CN104418400A - 铁基纳米合金及其在吸附铯中的应用 - Google Patents
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 94
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 39
- 229910052792 caesium Inorganic materials 0.000 title claims abstract description 25
- 239000000956 alloy Substances 0.000 title claims abstract description 15
- 238000001179 sorption measurement Methods 0.000 title claims abstract description 11
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 10
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 title claims abstract 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- -1 cesium ions Chemical class 0.000 claims abstract description 8
- 238000010521 absorption reaction Methods 0.000 claims description 30
- 239000000463 material Substances 0.000 claims description 25
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 21
- 238000002360 preparation method Methods 0.000 claims description 13
- 239000007864 aqueous solution Substances 0.000 claims description 11
- 229910000990 Ni alloy Inorganic materials 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 6
- 238000000926 separation method Methods 0.000 claims description 6
- 150000003839 salts Chemical class 0.000 claims description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- 239000010941 cobalt Substances 0.000 claims description 4
- 229910017052 cobalt Inorganic materials 0.000 claims description 4
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 4
- 229910052759 nickel Inorganic materials 0.000 claims description 4
- 238000001556 precipitation Methods 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 4
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 150000002500 ions Chemical class 0.000 claims description 3
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 2
- 238000010907 mechanical stirring Methods 0.000 claims description 2
- 229910021645 metal ion Inorganic materials 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 5
- 239000002253 acid Substances 0.000 abstract description 3
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- 230000005855 radiation Effects 0.000 abstract description 2
- 238000006722 reduction reaction Methods 0.000 abstract description 2
- 239000007791 liquid phase Substances 0.000 abstract 1
- NCMHKCKGHRPLCM-UHFFFAOYSA-N caesium(1+) Chemical compound [Cs+] NCMHKCKGHRPLCM-UHFFFAOYSA-N 0.000 description 22
- 239000000243 solution Substances 0.000 description 12
- 238000011068 loading method Methods 0.000 description 8
- 239000010808 liquid waste Substances 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 5
- 238000006555 catalytic reaction Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- KMAQZIILEGKYQZ-UHFFFAOYSA-N 1-chloro-3-nitrobenzene Chemical compound [O-][N+](=O)C1=CC=CC(Cl)=C1 KMAQZIILEGKYQZ-UHFFFAOYSA-N 0.000 description 4
- CZGCEKJOLUNIFY-UHFFFAOYSA-N 4-Chloronitrobenzene Chemical compound [O-][N+](=O)C1=CC=C(Cl)C=C1 CZGCEKJOLUNIFY-UHFFFAOYSA-N 0.000 description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 4
- 229910000808 amorphous metal alloy Inorganic materials 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000005984 hydrogenation reaction Methods 0.000 description 4
- 229910017604 nitric acid Inorganic materials 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 3
- 238000004070 electrodeposition Methods 0.000 description 3
- 239000000706 filtrate Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- UGACIEPFGXRWCH-UHFFFAOYSA-N [Si].[Ti] Chemical compound [Si].[Ti] UGACIEPFGXRWCH-UHFFFAOYSA-N 0.000 description 2
- 238000013019 agitation Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000010790 dilution Methods 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- 238000005342 ion exchange Methods 0.000 description 2
- 238000005374 membrane filtration Methods 0.000 description 2
- 239000003758 nuclear fuel Substances 0.000 description 2
- 150000003016 phosphoric acids Chemical class 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 239000002901 radioactive waste Substances 0.000 description 2
- 238000012958 reprocessing Methods 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 239000002228 NASICON Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
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- 238000004090 dissolution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000004992 fission Effects 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 239000011964 heteropoly acid Substances 0.000 description 1
- 229910001410 inorganic ion Inorganic materials 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 239000012716 precipitator Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000002285 radioactive effect Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002594 sorbent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- UTYXJYFJPBYDKY-UHFFFAOYSA-N tetrapotassium;iron(2+);hexacyanide;trihydrate Chemical compound O.O.O.[K+].[K+].[K+].[K+].[Fe+2].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] UTYXJYFJPBYDKY-UHFFFAOYSA-N 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
本发明公开了铁基纳米合金及其在吸附铯中的应用，首先利用液相化学还原法制备磷铁纳米合金材料；然后制备的磷铁合金材料用于吸附水溶液中铯离子。本发明技术方案中利用铁基纳米合金材料通过吸附去除水中铯离子，铁基纳米合金材料具有制备过程简单、耐酸、耐辐射、易回收等特点，并且对铯离子吸附容量可观。
Description
技术领域
本发明属于无机材料吸附技术领域，更加具体地说，涉及一种铁基纳米合金在吸附铯中的应用。
背景技术
以核能为代表的新能源发展越来越受到众多国家的重视。核燃料后处理是目前己知的最复杂和最具挑战性的化学处理过程之一，这也是核燃料后处理技术进展比较缓慢的重要原因之一。137Cs是高放废液中寿命较长的高释热裂变产物，所占放射性份额较大，在分离工艺去除和回收137Cs，既可将高放废液变为中低放废液，还可进行资源化利用。从废液中分离铯的常用手段包括离子交换法、沉淀法和溶剂萃取法。无机离子交换技术成熟，处理设备简单，不引入危险溶剂，具有对目标元素选择性好、可稳定存在（状态稳定）、抗辐射性强等特点，成为目前应用较为广泛的处理手段。用于除铯的无机离子交换材料主要有杂多酸盐，多价金属磷酸盐，不溶性铁氰化合物，钛硅化合物，天然及人造沸石等，其中沸石类材料交换容量易受溶液的酸度和盐含量影响，仅适于处理低酸度、低盐含量的放射性废液，对于高盐度、高酸性废液效果低下；不溶性亚铁氰化物交换剂交换平衡时间长，不能重复再生使用；合成硅钛化合物主要是针对碱性的高放废液，在酸性高放废液中去除铯的涉及较少；NASICON构型的磷酸盐适合用于固定放射性废料载体，对于水体中铯离子的去除分配系数较低，吸附容量不大。
发明内容
本发明的目的在于克服现有技术的不足，提供一种铁基纳米合金及其在吸附铯中的应用，利用铁基纳米合金材料通过吸附去除水中铯离子，铁基纳米合金材料具有制备过程简单、耐酸、耐辐射、易回收等特点，并且对铯离子吸附容量可观。
本发明的技术目的通过下述技术方案予以实现：
铁基纳米合金及其在吸附铯中的应用，首先利用液相化学还原法制备磷铁（铁基）纳米合金材料；然后制备的磷铁（铁基）合金材料用于吸附水溶液中铯离子即可。
在进行水体中铯的吸附时，选择将铁基纳米合金置于水体中，吸附后进行过滤分离，由于材料中含有具有磁性的铁元素，可利用外加磁场对吸附后材料分离，通过材料制备环节调节材料的磁性强度，提高分离效率。
在进行吸附时，选择常温常压即可（20—25摄氏度，一个大气压），并可选择进行搅拌（例如超声或者机械搅拌），吸附时间选择至少在1h之上，优选2—4h。
本发明技术方案中利用铁基纳米合金作为吸附载体，选择磷铁合金、磷铁镍合金或者磷铁钴合金，制备方法可参考下述文献进行：
（1）磷铁合金制备：Physicochemical and catalytic properties of Fe–Pultrafineamorphous catalysts，Baskaran Rajesh,Natarajan Sasirekha,Yu-Wen Chen，MolecularCatalysis A:Chemical275(2007)174–182；
（2）磷铁镍合金制备：A Fe-promoted Ni–P amorphous alloy catalyst(Ni–Fe–P)forliquidphase hydrogenation of m-and p-chloronitrobenzene。Xinhuan Yana,,Junqing Suna,Youwen Wangb,Jianfeng Yanga.Journal of Molecular Catalysis A:Chemical252(2006)17–22；
（3）磷铁钴合金制备：Preparation of Fe-Co-P amorphousalloys by electrodeposition，J.Herreros，J.M.Barandiar，A.Garcia-Arribas。Journal of Non-Crystalline Solids201(1996)102-109。
在具体制备中也可按照下述方案进行：配置铁离子的水溶液和次磷酸钠的水溶液进行混合，其中可根据添加元素种类和要求向铁离子的水溶液中加入镍、钴，在选择铁源、镍源、钴源时，选择相应的可溶性盐即可，并通过1mol/L的盐酸调节混合液的pH至1.5，然后向混合液中滴加KBH4水溶液，待滴加完毕反应结束后将产生的棕黑色沉淀，将此沉淀依次用去离子水、乙醇、丙酮洗涤数次去掉游离离子，于80℃真空干燥，700℃下煅烧0.5—1h即可得到铁基纳米合金。
其中铁源可选择FeCl2、FeSO4、FeCl3等可溶铁盐，所述KBH4加入量需根据混合液中金属离子和磷元素进行还原所需的化学反应计量进行添加。
使用的磷铁合金、磷铁镍合金、磷铁钴合金中，三种元素的摩尔比在下述范围内选择：
（1）磷铁合金：Fe/P:（4—7）:1
（2）磷铁镍合金：Ni:Fe:P=9:30:（10—11）
（3）磷铁钴合金：Fe:Co:P=（28—30）:15:（7—10）
在完成吸附过滤之后，将滤液利用原子吸收分光光度计（日本日立公司型号：Z-5300）测定吸附后溶液中铯离子浓度，即可计算材料的吸附容量。
本发明的技术方案通过铁基纳米合金作为吸附载体，直接投入水体中进行铯的吸附，通过检测吸附后溶液中铯离子浓度，确定材料的吸附容量（平均可达35—40mg/g）；并在实验室模拟高放废液环境（1500ppm的铯离子硝酸水溶液，硝酸的浓度为3mol/L）中进行吸附，材料的吸附容量亦可达到上述平均值，并同时较为完好地保持材料的形貌，说明吸附材料具有耐酸、耐腐蚀等特点。
附图说明
图1是本发明实施例中制备的铁基纳米合金的扫描电镜照片（SEM，日本日立公司，S-4800）。
具体实施方式
下面结合具体实施例进一步说明本发明的技术方案。
实施例1
将5.40gFeCl3·6H2O溶于100ml去离子水中，完全溶解后，加入次磷酸钠固体溶解，会有白色沉淀产生不影响后续试验进行，将上述溶液调节pH值至1.5左右得到磷铁溶液。配制1mol/L的KBH4水溶液，溶解完全后。在搅拌得得情况下缓慢加入到磷铁溶液中，出现棕黑色沉淀，滴加结束，继续搅拌1小时。然后离心洗涤数次。80℃真空干燥，在700℃下煅烧1h。
实施例2
磷铁合金制备：Physicochemical and catalytic properties of Fe–Pultrafine amorphouscatalysts，Baskaran Rajesh,Natarajan Sasirekha,Yu-Wen Chen，Molecular Catalysis A:Chemical275(2007)174–182；磷铁合金：Fe/P:4:1
实施例3
磷铁合金制备：Physicochemical and catalytic properties of Fe–Pultrafine amorphouscatalysts，Baskaran Rajesh,Natarajan Sasirekha,Yu-WenChen，Molecular Catalysis A:Chemical275(2007)174–182；磷铁合金：Fe/P:7:1
实施例4
磷铁镍合金制备：A Fe-promoted Ni–P amorphous alloy catalyst(Ni–Fe–P)forliquidphase hydrogenation of m-and p-chloronitrobenzene。Xinhuan Yana,,Junqing Suna,Youwen Wangb,Jianfeng Yanga.Journal of Molecular CatalysisA:Chemical252(2006)17–22；Ni:Fe:P=9:30:10
实施例5
磷铁镍合金制备：A Fe-promoted Ni–P amorphous alloy catalyst(Ni–Fe–P)forliquidphase hydrogenation of m-and p-chloronitrobenzene。Xinhuan Yana,,Junqing Suna,Youwen Wangb,Jianfeng Yanga.Journal of Molecular Catalysis A:Chemical252(2006)17–22；Ni:Fe:P=9:30:11
实施例6
磷铁钴合金制备：Preparation of Fe-Co-P amorphousalloys by electrodeposition，J.Herreros，J.M.Barandiar，A.Garcia-Arribas。Journal of Non-Crystalline Solids201(1996)102-109；Fe:Co:P=28:15:7
实施例7
磷铁钴合金制备：Preparation of Fe-Co-P amorphousalloys by electrodeposition，J.Herreros，J.M.Barandiar，A.Garcia-Arribas。Journal of Non-Crystalline Solids201(1996)102-109；Fe:Co:P=30:15:10
实施例8
磷铁镍合金制备：A Fe-promoted Ni–P amorphous alloy catalyst(Ni–Fe–P)forliquidphase hydrogenation of m-and p-chloronitrobenzene。Xinhuan Yana,,Junqing Suna,Youwen Wangb,Jianfeng Yanga.Journal of Molecular Catalysis A:Chemical252(2006)17–22；Ni:Fe:P=9:29.9:11.1
将实施例2—8中制备的吸附材料80℃真空干燥，在700℃下煅烧1h；将煅烧后的实施例1—8研细用于吸附实验，预先配制浓度为150ppm(150mg/L)铯离子水溶液100ml，称取0.4g吸附剂加入铯离子溶液中，超声分散均匀，然后磁力搅拌反应2h，取样5ml用0.45μm滤膜过滤，滤液稀释使用原子吸收分光光度计测定吸附后铯离子溶液浓度，计算材料的吸附容量（每组实施例进行三次试验然后计算平均），如下
（1）实施例1：35.2mg/g
（2）实施例2：36.4mg/g
（3）实施例3：40.3mg/g
（4）实施例4：37.2mg/g
（5）实施例5：38.3mg/g
（6）实施例6：39.8mg/g
（7）实施例7：37.1mg/g
（8）实施例8：36.4mg/g
配制1500ppm的铯离子硝酸水溶液，其中硝酸的浓度为3mol/L，加入准确称量的1.0g吸附材料加入铯离子溶液中，超声分散均匀，然后磁力搅拌反应2h，取样5ml用0.45μm滤膜过滤，滤液稀释使用原子吸收分光光度计测定吸附后铯离子溶液浓度，计算材料的吸附容量（每组实施例进行三次试验然后计算平均），如下
（1）实施例1：35.4mg/g
（2）实施例2：36.2mg/g
（3）实施例3：39.9mg/g
（4）实施例4：37.1mg/g
（5）实施例5：38.7mg/g
（6）实施例6：38.4mg/g
（7）实施例7：36.9mg/g
（8）实施例8：37.4mg/g
针对两种不同环境中的Cs，材料的吸附容量均可达到比较理想的水平，在酸性条件下同时较为完好地保持材料的形貌，说明吸附材料具有耐酸、耐腐蚀等特点。
以上对本发明做了示例性的描述，应该说明的是，在不脱离本发明的核心的情况下，任何简单的变形、修改或者其他本领域技术人员能够不花费创造性劳动的等同替换均落入本发明的保护范围。
Claims (10)
1.铁基纳米合金在吸附铯中的应用，其特征在于，在进行水体中铯的吸附时，将磷铁（铁基）纳米合金置于水体中，吸附后进行过滤分离。
2.根据权利要求1所述的铁基纳米合金在吸附铯中的应用，其特征在于，利用外加磁场对吸附后材料分离，通过材料制备环节调节材料的磁性强度，提高分离效率。
3.根据权利要求1所述的铁基纳米合金在吸附铯中的应用，其特征在于，在进行吸附时，选择常温常压，例如20—25摄氏度和一个大气压。
4.根据权利要求1所述的铁基纳米合金在吸附铯中的应用，其特征在于，在进行吸附时，选择进行搅拌，例如超声或者机械搅拌。
5.根据权利要求1所述的铁基纳米合金在吸附铯中的应用，其特征在于，在进行吸附时，吸附时间选择至少在1h之上，优选2—4h。
6.根据权利要求1所述的铁基纳米合金在吸附铯中的应用，其特征在于，所述磷铁（铁基）纳米合金选择磷铁合金、磷铁镍合金或者磷铁钴合金。
7.根据权利要求6所述的铁基纳米合金在吸附铯中的应用，其特征在于，所述磷铁合金中元素摩尔比为Fe/P:（4—7）:1；所述磷铁镍合金中元素摩尔比为Ni:Fe:P=9:30:（10—11）；所述磷铁钴合金中元素摩尔比为Fe:Co:P=（28—30）:15:（7—10）。
8.根据权利要求1所述的铁基纳米合金在吸附铯中的应用，其特征在于，所述磷铁（铁基）纳米合金具体制备方法按照下述方案进行：配置铁离子的水溶液和次磷酸钠的水溶液进行混合，其中根据添加元素种类和要求向铁离子的水溶液中加入镍、钴，在选择铁源、镍源、钴源时，选择相应的可溶性盐即可，并通过1mol/L的盐酸调节混合液的pH至1.5，然后向混合液中滴加KBH4水溶液，待滴加完毕反应结束后将产生的棕黑色沉淀，将此沉淀依次用去离子水、乙醇、丙酮洗涤数次去掉游离离子，于80℃真空干燥，700℃下煅烧0.5—1h即可得到铁基纳米合金。
9.根据权利要求8所述的铁基纳米合金在吸附铯中的应用，其特征在于，所述铁源可选择FeCl2、FeSO4、FeCl3等可溶铁盐。
10.根据权利要求8所述的铁基纳米合金在吸附铯中的应用，其特征在于，所述KBH4加入量需根据混合液中金属离子和磷元素进行还原所需的化学反应计量进行添加。
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| CN112661227A (zh) * | 2019-10-15 | 2021-04-16 | 韩国原子力研究院 | 放射性化学废物处理装置以及放射性化学废物处理方法 |
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