CN100569658C - 碳酸锆钠和碱式碳酸锆及其制备方法 - Google Patents

碳酸锆钠和碱式碳酸锆及其制备方法 Download PDF

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CN100569658C
CN100569658C CNB018217664A CN01821766A CN100569658C CN 100569658 C CN100569658 C CN 100569658C CN B018217664 A CNB018217664 A CN B018217664A CN 01821766 A CN01821766 A CN 01821766A CN 100569658 C CN100569658 C CN 100569658C
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zirconium carbonate
sodium zirconium
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zirconium
sodium
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雷蒙德·J·王
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Renal Solutions Inc
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Abstract

公开了一种生产碳酸锆钠的方法，该法包括形成氯氧化锆与纯碱的混合物而后在足够的温度下加热足够的时间以形成碳酸锆钠。随后的洗涤和过滤步骤进一步构成了本发明方法的一部分。还公开一种新型的碳酸锆钠，它含有约2wt%～约5wt%的Na+；约44wt%～约50wt%的ZrO2；约12wt%～约18wt%的CO3 2-；和约30wt%～约40wt%的H2O或LOD。还公开了生产碱式碳酸锆的方法，该方法包括用酸性试剂滴定碳酸锆钠含水浆料至pH约3.5～4.0，其中固体形式的碳酸锆钠具有的水分约15%～约25%LOD。该方法还包括用水洗涤含有所形成的碱式碳酸锆的含水浆料。进一步公开了一种新型的碱式碳酸锆，它具有约30～约35mg/PO4-P/gmSZC的最小吸附容量；约2～约4mEqCO3-gm/SZC的最小HCO3-含量；可浸取的Na+约1.5～约2.0mEqNa+/gmSZC；和/或滴定过的碳酸锆钠pH约6～约7。还公开了一种生产磷酸锆的方法，该方法包括用苛性钠处理碳酸锆钠以形成碱性含水氧化锆，随后对其进行加热并与磷酸混合，以获得酸性磷酸锆，再用苛性钠对其加以滴定，以获得所要求的磷酸锆。还公开了新型的磷酸锆以及上述含锆材料的用途。

Description

碳酸锆钠和碱式碳酸锆及其制备方法
本发明是于2000年11月28日提出的U.A.专利申请号09/723,396的连续申请中的一部分，在此作为参考文献全文引入。
发明背景
本发明涉及碳酸锆钠、磷酸锆和碱式碳酸锆以及这些化合物的制备方法。
碳酸锆钠(SZC)是一种无定形锆的聚合化合物，其结构式如下：
Figure C0182176600041
滴定前SZC的分子结构
(NaZrO2CO3·nH2O)
上述颗粒状的碳酸锆钠可以通过下列两种方法获得：
方法A：颗粒碱式硫酸锆与饱和纯碱溶液反应，接着洗涤所得到的产品以除去硫酸盐。
方法B：使通过可溶性锆盐溶液与过量的纯碱溶液混合而形成的亚稳态碳酸锆钠溶液进行可控的聚合颗粒生长反应。
颗粒SZC的一种工业用途是把这种化合物转化成碱式碳酸锆(ZBC)，它在制备其它锆化学产品中是一种工业原料。完成所述的转化是通过用酸滴定颗粒状的SZC直到pH为3.5～4.0，以除去过量的碳酸钠。用于生产ZBC的颗粒SZC通常是由方法A生产的。SZC的另一个重要用途是把所述化合物转化成颗粒锆化学离子交换剂，即，磷酸锆(ZrP)和含水氧化锆(HZO)。这些锆离子交换材料在商业上用于肾透析。决定其生产方法的质量和经济标准，构成了制作目前用于血液透析再生用的
Figure C0182176600042
吸附剂筒工艺，由SORBTM技术有限公司(俄克拉何马州，俄克拉何马城)所生产。有关SORBTM技术有限公司在腹膜透析(PD)体液再生用的吸附剂筒设计方面的最新研究表明，颗粒SZC由于其具有独自的性质，使它在影响吸附剂PD筒效能上比HZO更为有利。下面概述有关制作适合PD治疗症状的吸附剂筒材料的性质如下：
1.材料具有足够的磷酸盐吸附能力，以除去用于治疗肾病患者的高磷血症患者体液中的磷酸盐。
2.材料补充PD体液的碳酸氢盐，这对于矫正患者的代谢酸中毒是重要的。
3.材料可以防止PD体液的pH下降，pH的下降会引起患者碳酸氢盐的缺失。这点使再生的PD成为可能的。
为了生产用作吸附剂PD的颗粒SZC，要考虑质量和经济两种因素。不使用方法A是因为这种方法的产品硫酸盐含量高，这会降低材料用作吸附剂时的质量。通过使用酸性硫酸锆四水合物(AZST)作锆原料的方法B已用于生产中。就这种方法而言，方法的效率低且其制造费用高，然而由颗粒SZC制成的ZrP所具有的铵吸附容量高于由碱式硫酸锆(ZBS)制成的ZrP。
尽管这些方法都可以使用，但仍有必要提供一种尤其是在透析领域中使用的质量更好的碳酸锆钠和碱式碳酸锆，另外也有必要降低这些化合物的生产费用。
发明概述
本发明的特征在于提供一种改进的碳酸锆钠。
本发明的另一特征在于提供生产所述碳酸锆钠的改进方法。
本发明的又一特征在于提供一种生产碱式碳酸锆的方法。
还有，本发明的特征在于提供多种生产碱式碳酸锆的方法。
本发明的另一特征在于提供改进的磷酸锆和生产磷酸锆的方法。
本发明的另外特征在于提供更经济的生产碳酸锆钠、磷酸锆和碱式碳酸锆的方法以及提供能产生质量更好的产品的方法。
本发明另外的特征和优点将陈述于说明书部分中，根据说明书部分将会明白，或者通过实施本发明而获悉。借助于撰写的说明书和所附的权利要求书中特别指出的要素及其组合，本发明的目的和其它的优点将得以实现和获得。
为了获得种种优点和根据本发明的目的，正如本发明具体和广泛说明的，本发明涉及生产碳酸锆钠的方法，该法包括在足够的温度下加热氯氧化锆与纯碱并以足够的时间以生成碳酸锆钠。优选的是，纯碱是呈含水浆料或溶液的形式，而氯氧化锆是呈粉末或溶液的形式。在加热前，氯氧化锆和纯碱优选进行搅拌，或者通过其它的方式进行混合，以便在环境温度，如室温下形成溶液混合物。在加热步骤后，洗涤碳酸锆钠以除去杂质和任何的氯化物。
碳酸锆钠在开始制备后要经过滴定。优选是，碱性浆料含有碳酸锆钠，采用至少一种酸性试剂，如酸而进行滴定，使pH低于7.0。其它更多的步骤也可以在这一方法中使用，如过滤，洗涤和干燥步骤。
本发明还涉及一般的碳酸锆钠和优选的碳酸锆钠，优选的碳酸锆钠，按碳酸锆钠的重量计，含有
约2wt％～约5wt％的Na+；
约44wt％～约50wt％的ZrO2；
约12wt％～约18wt％的CO3 2-；和
约30wt％～约40wt％的LOD。
另外，本发明涉及生产碱式碳酸锆的方法，该方法包括用酸性试剂滴定碳酸锆钠含水浆料至pH约3.5～约4。用于制备所述浆料的碳酸锆钠的所含水分最好约15wt％～约25wt％LOD。在滴定后，含水浆料用水洗涤。然后通过各种技术从浆料中回收湿粉状的碱式碳酸锆。
此外，本发明涉及碱式碳酸锆钠，其优选的特征在于按固体粉末的组合物(最终产品)的wt％计，
Na+含量低于约1000ppm；
ZrO2含量约35wt％～约40wt％；和
CO3 2-含量约8wt％～约10wt％。除非另有说明，本申请中所有的％和wt％都是基于最终产品的重量计。
本发明还涉及生产磷酸锆的方法，该方法包括在足够的温度下加热氯氧化锆和纯碱足够的时间以生成碳酸锆钠，并用苛性钠处理碳酸锆钠以生成碱性含水氧化锆。之后，加热呈浆料状的碱性含水氧化锆，并加入酸性试剂如磷酸。加热后，冷却浆料并把酸性磷酸锆过滤并加以洗涤，以降低未反应的可浸取的磷酸盐量。然后用酸性磷酸锆制成含水浆料，用碱性试剂，如苛性钠，滴定所述浆料到pH达到预定值，如约5～约6。之后，滴定过的产品，即滴定过的磷酸锆，进行过滤并洗涤以优选降低可浸取的钠离子。之后，干燥磷酸锆成为自由流动的粉末，优选其水分约为12～约18％LOD。
本发明还涉及新型的磷酸锆，以磷酸锆的重量计，它优选具有H+含量约1.4wt％～2.0wt％；Na+wt％含量约4wt％～约6wt％；ZrO2wt％含量约34wt％～约37wt％；PO4-wt％含量约41wt％～约43wt％；和LODwt％约14wt％～约18wt％。本发明的磷酸锆优选对铵、Ca2+、Mg2+、K+和有毒重金属具有良好的吸附容量。优选的是，磷酸锆没有残留的硫酸盐或氯化物并满足透析用或其它离子交换用所要求的其它特征。
应该理解的是，上面一般性的描述和下面详细的描述都只是示范性和说明性的，并且用于提供对本发明作进一步的阐述，正如所要求保护的。
引入并构成本发明一部分的附图，说明本发明的具体实施方案并与说明书一起，作为解释本发明的原理。
附图简述
图1是说明制备碳酸锆钠的一个具体实施方案的示意图。
本发明的详细说明
本发明涉及生产碳酸锆钠的方法和涉及生产碱式碳酸锆和磷酸锆的方法。在各种场合下，原料优选为氯氧化锆。本发明进一步涉及新型的碳酸锆钠、磷酸锆和碱式碳酸锆。碳酸锆钠、碱式碳酸锆和磷酸锆作为原料可以用于各种工业用途中，并且还可以用于肾透析以及其它的分离应用中。
更详细地说，在本发明的一个具体实施方案中，本发明涉及一种生产碳酸锆钠的方法。该方法包括在足够的温度下加热氯氧化锆和纯碱足够的时间以生成碳酸锆钠。加热前，可部分或全部形成碳酸锆钠。
优选的是，纯碱是以含水浆料或溶液的形式存在。用于形成溶液或浆料的纯碱的用量最好是制成含纯碱的饱和溶液或浆料的用量。例如，每升水约260克～约920克的纯碱可用来制取饱和溶液或浆料。
氯氧化锆优选具有分子式ZrOCl2·8H2O并且从Teledyne Wah Chang公司、Dastech国际有限责任公司和Zirconia Sales有限责任公司那样的来源可以购得。优选的是，氯氧化锆和纯碱的重量比约3.0∶1～约4.0∶1；更好的约3.5∶1～约4.0∶1；最好的约3.6∶1。
氯氧化锆优选以粉末或溶液的形式存在。如以溶液的形式存在，氯氧化锆优选每升水含有约400克的氯氧化锆。
对于上述方法，优选的是，在加热步骤前，优选在环境温度，如室温(例如，约40°F～约110°F)下，搅拌氯氧化锆和纯碱或通过其它方式加以混合，以形成溶液混合物。有关加热步骤前所获得的亚稳态碳酸锆钠溶液而言，当将氯氧化锆(溶液或固体)加到纯碱溶液中时，优选形成碳酸锆的凝胶状沉淀。由于该物质是两性的，因此碳酸锆在室温下能再次溶解于过量的纯碱溶液中，以优选形成亚稳态的碳酸锆钠(碱性)溶液。当优化ZrOCl2·8H2O与纯碱的混合比时，混合温度优选保持在约90°F～约95°F的范围内(可借助于混合过程所产生的反应热量)，优选使该物质完全溶解以形成清澈的溶液。在室温下贮存数小时时，溶液在沉淀开始形成时变得浑浊。起始溶液的浑浊度并不影响产品的粒度和回收率％。尽管如此，优选的是，在形成后立即开始加热亚稳态SZC溶液。在加热步骤中，约150°F下SZC优选由于饱和而开始沉淀。当持续加热时，聚合的SZC粒子在碳酸锆钠的最终温度(沸腾)下开始生长成30～50微米的粒径。优选的是，足够的温度是氯氧化锆与纯碱混合物的沸腾温度。例如，加热的温度可以在约150°F～250°F(在压力下过热)下持续约2小时。在最终温度时的平衡时间约2小时。最高的加热温度和最长的加热时间影响所得到的粒径。当加热碳酸锆钠和纯碱时，混合物的优选加热速率约0.5°F～约1°F/分钟，直至混合物沸腾。在压力下加热混合物可使混合物达到过热的温度。
优选的是，在室温下用于获得混合物的搅拌或其它混合方式能导致生成清澈的亚稳态的溶液。在加热步骤的过程中，最好对混合物进行缓慢的搅拌或通过其他方式混合以得到改进的颗粒。
在上述方法中，并且在加热步骤后，碳酸锆钠的温度可以从沸腾温度降至约150°F或更低的温度。过滤含有碳酸锆钠的这种产品的溶液，回收优选为颗粒状的碳酸锆钠。水的分离可以通过任何一种标准过滤技术来完成，例如使用离心或过滤。之后，过滤后的碳酸锆钠可用水，如RO水进行洗涤，以除去任何来自碳酸锆钠的氯化物或其它杂质。通常，许多这些杂质都来源于纯碱。
作为所述方法的优选部分，作为可选择方案，可以使用至少一种酸性试剂滴定含碳酸锆钠的碱性浆料，直至pH低于约7，较好的pH约3.5～约6.0，最好的pH约6.0。用于滴定的酸性试剂可以是任何能降低碱性浆料pH的试剂，较好的是酸，最好的是HCl，如1N的HCl。滴定后，如前所述可过滤碳酸锆钠，并且可以任选地使用例如RO水进行洗涤。洗涤步骤优选降低可浸取的Na+含量。
在使用或不用任选步骤，但优选使用任选步骤下，从上述方法回收的碳酸锆钠(SZC)通常是洗涤过的碳酸锆钠的滤饼。这种碳酸锆钠优选经过干燥，并通常干燥足够时间以形成自由流动的粉末。可以采用任何技术实现干燥，如放置滤饼于盘上再于一炉内进行干燥。优选干燥温度在约100°F～约150°F的范围内。其它的温度也可以使用。在碳酸锆钠干燥的过程中，最终所能达到的水分优选约10％LOD～约60％LOD，更好的约30％LOD～约35％LOD。图1陈述了一种生产SZC的优选方法。
回收的碳酸锆钠优选具有约30微米～约50微米的平均粒径，而其它的粒径也能获得。
本发明的最终形式的碳酸锆钠，以碳酸锆钠的重量计，优选具有约2wt％～约5wt％的Na+；约44wt％～约50wt％的ZrO2；约12wt％～约18wt％的CO3 2-；和约30wt％～约40wt％的LOD，较好的约32wt％～约35wt％的LOD。LOD是干燥过程中损失的SZC的wt％并大部分是H2O。
本发明的碳酸锆钠进一步优选满足ANSI/AAMI RD-5-1992对可浸取有毒杂质所作的标准。
优选的是，本发明的碳酸锆钠能进一步达到下列性能或特性中的一种或多种：
-具有约30～约35mgPO4-P/gmSZC的最小磷酸盐吸收容量；
-约2～约4mEq HCO3 -/gmSZC的最小HCO3 -含量；
-约1.5～约2.0mEqNa+/gmSZC的最大可浸取Na+含量；
-和/或滴定过的碳酸锆钠为约6～约7的pH。
优选的是，本发明的碳酸锆钠具有至少一种上述特性，更好的是具有至少两种或三种特性，最好是具有上述所有的特性。
在一般的和优选的碳酸锆钠中，如上述优选的SZC优选通过提供足够的磷酸盐吸附容量，以经济地用作治疗例如肾病患者的高磷血症的临床吸附剂，而能为腹膜透析或血液透析提供所必须的效能的所要求条件。此外，本发明的碳酸锆钠还能在应用过程中为腹膜透析体液或血液透析体液提供特异的碳酸氢盐含量。如上所述，本发明进一步具有最小的可浸取的Na+。
在颗粒状SZC的生产中，产品的粒径和回收率％对于方法的效能，特别是经济性，方法的效率(洗涤，过滤)和产品的质量是重要的。较大的粒径有可能提高聚合颗粒在洗涤过程中抗磨损的稳定性以及改进过滤效率。在晶体生长反应过程中，颗粒的稳定性优选受控于亚稳态SZC溶液的ZrO2％，溶液中纯碱与ZrO2的比例，反应的加热速率，最高的加热温度和加热时间。以30～40微米范围内的粒径回收92～98％的产品可以通过调节以下工艺参数而实现：
表1
  SZC亚稳态溶液的ZrO<sub>2</sub>％   5.5～7.0％
  溶液中纯碱与ZrO<sub>2</sub>的反应比   按重量计3.6∶1
  颗粒生长反应的加热速率   0.5°F～1/°F/min
  最高加热温度   沸腾～过热(在压力下)
  在最高温度下的连续加热时间   2小时
滴定至3～8范围内的不同pH值的SZC，具有表2所概述的各种质量。筒效能试验表明，在材料试验时，例如在PD用的筒中SZC的pH7～8，在初始筒流中可能引起磷酸盐的泄漏和Na+和pH的峰值。
表2
作为pH函数对透析用颗粒SZC的质量变化
  SZCpH   磷酸盐吸附   可浸取的Na<sup>+</sup>含量   HCO<sub>3</sub><sup>-</sup>含量
  3.5   35.12mgPO<sub>4</sub>-P/gm   -   -
  5.0   -   0.87mEq/gm   2.1mEq/gm
  6.0   33.9mgPO<sub>4</sub>-P/gm   1.88mEq/gm   3.05mEq/gm
  8.0   33.5mgPO<sub>4</sub>-P/gm   -   -
低pH值有利于磷酸盐的吸收和降低可浸取的Na+，但这还能降低用作吸附筒材料的碳酸氢盐含量和缓冲能力。因此，正如筒效能试验所证实的，pH6.0～6.5应当是优选的范围。滴定后，为了控制可浸取的Na+含量，材料应当用大量的RO水进行洗涤直到总溶解固体量低于300ppm。
滴定和洗涤后的滤饼应当在适度的温度(例如100°F～150°F)下进行盘式干燥直到优选水分为约30～35％LOD。最终产品优选不过干，以防止碳酸氢盐的损失。如表3所示，对不同水分的干燥也能影响磷酸盐的吸附容量。最后，干燥过的产品应当储存在密闭的容器内，以避免水分和碳酸氢盐含量的损失。
表3
作为颗粒SZCpH6.0的水分量的函数对磷酸盐吸附容量的变化
  水分(％LOD)   磷酸盐吸附容量mgPO<sub>4</sub>-P/gmSZC
  10.6％   21.44
  14.9％   22.24
  21.0％   24.0
  28.3％   27.36
  36.7％   28.8
  42.9％   30.16
  51.6％   29.12
  57.9％   28.72
筒效能试验表明滴定至pH6.0并干燥至水分达30～35％LOD的颗粒ZSC，具有足够的磷酸盐吸附容量，完全可以除去8小时治疗过程中PD体液中的尿毒症毒素。材料还具有足够的碳酸氢盐，以保证能维持透析全过程的体液pH。初始筒流体中的Na+和pH峰值的水平总是可以允许的并且还能通过透析前的起动而消除。
另外，本发明还涉及生产碱式碳酸锆的方法，碱式碳酸锆优选具有以下化学式：
Figure C0182176600111
在生产碱式碳酸锆时，先用酸性试剂，例如酸(多种)滴定碳酸锆钠的含水浆料至pH在约3.5～约4.0的范围内。在把碳酸锆钠加到含水浆料前，其固体形式优选具有的水分约15％～25％LOD，较好的约15％～约20％LOD。尽管任何的碳酸锆钠都可以使用，但优选使用由上述方法所制成的碳酸锆钠。
滴定后，含水浆料优选用例如RO水洗涤。之后，从浆料中回收湿粉状的碱式碳酸锆。碱式碳酸锆的回收可以通过任何回收技术进行，例如真空过滤或离心或其它方式。用于滴定的酸性试剂可以是任何能降低上述pH的试剂，但最好使用稀HCl或HNO3或其它酸或其混合物。优选的是，在任何最终回收碱式碳酸锆前，碱式碳酸锆的最终洗涤都在于除去任何的钠。
还有，作为本发明的一部分，本发明涉及一般的碱式碳酸锆和优选的新型碱式碳酸锆，它基于碱式碳酸锆的重量计，具有Na+含量低于约1000ppm；
ZrO2的含量约35wt％～约40wt％；和
CO3 2-的含量约8wt％～约10wt％。
优选的是，碱式碳酸锆基本上不含SO4 2-，也基本上不含Cl-，例如低于约0.01wt％。
还有，碱式碳酸锆可以用于各种工业应用中以及吸附剂的应用中。
至于生产磷酸锆的方法，该方法包括与用于生产碳酸锆钠所用步骤相类似的步骤。上述讨论的和在碳酸锆钠起始加热步骤和任选过滤和洗涤后所获得的碳酸锆钠，都可用于本法中以制成本发明的磷酸锆。换句话说，另外的氯氧化锆也可以按上述讨论过的制取碳酸锆钠的方式进行加工处理，所得的碳酸锆钠也可以经过下面所述的后面步骤以获得所要求的磷酸锆。
在生产本发明的磷酸锆中，碳酸锆钠优选是通过在足够的温度下加热氯氧化锆与纯碱足够的时间而制成的碳酸锆钠。优选的原料、温度和时间与上述有关生产碳酸锆钠是相同的。所制成的碳酸锆钠优选冷却至例如约150°F的温度，并任选经过过滤和洗涤。之后，碳酸锆钠用苛性钠或其它的合适试剂进行处理以形成碱性含水氧化锆。该含水氧化锆能以浆料的形式，与一种酸性试剂，例如磷酸，最好优选以比例1∶1稀释的工业级磷酸与碱性含水氧化锆一起，例如在一个反应容器里，在足够的温度下加热足够的时间。优选的是，加热温度如上所述约180°F约～约185°F并持续1小时。之后，把产品冷却至最好约150°F的温度，再以酸性磷酸锆(H+ZrP)过滤。酸性磷酸锆优选用RO水洗涤一次或多次，以降低未反应的可浸取的磷酸盐含量。之后，用酸性磷酸锆制成含水浆料，滴定该浆料至pH值达约5～约6，优选约5.5～约6。优选的是，滴定剂是50％的苛性钠。之后，过滤和洗涤滴定过的磷酸锆，以降低可浸取的Na+，最好用RO水洗涤，以使总溶解固体达到300ppm或以下，以降低可浸取的Na+至最低逞度。
之后，干燥洗涤过的磷酸锆，以得到自由流动性粉末，其水分优选约12～约18％LOD。优选的是，只要保持粉末的完整性，干燥可在约100℃～约120℃的温度下进行，尽管其它的温度也可以使用。优选的是，粉末的粒径约30微米～约50微米，尽管基于所要求的参数也能获得其它粒径。
上述的洗涤、过滤和干燥步骤也能通过为所属技术领域的技术人员所通晓的常规技术而实现。
优选由本发明的方法获得的磷酸锆，以磷酸锆的重量计，具有下列的特性参数：
H+含量约1.4～约2.0wt％；
Na+含量约4～约6wt％；
ZrO2含量约34～约37wt％；
PO4 -含量约41～约43wt％；和
H2O含量约14～约18wt％。
另外，本发明的磷酸锆优选对铵、Ca2+、Mg2+、K+和有毒的重金属具有吸附容量。更为优选的是，吸附容量接近约20～约45mg NH4-N/gmZrP，较好约30mgNH4-N/mgZrP～约35NH4-N/mgZrP，甚至更好约30mg或更高NH4-N/gmZrP；约2～约7mEqCa2+/gmZrP，较好约3mEqCa2+/gmZrP～约5mEqCa2+/gmZrP，甚至更好约3mEqCa2+/gmZrP或更多；约1～5mEqMg2+/gmZrP，较好约2mEq Mg2+/gmZrP～约3mEq Mg2+/gmZrP，甚至更好约2mEq Mg2+/gmZrP或更多；以及就重金属(HM)而言，约3～约9mEqHM/gmZrP，较好约5mEq HM/gmZrP～约7mEq HM/gmZrP，甚至更好约6mEq HM/gmZrP或更高。
此外，磷酸锆优选具有Na+含量约2mEq Na+/gmZrP～约3mEqNa+/gmZrP，较好约2.4mEq Na+/gmZrP，而pH约5.5～约6。其它的pH值和Na+含量也可以使用。
还有，本发明的磷酸锆对于该材料来说优选具有最小的可浸取PO4 3-，较好的是低于约0.05mg％PO4 3-/gmZrP。
此外，磷酸锆的平均粒径优选约30～约40微米，没有残留的硫酸盐或氯化物(例如低于0.01％)。此外，磷酸锆优选满足ANSI/AAMI RD-5-1992在可浸取有毒杂质方面的标准，并其在水中时的pH值约6～约7。正如早已说明的，磷酸锆可以在各种分离装置，例如透析分离器中使用。
通过下列的实施例本发明将得到更进一步的阐明，这些实施例单纯用于举例以说明本发明。
实施例
实施例1
将789克的纯碱溶于3升的去离子水中。在搅拌下，将610克的ZrOCl2粉末加到纯碱溶液中。持续搅拌一直到固体完全溶解而形成亚稳态的溶液。将该亚稳态溶液以每10分钟升温6～10°F的速率缓慢加热直到沸腾或过热温度(在压力下)。在平衡温度下持续加热1.5～2小时。在约150°F开始形成的SZC颗粒，在平衡过程中继续生长到粒径为30～50微米。缓慢的搅拌能使粒子生长得更好。在加热后，把产品浆料冷却至约120°F。过滤出颗粒状的SZC，滤饼用去离子水洗涤，以除去氯化钠和过剩的碳酸盐。发现SZC湿滤饼的产率为862克，由亚稳态溶液回收的ZrO2％为95％。
将SZC湿滤饼放回盛于烧杯中的500ml去离子水中。在搅拌下，用3N的HCl滴定所述浆料。在该pH值下继续保持平衡30分钟，之后再将pH调节至6.0。过滤出滴定过的SZC并用去离子水洗涤，直到滤液中的总溶解固体低于300ppm。在适度的温度下(约150°F)于盘式干燥器干燥洗涤过的滤饼直到水分约30％，形成自由流动性粉末。
实施例2：由氯氧化锆合成ZrP
在搅拌下，将实施例1所得洗涤的SZC湿滤饼，搅拌下转移至500ml的10％NaOH中。碱处理持续半小时。然后过滤并用去离子水简单地洗涤。将滤饼转移至反应器内的1升的去离子水中。将浆料加热至约185°F。把1200gm1∶1经稀释的磷酸(与等体积水混合的600gm76％的H3PO4)缓慢地加到加热过的浆料中直到添加完毕。在190°F～195°F下持续加热1小时。然后把产品浆料冷却至150°F，过滤并用去离子水洗涤以除去过量的磷酸盐。把如此制得的酸性ZrP置于500ml去离子水中用50％NaOH滴定至pH5.75。过滤滴定过的ZrP，并用去离子水漂洗，以除去可浸取的Na+，直到滤液中的总溶解固体低于300ppm。滴定过的ZrP湿滤饼，在洗涤后，采用盘式干燥器干燥至水分为14～18％，以形成自由流动性粉末。
由本文公开的本发明的说明书和实施，本发明的其它具体实施方案对所属技术领域的技术人员来说将是明显的。说明书和实施例仅供列举说明，本发明的真实范围和精神由所附的权利要求和其等同物所说明。

Claims (22)

1.一种生产由下式表示的碳酸锆钠的方法，该方法包括在足够的温度下加热氯氧化锆与纯碱的混合物足够的时间以生成所述的碳酸锆钠，其中所述温度为150°F～250°F，其中所述纯碱是呈含水浆料或溶液形式
Figure C018217660002C1
2.按权利要求1所述的方法，进一步包括，在所述加热之前，在环境温度下搅拌氯氧化锆与纯碱以形成溶液混合物。
3.按权利要求1所述的方法，其中氯氧化锆与纯碱的重量比为3.0∶1～4.0∶1。
4.按权利要求3所述的方法，其中所述重量比为3.5∶1～4.0∶1。
5.按权利要求3所述的方法，其中所述重量比为3.6∶1。
6.按权利要求1所述的方法，其中所述氯氧化锆是呈粉末或溶液形式。
7.按权利要求1所述的方法，其中加热进行2小时。
8.按权利要求1所述的方法，进一步包括，在所述加热后，滤出所述碳酸锆钠。
9.按权利要求8所述的方法，进一步包括，在过滤后，由所述碳酸锆钠中洗出任何杂质。
10.按权利要求9的方法，其中所述杂质为氯化物。
11.按权利要求1所述的方法，进一步包括，加热后，用至少一种酸性试剂滴定含所述碳酸锆钠的碱性浆料以使pH低于7.0。
12.按权利要求11所述的方法，其中所述pH为3.5～6.0。
13.按权利要求11所述的方法，其中所述pH为6。
14.按权利要求11所述的方法，进一步包括，在滴定后，滤出所述碳酸锆钠并洗涤所述碳酸锆钠。
15.按权利要求14所述的方法，进一步包括，洗涤后，干燥所述碳酸锆钠。
16.按权利要求15所述的方法，其中所述干燥进行足够的时间以形成自由流动的粉末。
17.按权利要求15所述的方法，其中在所述干燥后，所述碳酸锆钠具有的水分为10％LOD～60％LOD，其中LOD是干燥过程中损失的碳酸锆钠的wt％。
18.按权利要求17所述的方法，其中所述水分为30％LOD～35％LOD。
19.按权利要求16所述的方法，其中所述碳酸锆钠具有平均粒径30微米～50微米。
20.按权利要求1所述的方法，其中所述加热是以0.5°F～1°F/分钟的加热速率进行直到所述混合物的沸腾温度。
21.一种生产由下式表示的碳酸锆钠的方法，该方法包括在环境温度下混合和搅拌氯氧化锆与纯碱以形成溶液混合物；在足够的温度下加热所述溶液混合物足够的时间以形成所述碳酸锆钠，其中所述足够的温度是氯氧化锆与纯碱形成的溶液混合物的沸腾温度；在所述加热后，滤出碳酸锆钠；过滤后，由所述碳酸锆钠中洗出任何杂质；使用至少一种酸性试剂滴定含有所述碳酸锆钠的碱性浆料以使pH低于7.0；滴定后，滤出所述碳酸锆钠并洗涤所述碳酸锆钠；以及在洗涤后，干燥所述碳酸锆钠，其中所述温度为150°F～250°F，
Figure C018217660003C1
22.按权利要求21所述的方法，其中所述杂质为氯化物。
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