CN112158821A - 一种镉-氟磷灰石固溶体制备方法及其应用 - Google Patents
一种镉-氟磷灰石固溶体制备方法及其应用 Download PDFInfo
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Abstract
本发明公开了一种水热法合成镉‑氟磷灰石固溶体的方法。先使用氮气对超纯水进行脱气，再配制0.2mol/L硝酸镉溶液作为基础液，将氟化钠溶液加入至硝酸镉溶液中并充分混匀，以15s的时间间隔分3次连续将磷酸氢二胺加入至硝酸镉和氟化钠的混合溶液中，最后加入浓氨水，调节pH至7.5后持续在室温下搅拌，将其放入373.15K条件下水浴48h，最后取出样品，得到结晶度高、稳定性好的镉‑氟磷灰石固溶体。取适量镉‑氟磷灰石固溶体在不同pH和不同温度下进行溶解，掌握镉和氟在环境中的迁移、转化与富集的规律。利用该方法合成的镉‑氟磷灰石固溶体具有低成本，易操控，能够实现镉和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，涉及镉-氟磷灰石固溶体合成方法及其应用。该方法利用镉离子和氟离子可以替代钙离子和羟基(-OH)进入羟基磷灰石晶格，形成镉-氟磷灰石的完全类质同像固溶体。
背景技术
镉(Cd)，呈银白色，熔点为320.9℃，位于元素周期表第五周期IIB族，原子序数为48。镉有+1价和+2价两种价态，在环境中镉金属以+1价形态存在并不多见，而是主要以+2价的形态存在。对于镉污染主要是通过三废的排放，在环境中易被农作物吸收，并通过食物链进入到人体。当镉元素被人体吸收后，则会取代骨骼中钙，出现骨软化、骨质疏松、萎缩、变形等症状。而世界卫生组织对于镉污染的食品列为优先研究对象；联合国环境规划署提出的12种具有全球意义的危险化学物质中，然而镉元素被列为首位。镉污染主要来源于电镀、冶炼、汽车、航空、颜料、油漆和印刷等行业。2014年我国《全国土壤污染状况调查公报》指出，目前全国土壤污染超标率为16.1％，而以无机型污染占比最大，达到全部超标点位的82.8％。重金属镉是土壤主要无机污染物，占点位超标率为7.0％，对我国土壤安全造成了严重威胁。
镉-氟磷灰石属于磷酸盐类矿物，其可以发生同价或异价类质同象替换形成不同类型矿物。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镉-氟磷灰石，固定废水中的镉、磷和氟。对固定镉、磷及氟元素具有重要意义。
发明内容
本发明目的是提供一种水热合成镉-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)表征，测试在pH分别为恒定2.00、2.00、5.60和9.00以及温度分别为25、35和45℃条件下对于镉、磷和氟的浸出浓度，对溶解度和稳定性进行详细实验分析，为固定镉、磷和氟提供数据支撑。
1.一种镉-氟磷灰石混合晶体固溶体合成方法，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处理，然后配制0.2mol/L Cd(NO3)2溶液，0.2mol/L NaF溶液，0.2mol/L(NH4)2HPO4溶液；
(2)在干净的烧杯中准备500mL 0.2mol/L Cd(NO3)2溶液,并将其转移至干净的1L聚乙烯瓶中；
(3)在磁力搅拌器转速为350～400rmp条件下向(2)中以10mL/s加入100mL0.2mol/L NaF溶液，待加完NaF溶液后持续搅拌2～3min；
(4)在3个100mL的量筒中分别准备好100mL 0.2mol/L(NH4)2HPO4溶液，调节磁力搅拌器转速为650～700rmp，分别以15s的时间间隔连续将3个100mL 0.2mol/L(NH4)2HPO4溶液加入到聚乙烯瓶，待加完(NH4)2HPO4溶液后立刻向聚乙烯瓶中加入浓氨水，快速将pH调至7.5后持续在室温下搅拌10～12min；
(5)待溶液完全混匀后，在373.15K条件下水浴(陈化)48h；
(6)待反应完全后，取出样品自然冷却，通过离心分离得到沉淀物，并利用超纯水反复洗涤至中性，然后在70℃条件下干燥，得到镉-氟磷灰石固溶体。
本发明的镉-氟磷灰石固溶体的应用于实现镉、磷和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，即实现镉、磷和氟在环境中长期稳定化推存。
本发明利用镉离子和氟离子可以替代钙离子和羟基进入羟基磷灰石晶格，形成方镉-氟磷灰石的完全类质同像固溶体。利用该方法合成的镉-氟磷灰石固溶体具有低成本，易操控，能够实现镉、磷和氟在环境中的长期稳定化推存等优点。
附图说明
图1为本发明合成镉-氟磷灰石固溶体和初始pH＝2.00、5.60、9.00和25-45℃溶解7200h后的XRD图，其中镉-氟磷灰石标准卡片PDF#01-070-1207。
图2为本发明合成镉-氟磷灰石固溶体和初始pH＝2.00、5.60、9.00和25-45℃溶解7200h后的场发射扫描电子显微镜图。
图3为本发明合成镉-氟磷灰石固溶体在pH＝2.00、恒定2.00、5.60、9.00和温度为25、35和45℃溶解7200h后Cd、P和F的浸出浓度变化图。
具体实施方式
实施例1
首先利用氮气对超纯水进行脱气，然后配制0.2mol/L Cd(NO3)2溶液，0.2mol/LNaF溶液，0.2mol/L(NH4)2HPO4溶液，然后，取500mL 0.2mol/L Cd(NO3)2溶液于1L聚乙烯瓶中，将磁力搅拌器转速调为350～400rmp，以10mL/s加入100mL 0.2mol/L NaF溶液，将其搅拌2～3min充分混匀，最后调节磁力搅拌器转速为650～700rmp，分别以15s的时间间隔连续将3个100mL 0.2mol/L(NH4)2HPO4溶液加入聚乙烯瓶，待加完(NH4)2HPO4溶液后立刻向聚乙烯瓶中加入浓氨水，快速将pH调至7.5后持续在室温下搅拌10～12min，待溶液完全混匀后，盖好聚乙烯瓶瓶盖并放入373.15K条件下水浴(陈化)48h，待反应完全后，取出样品自然冷却，即可制得镉-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，得到高度结晶的镉-氟磷灰石固溶体。
浸出测试：
pH为恒定2.00，温度为25℃条件下溶解7200h，镉浸出浓度64.2647mmol/L，磷浸出浓度32.4466mmol/L，氟浸出浓,0.2411mmol/L；
pH为2.00，温度为25℃条件下溶解7200h，镉浸出浓度7.0474mmol/L，磷浸出浓度2.2127mmol/L，氟浸出浓度0.0319mmol/L；
pH为2.00，温度为35℃条件下溶解7200h，镉浸出浓度6.8037mmol/L，磷浸出浓度2.5215mmol/L，氟浸出浓度0.0278mmol/L；
pH为2.00，温度为45℃条件下溶解7200h，镉浸出浓度7.3356mmol/L，磷浸出浓度1.6821mmol/L，氟浸出浓度0.0439mmol/L；
pH为5.60，温度为25℃条件下溶解7200h，镉浸出浓度0.0427mmol/L，磷浸出浓度0.0768mmol/L，氟浸出浓度0.0853mmol/L；
pH为9.00，温度为25℃条件下溶解7200h，镉浸出浓度0.0137mmol/L，磷浸出浓度0.0904mmol/L，氟浸出浓度0.0882mmol/L。
Claims (1)
1.一种镉-氟磷灰石混合晶体固溶体合成方法，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处理，然后配制0.2mol/L Cd(NO3)2溶液，0.2mol/LNaF溶液，0.2mol/L(NH4)2HPO4溶液；
(2)在干净的烧杯中准备500mL 0.2mol/L Cd(NO3)2溶液,并将其转移至干净的1L聚乙烯瓶中；
(3)在磁力搅拌器转速为400rmp条件下向(2)中以10mL/s加入100mL 0.2mol/L NaF溶液，待加完NaF溶液后持续搅拌3min；
(4)在3个100mL的量筒中分别准备好100mL 0.2mol/L(NH4)2HPO4溶液，调节磁力搅拌器转速为700rmp，分别以15s的时间间隔连续将3个100mL 0.2mol/L(NH4)2HPO4溶液加入到聚乙烯瓶，待加完(NH4)2HPO4溶液后立刻向聚乙烯瓶中加入浓氨水，快速将pH调至7.5后持续在室温下搅拌12min；
(5)待溶液完全混匀后，在373.15K条件下水浴(陈化)48h；
(6)待反应完全后，取出样品自然冷却，通过离心分离得到沉淀物，并利用超纯水反复洗涤至中性，然后在70℃条件下干燥72h，得到镉-氟磷灰石固溶体进行推存，即实现镉、磷和氟在环境中长期稳定化推存；
(7)分别称量2.0g镉-氟磷灰石固溶体材料于3组100mL聚乙烯瓶中，向第一组分别加入pH＝2.0、恒定2.0、5.6和9.0的溶液并将其密封放置于25℃水浴锅中；向第二组加入pH＝2.0的硝酸溶液并将其密封放置于35℃水浴锅中；向第三组加入pH＝2.0的硝酸溶液并将其密封放置于45℃水浴锅中；
(8)当溶解到达300天后，从(7)中取出样品，测定其上清液镉、磷和氟的浸出浓度；结果为：pH为2.00，温度为25℃条件下溶解7200h，镉浸出浓度7.0474mmol/L，磷浸出浓度2.2127mmol/L，氟浸出浓度0.0319mmol/L；pH为恒定2.00，温度为25℃条件下溶解7200h，镉浸出浓度64.2647mmol/L，磷浸出浓度32.4466mmol/L，氟浸出浓,0.2411mmol/L；pH为2.00，温度为35℃条件下溶解7200h，镉浸出浓度6.8037mmol/L，磷浸出浓度2.5215mmol/L，氟浸出浓度0.0278mmol/L；pH为2.00，温度为45℃条件下溶解7200h，镉浸出浓度7.3356mmol/L，磷浸出浓度1.6821mmol/L，氟浸出浓度0.0439mmol/L；pH为5.60，温度为25℃条件下溶解7200h，镉浸出浓度0.0427mmol/L，磷浸出浓度0.0768mmol/L，氟浸出浓度0.0853mmol/L；pH为9.00，温度为25℃条件下溶解7200h，镉浸出浓度0.0137mmol/L，磷浸出浓度0.0904mmol/L，氟浸出浓度0.0882mmol/L；
其以上结果可知，初始pH为2.00，温度为25、35和45℃条件下0.2mol/L镉和氟溶液被矿化后，溶解7200h后氟的浸出浓度低于地表水环境质量标准(GB 3838-2002)Ⅰ类水氟离子的浓度限值，证明镉-氟磷灰石对固定氟具有较好的效果。
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