CN112158820A - 一种氟磷灰石固溶体制备方法及其应用 - Google Patents
一种氟磷灰石固溶体制备方法及其应用 Download PDFInfo
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- VSIIXMUUUJUKCM-UHFFFAOYSA-D pentacalcium;fluoride;triphosphate Chemical compound [F-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O VSIIXMUUUJUKCM-UHFFFAOYSA-D 0.000 title claims abstract description 29
- 239000006104 solid solution Substances 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title abstract description 3
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- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 46
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- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 4
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- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 abstract 4
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Abstract
本发明公开了一种水热法合成氟磷灰石固溶体的方法。通过配制硝酸钙溶液作为基础液，将氟化钠溶液以5mL/s的速度加入至硝酸钙溶液中，再将磷酸氢二胺加入至硝酸钙和氟化钠的混合溶液中并快速搅拌，同时加入浓氨水，调节pH至8.0后持续在20℃下搅拌30min，将其放入373.15K条件下恒温水浴锅加热2d，最后取出样品，得到结晶度高、稳定性好的氟磷灰石固溶体。取适量氟磷灰石固溶体在pH＝2.0，温度为25‑45℃下进行溶解，掌握氟在环境中的迁移、转化与富集的规律。利用该方法合成的氟磷灰石固溶体具有低成本，易操控，能够实现氟在环境中的长期稳定化推存等优点。
Description
技术领域
本发明属于材料安全领域，涉及氟磷灰石固溶体合成方法及其应用。该方法利用氟离子可以替代羟基(-OH)进入羟基磷灰石晶格，形成氟磷灰石固溶体。
背景技术
氟(F)，位于元素周期表第二周期ⅦA族，原子序数为9，其属于卤族元素之一。氟具有高度的生物活性，是人类生命活动必需的微量元素之一。低含量氟(<1.5mg/L)可促进骨骼和牙齿的正常生长，但是人体长期摄入过高含量的氟会导致氟斑牙和氟骨症等疾病。氟是自然界中广泛分布的元素之一，在地壳中的存量约为0.06％～0.09％。氟主要存在于萤石(CAF2)、冰晶石(Na3AlF6)等物质中。据世界卫生组织1970年统计：46个国家中有28个国家的饮水含氟量超标；另外，含氟量低于1.5mg/L的有18个国家。在我国，高氟地下水遍及全国27个省、市和自治区，各地大约有70000万人饮用含氟量超过1mg/L的水。饮水高氟水导致的氟骨症和氟斑牙遍布全国20多个省，主要集中在东北、华北和西北地区。
氟磷灰石属于磷酸盐类矿物，并且磷酸盐类矿物材料对于重金属和氟等具有很好的处理能力，其可以发生同价或异价类质同象替换形成不同类型矿物，而氟离子与氢氧根离子的半径非常接近，因此氟离子和羟基可相互取代。有研究者进行研究，结果表明生成的矿物能够稳定存在，可以成为固定重金属的一种新方法。本发明提供一种以水热合成法合成氟磷灰石，对于固定废水中的氟具有重要意义。
发明内容
本发明目的是提供一种水热合成氟磷灰石固溶体的方法。对制备固溶体经过X射线衍射(XRD)、扫描电镜(SEM)、傅里叶变换红外光谱(FTIR)表征，测试在pH为2.00，温度分别为25、35和45℃条件下对于氟离子的浸出浓度，对溶解度和稳定性进行详细实验分析，为固定氟离子提供数据支撑。
1.一种氟磷灰石固溶体合成方法，其特征在于具体步骤为：
(1)首先利用氮气对超纯水进行脱气，然后配制0.2mol/L Ca(NO3)2溶液，0.2mol/LNaF溶液，0.2mol/L(NH4)2HPO4溶液；
(2)量取500mL 0.2mol/L Ca(NO3)2，并将其倒入干净的1000mL聚乙烯瓶中；
(3)将聚乙烯瓶放置于恒温加热搅拌器，并调节搅拌器转速为500～550rmp，温度为20℃；
(4)向(3)聚乙烯瓶中以5mL/s的速度加入100mL 0.2mol/L NaF溶液，并在转速为500～550rmp下搅拌3～5min；
(5)调节搅拌器转速为800～850rmp，并将300mL 0.2mol/L(NH4)2HPO4溶液加入聚乙烯瓶中，同时向聚乙烯瓶中加入浓氨水，快速将pH调至8.0后持续在20℃下搅拌25～30min；
(6)待溶液完全混匀后，盖好瓶盖并放入373.15K条件下恒温水浴锅中加热2d；
(7)待反应完全后，取出样品自然冷却，得到氟磷灰石固溶体。
本发明的氟磷灰石固溶体的应用于实现氟在环境中长期稳定化推放，则具体步骤为：
在100℃下反应完成后进行固液分离，所得固相沉淀物经超纯水反复洗涤至中性并离心分离得到白色沉淀物，然后将洗涤后的固相物置于瓷盘中并放于70℃烘箱干燥72h，所得的产物进行推存，即实现氟在环境中长期稳定化推存。
本发明利用氟离子可以替代羟基(-OH)进入羟基磷灰石晶格，形成氟磷灰石的完全类质同像固溶体。利用该方法合成的氟磷灰石固溶体具有低成本，易操控，能够实现氟在环境中的长期稳定化推存等优点。
附图说明
图1为本发明氟磷灰石固溶体XRD图，其中氟磷灰石标准卡片PDF#015-0876。
图2为本发明氟磷灰石固溶体扫描电镜图。
图3为本发明氟磷灰石固溶体傅里叶变换红外光谱图。
图4为本发明氟磷灰石固溶体在pH＝2.0，温度为25、35和45℃条件下溶解浸出氟的浓度变化图。
具体实施方式
实施例1
首先利用氮气对超纯水进行脱气，0.2mol/L Ca(NO3)2溶液，0.2mol/L NaF溶液，0.2mol/L(NH4)2HPO4溶液，然后，取500mL 0.2mol/L Ca(NO3)2溶液于聚乙烯瓶中，调节恒温加热搅拌器转速为500～550rmp，温度为20℃，以5mL/s的速度加入100mL 0.2mol/L NaF溶液，并持续搅拌3～5min，最后在搅拌器转速为800～850rmp下加入300mL 0.2mol/L(NH4)2HPO4溶液，同时加向聚乙烯瓶中加入浓氨水，快速将pH调至8.0后持续在20℃下搅拌25～30min，待溶液完全混匀后，盖好瓶盖并放入373.15K条件下恒温水浴锅中加热2d，待反应完全后，取出样品自然冷却，即可制得氟磷灰石固溶体。将制得的沉淀物进行固液分离，固相沉淀物用超纯水反复洗涤至中性，然后在70℃下干燥72h，得到高度结晶的氟磷灰石固溶体。
浸出测试：pH为2.00，温度为25℃条件下溶解240d，氟浸出浓度0.2340mmol/L；
pH为2.00，温度为35℃条件下溶解240d，氟浸出浓度0.2535mmol/L；
pH为2.00，温度为45℃条件下溶解240d，氟浸出浓度0.2769mmol/L；
pH为2.00，温度为25℃条件下溶解270d，氟浸出浓度0.2280mmol/L；
pH为2.00，温度为35℃条件下溶解270d，氟浸出浓度0.2517mmol/L；
pH为2.00，温度为45℃条件下溶解270d，氟浸出浓度0.2744mmol/L；
pH为2.00，温度为25℃条件下溶解300d，氟浸出浓度0.2342mmol/L；
pH为2.00，温度为35℃条件下溶解300d，氟浸出浓度0.2507mmol/L；
pH为2.00，温度为45℃条件下溶解300d，氟浸出浓度0.2813mmol/L。
Claims (2)
1.一种氟磷灰石固溶体合成方法，其特征在于具体步骤为：
(1)首先利用氮气对超纯水进行脱气，然后配制0.2mol/L Ca(NO3)2溶液，0.2mol/L NaF溶液，0.2mol/L(NH4)2HPO4溶液；
(2)量取500mL 0.2mol/L Ca(NO3)2，并将其倒入干净的1000mL聚乙烯瓶中；
(3)将聚乙烯瓶放置于恒温加热搅拌器，并调节搅拌器转速为500rmp，温度为20℃；
(4)向(3)聚乙烯瓶中以5mL/s的速度加入100mL 0.2mol/L NaF溶液，并在转速为500rmp下搅拌5min；
(5)调节搅拌器转速为800rmp，并将300mL 0.2mol/L(NH4)2HPO4溶液加入聚乙烯瓶中，同时向聚乙烯瓶中加入浓氨水，快速将pH调至8.0后持续在20℃下搅拌30min；
(6)待溶液完全混匀后，盖好瓶盖并放入373.15K条件下恒温水浴锅中加热2d；
(7)待反应完全后，取出样品自然冷却，得到氟磷灰石固溶体。
2.一种如权利要求所述方法合成氟磷灰石固溶体的应用，其特征在氟磷灰石固溶体应用于实现氟在环境中长期稳定化推放，则具体步骤为：
在100℃下反应完成后进行固液分离，所得固相沉淀物经超纯水反复洗涤至中性并离心分离得到白色沉淀物，然后将洗涤后的固相物置于瓷盘中并放于70℃烘箱干燥72h，所得的产物进行推存，即实现氟在环境中长期稳定化推存；
分别称量2.0000g氟磷灰石固溶体于3个100mL聚乙烯瓶中，然后向每个聚乙烯瓶中加入100mL初始pH＝2.0的HNO3溶液，加盖分别置于25、35和45℃恒温水浴锅中；
当置于25、35和45℃恒温水浴锅中达240天时，分别从3个聚乙烯瓶中取5mL样品，测定溶液中氟的浓度，再向聚乙烯瓶中补回5mL pH＝2.0的HNO3溶液，放回相应的恒温水浴锅中；当溶解达到270天时，取样方法与240天相同；当溶解达到300天时，取上清液测定氟的浓度；
氟磷灰石应用于pH＝2.0，温度为25、35和45℃条件下，其测定氟的结果为：pH为2.00，温度为25℃条件下溶解240d，氟浸出浓度0.2340mmol/L；温度为35℃条件下溶解240d，氟浸出浓度0.2535mmol/L；温度为45℃条件下溶解240d，氟浸出浓度0.2769mmol/L；温度为25℃条件下溶解270d，氟浸出浓度0.2280mmol/L；温度为35℃条件下溶解270d，氟浸出浓度0.2517mmol/L；温度为45℃条件下溶解270d，氟浸出浓度0.2744mmol/L；温度为25℃条件下溶解300d，氟浸出浓度0.2342mmol/L；温度为35℃条件下溶解300d，氟浸出浓度0.2507mmol/L；温度为45℃条件下溶解300d，氟浸出浓度0.2813mmol/L。
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Application publication date: 20210101 Assignee: Guangxi Huayuan Environmental Protection Technology Co.,Ltd. Assignor: GUILIN University OF TECHNOLOGY Contract record no.: X2023980044226 Denomination of invention: A Method for Preparing Fluorophosphatite Solid Solution and Its Application Granted publication date: 20230505 License type: Common License Record date: 20231023 Application publication date: 20210101 Assignee: Guangxi Borui Engineering Management Consulting Co.,Ltd. Assignor: GUILIN University OF TECHNOLOGY Contract record no.: X2023980044225 Denomination of invention: A Method for Preparing Fluorophosphatite Solid Solution and Its Application Granted publication date: 20230505 License type: Common License Record date: 20231023 Application publication date: 20210101 Assignee: Guangxi Borui Engineering Management Consulting Co.,Ltd. Assignor: GUILIN University OF TECHNOLOGY Contract record no.: X2023980044176 Denomination of invention: A Method for Preparing Fluorophosphatite Solid Solution and Its Application Granted publication date: 20230505 License type: Common License Record date: 20231024 Application publication date: 20210101 Assignee: Guangxi Huayuan Environmental Protection Technology Co.,Ltd. Assignor: GUILIN University OF TECHNOLOGY Contract record no.: X2023980044168 Denomination of invention: A Method for Preparing Fluorophosphatite Solid Solution and Its Application Granted publication date: 20230505 License type: Common License Record date: 20231024 |
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