CN112499653A - 一种含碘方钠石的制备方法 - Google Patents

一种含碘方钠石的制备方法 Download PDF

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CN112499653A
CN112499653A CN202011455079.9A CN202011455079A CN112499653A CN 112499653 A CN112499653 A CN 112499653A CN 202011455079 A CN202011455079 A CN 202011455079A CN 112499653 A CN112499653 A CN 112499653A
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林世建
杨冬燕
王梦辉
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Abstract

本发明涉及一种含碘方钠石的制备方法，包括以下步骤：S1.称取原料；S2.混合研磨；S3.压片；S4.高温烧结；S5.二次研磨；S6.配置NaOH溶液；S7.溶解杂质；S8.洗涤；S9.干燥。本发明提出的高温固相+压片+NaOH溶液洗涤的制备方法可得到理想的含碘方钠石，避免了水热法中出现的相分离，又因为含碘方钠石的高温固相合成没有引入H2O和OH‑，因此避免了羟基方钠石杂质相的生成。产物中剩余的未反应物质和产生的其他杂质相可通过NaOH溶液溶解并通过抽滤洗涤去除，得到纯净的含碘方钠石。碘挥发的问题也可通过压片得到较好的解决，成功的将碘固定在方钠石上。

Description

一种含碘方钠石的制备方法
技术领域
本发明涉及核废物固化和化工技术领域，特别涉及一种含碘方钠石的制备方法。
背景技术
高放废物的长久安全处置是制约核能可持续发展的关键问题，放射性同位素129I具有长半衰期、强放射性和高迁移率，如果处置不当，129I易迁移到生态环境中，从而对生物造成危害。对人类而言，129I会积累在甲状腺中，对人体产生危害，所以129I是需重点处置的放射性核素。方钠石Na8Al6Si6O24Cl2是自然界中稳定存在的一种矿相，根据“类质同象”原理,I-可占据Cl-位置，所以，方钠石矿相是潜在的129I固化基材。
本发明以稳定的127I作为模拟核素，对含碘方钠石Na8Al6Si6O24Cl2-xIx(x＝0-2)进行制备。含碘方钠石的合成通常有水热法和高温固相法，水热法可在低于200℃的温度环境下进行，从而避免碘的挥发。然而，水热法合成的产物中会有羟基方钠石的存在，并且I-和Cl-半径的显著差异，会使方钠石晶格发生畸变，出现相分离。高温固相法可克服I-和Cl-离子占位的互相排斥，从而形成热力学上稳定的固溶体，避免因I-与Cl-的半径差异引起的相分离现象。然而传统的高温固相法容易造成碘化物的挥发，并引入其他杂质相，无法得到纯净的含碘方钠石。
发明内容
本发明为了解决上述问题，用高温固相法代替水热法制备含碘的方钠石材料，并对传统高温固相法制备含碘方钠石的流程进行了改进。
一种含碘方钠石的制备方法，包括以下步骤：
S1.称取原料：
6 NaAlO2+6 SiO2+2(1-x)NaCl+2 x NaI＝Na8Al6Si6O24Cl2-xIx
根据上述化学反应方程式，称取适量的NaAlO2、SiO2、NaCl和NaI作为原始反应物制备含碘方钠石Na8Al6Si6O24Cl2-xIx(x＝0-2)；
S2.混合研磨：将称量好的原始反应物在球磨机上球磨4次，每次30min；
S3.压片：将混合充分的原始反应物在压片机上压片，压强为40MPa，时间保持5min，制得片状物料；
S4.高温烧结：将压成片状的物料放在氧化铝坩埚上，放入马弗炉中烧结，升温速率为5℃/min，反应温度为850℃，反应时间为3h，降温速率为5℃/min，合成含有SiO2和Na2SiO3杂质的含碘方钠石；
S5.二次研磨：将反应后的片状产物再次放入球磨机中球磨120min，将其球磨成粉末状产物；
S6.配置NaOH溶液：配置5mol/L的NaOH溶液；
S7.溶解杂质：将球磨好的粉末状产物放入5mol/L的NaOH溶液中，用磁力搅拌器搅拌120min,溶解SiO2和Na2SiO3杂质，并制得固液混合物；
S8.洗涤：将搅拌好的固液混合物用循环水式真空泵进行抽滤，使其固液分离并用去离子水进行稀释洗涤，得到沉淀物；
S9.干燥：将沉淀物在恒温干燥箱下干燥，温度为120℃，时间为24h,即得到干燥的、物相纯净的含碘方钠石样品粉末。
作为优选的，步骤S6中按5g产物对应100mL的5mol/L NaOH溶液的比例，确定NaOH溶液的用量。
作为优选的，步骤S8中，用去离子水进行多次稀释洗涤，直至水溶液为中性，得到沉淀物。
本发明的有益效果为：
(1)用高温固相法代替水热法，避免了水热法中出现的相分离；
(2)含碘方钠石的高温固相合成没有引入H2O和OH-，因此避免了羟基方钠石杂质相的生成，产物中剩余的未反应物质和产生的其他杂质相可通过NaOH溶液抽滤并洗涤去除；
(3)碘的挥发可通过对原始反应物压片抑制，成功的将碘固定在方钠石上。
附图说明
为了更清楚地说明本发明实施例的技术方案，下面将对实施例中所需要使用的附图作简单地介绍，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相关的附图。
图1为x＝1含碘方钠石NaOH溶液洗涤与未洗涤的X射线衍射(XRD)图；
图2为x＝1含碘方钠石压片与未压片的XRD衍射图；
图3为高温固相+压片+NaOH溶液洗涤成功合成的含碘方钠石Na8Al6Si6O24Cl2-xIx(x＝0-2)XRD衍射图。
具体实施方式
下面将结合对本发明的实施方案进行详细描述，本领域技术人员将会理解，下列实施例仅用于说明本发明，而不视为限定本发明的范围，实施例中未注明具体技术或条件者，按照本领域内的文献所描述的技术或条件或者按照产品说明书进行。
一种含碘方钠石的制备方法，包括以下步骤：
S1.称取原料：
6 NaAlO2+6 SiO2+2(1-x)NaCl+2 x NaI＝Na8Al6Si6O24Cl2-xIx
根据上述化学反应方程式，称取适量的NaAlO2、SiO2、NaCl和NaI作为原始反应物制备含碘方钠石Na8Al6Si6O24Cl2-xIx(x＝0-2)；
S2.混合研磨：将称量好的原始反应物在球磨机上球磨4次，每次30min，目的是将原始反应物充分混合研磨，以确保后续的反应充分；
S3.压片：将混合充分的原始反应物在压片机上压片，压强为40MPa，时间保持5min，制得片状物料；
S4.高温烧结：将压成片状的物料放在氧化铝坩埚上，放入马弗炉中高温烧结，升温速率为5℃/min，反应温度为850℃，反应时间为3h，降温速率为5℃/min，合成含有SiO2和Na2SiO3杂质的含碘方钠石；
S5.二次研磨：将反应后的片状产物再次放入球磨机中球磨120min，将其球磨成粉末状产物；
S6.配置NaOH溶液：配置5mol/L的NaOH溶液，按5g产物对应100mL的5mol/L NaOH溶液的比例，确定NaOH溶液的用量；
S7.溶解杂质：将球磨好的粉末状产物放入5mol/L的NaOH溶液中，用磁力搅拌器搅拌120min,溶解SiO2和Na2SiO3杂质，并制得固液混合物；
S8.洗涤：将搅拌好的固液混合物用循环水式真空泵进行抽滤，使其固液分离并用去离子水进行稀释洗涤，得到沉淀物；
S9.干燥：将沉淀物在恒温干燥箱下干燥温度为120℃，时间为24h,即得到干燥的、物相纯净的含碘方钠石样品粉末。
根据附图实验数据可知，图1表明NaOH溶液洗涤可成功去除含碘方钠石中的SiO2和Na2SiO3杂质，得到纯净的含碘方钠石相。
图2表明压片可有效抑制碘的挥发，含碘方钠石中碘的含量可通过(110)晶面的衍射峰的强度定性判断，强度越高碘含量越低。
图3表明高温固相+压片+NaOH溶液洗涤可成功合成不同系列的含碘方钠石Na8Al6Si6O24Cl2-xIx(x＝0-2)。所有组分的衍射峰与含碘方钠石一致，且没有其他杂质峰的存在。
本发明的含碘方钠石高温固相+压片+NaOH溶液洗涤的制备方法可得到理想的含碘方钠石，避免了水热法中出现的相分离。又因为含碘方钠石的高温固相合成没有引入H2O和OH-，因此避免了羟基方钠石杂质相的生成。产物中剩余的未反应物质和产生的其他杂质相可通过NaOH溶液抽滤并洗涤去除，得到纯净的含碘方钠石。碘挥发的问题也可通过压片得到较好的解决，成功的将碘固定在方钠石上。
以上所述仅为本发明专利的较佳实施例而已，并不用以限制本发明专利，凡在本发明专利的精神和原则之内所作的任何修改、等同替换和改进等，均应包含在本发明专利的保护范围之内。

Claims (3)

1.一种含碘方钠石的制备方法，其特征在于，包括以下步骤：
S1.称取原料：
6NaAlO2+6SiO2+2(1-x)NaCl+2x NaI＝Na8Al6Si6O24Cl2-xIx
根据上述化学反应方程式，称取适量的NaAlO2、SiO2、NaCl和NaI作为原始反应物制备含碘方钠石Na8Al6Si6O24Cl2-xIx(x＝0-2)；
S2.混合研磨：将称量好的原始反应物在球磨机上球磨4次，每次30min；
S3.压片：将混合充分的原始反应物在压片机上压片，压强为40MPa，时间保持5min，制得片状物料；
S4.高温烧结：将压成片状的物料放在氧化铝坩埚上，放入马弗炉中进行高温烧结，升温速率为5℃/min，烧结温度为850℃，保温时间为3h，降温速率为5℃/min，合成含有SiO2和Na2SiO3杂质的含碘方钠石；
S5.二次研磨：将烧结后的片状产物再次放入球磨机中球磨120min，将其球磨成粉末状产物；
S6.配置NaOH溶液：配置5mol/L的NaOH溶液；
S7.溶解杂质：将球磨好的粉末状产物放入5mol/L的NaOH溶液中，用磁力搅拌器搅拌120min,溶解SiO2和Na2SiO3杂质，得到固液混合物；
S8.洗涤：将搅拌好的固液混合物用循环水式真空泵进行抽滤，使其固液分离并用去离子水进行稀释洗涤，得到沉淀物；
S9.干燥：将沉淀物放在恒温干燥箱中干燥，温度为120℃，干燥时间为24h,即得到干燥的、物相纯净的含碘方钠石样品粉末。
2.根据权利要求1所述的一种含碘方钠石的制备方法，其特征在于，步骤S6中按5g产物对应100mL的5mol/L NaOH溶液的比例，确定NaOH溶液的用量。
3.根据权利要求1所述的一种含碘方钠石的制备方法，其特征在于，步骤S8中，用去离子水进行多次稀释洗涤，直至水溶液为中性，得到沉淀物。
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