎强度。
13.根据实施方式7-8中任意一项所述的方法,其中,所述颗粒态活性炭载体包括煤基碳、椰壳炭、果壳碳或其组合,优选具有0.5到5mm的颗粒度,和/或2-150N/particle的压碎强度。
14.根据实施方式7-8中任意一项所述的方法,其中,所述亚铁氰化物包括亚铁氰化钾、亚铁氰化钠或其组合,优选地,所述亚铁氰化物的水溶液具有10~50wt%的浓度。
15.根据实施方式7-8中任意一项所述的方法,其中,所述过渡金属盐包括硫酸铜、硝酸铜、氯化铜、硫酸亚铁、硝酸铁、硝酸镍、硫酸镍、氯化锌、硫酸锌、醋酸锌、硝酸钴、氯化钴、氧氯化锆、硫酸锰、或其任意组合,优选地,所述过渡金属盐的水溶液具有10~60wt%的浓度。
16.一种由实施方式6-15中任一项所述方法制备所得的颗粒状无机氧化物或活性炭负载型金属离子稳定的亚铁氰化物吸附剂。
17.由实施方式1-5中任意一项或者由实施方式16所述的颗粒状无机氧化物或活性炭负载型金属离子稳定的亚铁氰化物吸附剂用于吸附放射性同位素Cs离子或吸附稳定同位素Cs离子的用途。
18.如实施方式17所述的用途,用于去除或分离或提取放射性同位素Cs离子或用于去除或分离或提取稳定同位素Cs离子。
19.由实施方式1-5中任意一项或者由实施方式16所述的颗粒状无机氧化物或活性炭负载型金属离子稳定的亚铁氰化物吸附剂用于吸附放射性同位素Rb离子或吸附稳定同位素Rb离子的用途。
20.如实施方式19所述的用途,用于去除或分离或提取放射性同位素Rb离子或用于去除或分离或提取稳定同位素Rb离子。
Claims (10)
1.一种颗粒态无机氧化物或活性炭负载型过渡金属稳定的亚铁氰化物吸附剂,其包含:颗粒态的无机氧化物载体,或者颗粒态的活性炭载体;包覆所述无机氧化物或活性炭载体的过渡金属稳定的亚铁氰化物层;以及包覆所述过渡金属稳定的亚铁氰化物层的高分子材料层。
2.如权利要求1所述的吸附剂,其中,所述高分子材料层包括海藻酸钠、壳聚糖、数均分子量介于2000-6000之间的聚乙二醇、聚乙烯醇、蔗糖或其任意组合。
3.如权利要求1或2所述的吸附剂,其具有2-100N/particle的压碎强度。
4.如权利要求1或2所述的吸附剂,其具有这样的离子浸出特性,以至于所述吸附剂在10的液固比下浸泡24小时后,所得浸渍液的浊度为10mg/L或更低。
5.如权利要求1或2所述的吸附剂,其具有这样的离子浸出特性,以至于所述吸附剂在10的液固比下浸泡24小时后,所得液体的电导率为15μs/cm或更低。
6.用于制备颗粒态无机氧化物或活性炭负载型过渡金属稳定的亚铁氰化物吸附剂的方法,包括:
1)提供初级吸附剂;
2)用去离子水洗涤步骤1)的初级吸附剂,直到洗涤液的电导率为25.0μs/cm或更低,且浊度为30mg/L或更低;
3)用高分子材料包覆经洗涤的初级吸附剂,优选在酸或碱的存在下,从而得到经包覆的初级吸附剂;以及
4)可选地,用去离子水洗涤步骤3)的经包覆的初级吸附剂,直到洗涤液的电导率为20.0μs/cm或更低,且浊度为20mg/L或更低,
从而得到所述颗粒态无机氧化物或者活性炭负载型过渡金属稳定的亚铁氰化物吸附剂。
7.根据权利要求6所述的方法,其中,提供初级吸附剂的步骤包括,将颗粒态无机氧化物或者颗粒态活性炭载体浸渍在亚铁氰化物的水溶液中2-48小时,从而得到负载有亚铁氰化物的前体A,然后将前体A与过渡金属盐的水溶液混合,并在100-150℃的温度下反应2-24小时。
8.根据权利要求6所述的方法,其中,提供初级吸附剂的步骤包括,将颗粒态无机氧化物或者颗粒态活性炭载体浸渍在过渡金属盐的水溶液中2-48小时,从而得到负载有过渡金属盐的前体B,然后将前体B与亚铁氰化物的水溶液混合,并在100-150℃的温度下反应2-24小时。
9.一种由权利要求6-8中任一项所述方法制备所得的颗粒状无机氧化物或者活性炭负载型金属离子稳定的亚铁氰化物吸附剂。
10.由权利要求1-5中任意一项或者由权利要求9所述的颗粒状无机氧化物或颗粒活性炭负载型金属离子稳定的亚铁氰化物吸附剂用于吸附放射性同位素Cs离子或吸附稳定同位素Cs离子的用途,和/或用于吸附放射性同位素Rb离子或吸附稳定同位素Rb离子的用途。
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CN108160048B (zh) | 2023-07-14 |
CN117019109A (zh) | 2023-11-10 |
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GB2587072B (en) | 2022-09-07 |
GB2587072A (en) | 2021-03-17 |
GB202009144D0 (en) | 2020-07-29 |
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