CN100482820C - 从Ti浆液中分离出Ti的方法 - Google Patents

从Ti浆液中分离出Ti的方法 Download PDF

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CN100482820C
CN100482820C CNB038212455A CN03821245A CN100482820C CN 100482820 C CN100482820 C CN 100482820C CN B038212455 A CNB038212455 A CN B038212455A CN 03821245 A CN03821245 A CN 03821245A CN 100482820 C CN100482820 C CN 100482820C
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salt
metallic particles
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metal
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CN1681951A (zh
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R·安德森
D·阿姆斯特朗
兰斯·雅各布森
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International Titanium Powder LLC
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
    • C22B9/02—Refining by liquating, filtering, centrifuging, distilling, or supersonic wave action including acoustic waves
    • C22B9/023—By filtering
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B34/00—Obtaining refractory metals
    • C22B34/10—Obtaining titanium, zirconium or hafnium
    • C22B34/12—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
    • C22B34/1218—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining titanium or titanium compounds from ores or scrap by dry processes
    • C22B34/1231—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining titanium or titanium compounds from ores or scrap by dry processes treatment or purification of titanium containing products obtained by dry processes, e.g. condensation
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B34/00—Obtaining refractory metals
    • C22B34/10—Obtaining titanium, zirconium or hafnium
    • C22B34/12—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
    • C22B34/1263—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining metallic titanium from titanium compounds, e.g. by reduction
    • C22B34/1268—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining metallic titanium from titanium compounds, e.g. by reduction using alkali or alkaline-earth metals or amalgams
    • C22B34/1272—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining metallic titanium from titanium compounds, e.g. by reduction using alkali or alkaline-earth metals or amalgams reduction of titanium halides, e.g. Kroll process
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

Abstract

公开了一种将金属颗粒物从浆液中分离出来的方法，其中所述浆液由液态金属、金属颗粒物和盐颗粒物的原始成分构成。将至少部分液态金属除去以浓缩所述金属和盐颗粒物，然后，将液态金属或原始盐组成物液体或其混合物在高于原始盐组成物的熔点的温度下通过颗粒物，以进一步浓缩所述金属颗粒物。然后将金属颗粒物从剩余的原始组成物或盐组成物混合物中分离出来。还利用了液态金属和盐之间的密度差异以促进分离。

Description

从Ti浆液中分离出Ti的方法
相关申请
根据37C.F.R.1.78(c)，本申请要求于2002年9月7日提交的美国临时申请No.60/408932、于2002年9月7日提交的美国临时申请No.60/408925、于2002年9月7日提交的美国临时申请No.60/408933的优先权。
背景技术
本发明涉及从运行Armstrong工艺和方法来生产产品的过程中所生成的浆液中分离不需要的组分，所述Armstrong工艺和方法如美国专利申请5779761、5958106和6409797所公开，所述申请的公开内容在本文中引入作为参考.如上述确认并引入的专利申请所示，其中公开的连续工艺例如通过用过量的钠还原四氯化钛从而得到钛或钛合金。存在于反应器中的产品蒸汽为液态金属、盐颗粒或粉末、以及作为颗粒物或粉末的钛金属或金属合金的浆液.应当理解，本发明涉及可以根据Armstrong工艺得到的任一材料.当Armstrong工艺生成的浆液被过滤时，形成凝胶或凝胶状材料，其由金属粉末或颗粒物、盐粉末或颗粒物以及过量的液态还原金属构成.需要对所述浆液进行处理以从所期望的终产品中分离出不需要的组分，例如过量的液态金属、盐颗粒物，所述终产品为金属颗粒物或粉末.
发明概述
在开发针对钛及其合金的Armstrong工艺中，人们发现，上述作为参考的生产浆液的方法非常快速，在所述连续工艺的工程学方面，将产品从浆液中分离出来是最困难的.本说明书是针对用钠对四氯化钛的发热还原反应，从而得到钛颗粒、氯化钠颗粒和过量钠；然而，其不能理解为对本发明的限制，其仅仅是出于方便的目的.
因此，本发明的一个目的是提供一种将金属粉末或颗粒物从浆液中分离出来的方法，所述浆液由液态金属、金属粉末或颗粒物以及盐粉末或颗粒物构成.
本发明的另一目的是提供一种将金属颗粒物从上述类型的浆液中分离出来的方法，所述浆液中的一种不需要的组分用于从浆液中分离出两个组分.
本发明的另一目的是提供一种将金属颗粒从浆液中分离出来的方法，所述浆液由液态金属、金属颗粒物和盐颗粒物的原始成分构成，该方法包括除去至少一部分液态金属，以浓缩金属和盐颗粒物，将所述液态金属或原始盐成分液体或其混合物在高于原始盐成分或其混合物的熔点的温度下经过浓缩的金属和颗粒物，从而进一步浓缩所述金属颗粒物，之后，将金属颗粒物从剩余的原始成分或盐成分混合物中分离出来.
本发明的最终目的是提供一种将金属颗粒物从浆液中分离出来的方法，所述浆液由液态金属、金属颗粒物和盐颗粒物的原始成分构成，该方法包括将原始成分的浆液引入其内具有液体盐的容器中，由于最轻的液态金属和最重的金属颗粒之间存在密度差异，从而在容器中分层，金属颗粒物的浓度朝向容器底部不断增加，将液态金属从容器中去除，将经浓缩的金属颗粒物和某些液体盐从容器中分离出来，将盐从金属颗粒物中过滤出来，之后对从金属颗粒物中分离出的盐进行冷却和水洗.
通过以下描述和实施本发明，本发明的其它优势、目的和新颖特征对于本领域技术人员是显而易见的.
本发明包括特定的新颖特征和部件的组合，这在下文全面描述，在附图中进行阐述，并在所附的权利要求中特别指出，应当理解，在不偏离本发明的精神或不损害本发明的优势的情况下，可以对具体细节作出各种修改.
附图简述
为了便于理解本发明，在附图中描述了优选实施方案，当与以下描述相结合时，可以易于理解和评价本发明、其结构、操作和多个优势。
附图1为本发明第一实施方案的示意图；
附图2为本发明另一实施方案的示意图；
附图3为本发明另一实施方案的示意图。
优选实施方案的详细描述
参照附图特别是附图1，其显示了分离系统10，其中容器15具有大致圆柱形的部分16、圆盖状顶部17，截头圆锥形的底部18以及从所述容器15底部延伸出的排出管19.上述作为参考的专利申请中公开的反应器20类型具有外部液态金属或钠导管21，以及内部卤化物蒸汽或四氯化钛导管22.液态金属或钠供应罐25将钠或其它液态金属提供至反应器20，卤化物锅炉26将适当的卤化物蒸汽供应至反应器20，如前所述.
容器15的内部具有向下倾斜的挡板28，所述挡板具有以较大锐角延伸并通常与钠或液态金属出口29相反的远端28a。液态金属出口29与金属或钠泵31流体连通，所述泵通向具有液体进口34和液体出口35的热交换器33.液态金属补充管37与供应罐或存储池25相连通.在所述罐或存储池25上提供工程领域所公知的通风管线38.
具有致动器41的阀40位于容器15的出口19处，所述出口与两个排出管线42和43相通，所述每个排出管线均具有阀，例如管线42内显示的阀44。
过滤组件45包括容器46和倾斜的滤板47，其目的在下文描述.钝化气体入口50具有位于钝化气体源(未示出)和容器46之间的阀51.真空干燥管线52离开所述容器46，并具有阀53.位于容器46底部的浆液排出管线56具有阀57，盐排出管线61具有阀62.最后，冲洗水入口管道66具有阀57.
分离系统10通过以下方式操作，其中通过上文所述并引入的Armstrong专利申请中所描述的方法，在反应器20中生产例如金属或金属合金的材料.仅仅作为举例，可以通过用碱金属或碱土金属例如钠或镁还原四氯化钛蒸汽或用于合金的多种卤化物蒸汽，以得到钛或钛合金.用Armstrong工艺可以很容易制得合金，将适当量的卤化物蒸汽混合，并以之前所描述的相同方法对它们进行还原.在任何情况下，采用大量过量的还原金属控制反应，从而得到包括过量还原金属例如钠、金属颗粒物例如钛以及另一反应产物例如盐颗粒氯化钠的浆液.离开反应器20的浆液可以控制在各种温度下，在一个例子中，通过所存在的过量还原金属的量进行控制.
在实际例子中，所述浆液通常具有至多为大约10重量％的颗粒物，所述颗粒物可以是平均直径大约为10至大约50微米的盐，以及平均直径大约为0.1微米至大约500微米的钛，所述钛颗粒物或粉末的范围更可能为大约1-10微米，钛的聚集线(块)为大约50至大约1000微米.液态金属、盐颗粒物和钛颗粒物的组合离开管嘴20，进入容器15。容器15中的盐的液位可以任意选择，只要其位于钠出口29以下.所述盐可以是反应产物盐例如氯化钠，或熔点低于反应产物盐的盐混合物.尽管所述盐可以是任意的盐，但是优选所述盐为反应产物或其混合物，例如低共熔混合物，例如氯化钙-氯化钠的低共熔混合物，其在大约600℃熔化.
然后，整个系统10可以在更低温度下操作.例如，氯化钠在大约850℃熔化.因此，如果容器15中的盐为氯化钠，则容器15必须在上述熔点以上的温度下操作，但是，由于低共熔混合物在600℃熔化，其降低了操作温度.不论怎样，不论在容器15中的液位30之处存在何种盐，由于密度不同，所述液态金属将会漂浮起来，并通过钠或液态金属泵31通过出口29提取.具有适当入口和出口管线34、35的热交换器33将来自容器15的钠的温度从600℃降低(仅仅作为举例)，从而经回收的钠在预定温度(例如大约400℃)下进入反应器20.挡板28和28a防止从反应器20进入容器15的颗粒物被吸入钠出口29。
由于颗粒物沉降于容器15的下部18，由于通过管线29除去了钠，颗粒物浓度增加了.当阀40被启动时，经浓缩的浆液通过管线42流经出口或排出端19进入过滤组件45中.在过滤组件45中，其中的温度足够使熔融盐处于液相，金属颗粒被收集于滤板37上，而通过滤板的盐经管线61排出并返回至例如电解池中(未示出).阀62打开管线61，从而使盐流过，而阀57关闭以防止材料离开所述过滤组件45。当已经积聚成足够大的滤饼时，关闭阀62，当滤饼已经冷却低于大约100℃以后，关闭阀44，并打开真空干燥管线53，从而可以是氩和小百分含量的氧气的钝化气体可以通过阀51的启动而进入容器46.当可能主要为钛粉末并具有一定量盐的滤饼被钝化后，关闭阀51，打开冲洗水阀67，从而使水进入容器46中，其中溶解盐并移动滤饼通过管线56进行最终清洗和分类，应理解，阀67应在水洗之前打开。通过管线61离开过滤组件45的盐可以重新循环至容器15，如管线61a所示。
因此可以看出，分离系统10依赖于浆液中不需要的液态金属组分与在干燥蒸汽和还原金属的反应过程中生成的盐以及金属颗粒物之间的重力差异.尽管所述分离系统10为间歇式系统，但是，其可以根据需要经过一简单的阀分配系统从一个过滤组件45快速地循环至其它过滤组件，如本领域所公知的.
尽管用钠和四氯化钛对上述例子进行了描述，但是应理解，可以通过如前所述的方式分离由Armstrong工艺制成的任意材料.
附图2显示了另一备选实施方案的分离系统80，其中容器85类似于容器15，具有圆柱形部分86、圆顶部87，以及从其延伸出一出口89的截头圆锥形底部88.与上述相同类型的反应器90与容器85相连通，并具有卤化物入口91和还原金属入口92。浆液出口93与容器85的顶部87相连通.过滤器95可以是本领域公知的任意适当的过滤器，但是仅仅用作举例，其优选为“楔形网状过滤器”，其大小可以通过至多125微米的颗粒。流经过滤器95的材料通过出口管线96离开容器85，进入重力分离室97.所述重力分离室97为截头圆锥形，具有出口99，供较重的材料流出，在该特定例子中为氯化钠.出口98接收较轻的材料，在该例子中为钠，并将其通过未示出的适当过滤器和其它机构回收至反应器90.在该实施方案中，容器85通过本领域公知的内部或外部加热器保持在大约850℃的高温下，从而使盐为液态或熔化，在该例中为氯化钠.大量过量的熔融钠置换了颗粒物周围的氯化钠，从而钠和盐经滤板95进入重力分离室97，并如前所述被回收.当滤板95上积聚了适当的滤饼后，关闭阀，然后除去滤饼供进一步处理。本实施方案的优势在于，其中一种不需要的组成物即钠液态金属被用于置换另一种不需要的组成物，在该例中为熔融盐.需要用适当的热交换器将管线98中所排出的钠在回收之前降低其温度，以及加热并维持容器85和容器97中熔融盐的温度.
现在参照附图3，其为本发明的另一实施方案，表示为分离系统100.分离系统100具有如实施方案10和80所示的类似部件.在系统100中，具有容器105，所述容器具有圆柱形的部分106、圆盖状顶部107，截头圆锥形的底部108以及从其底部延伸出的排出管109。之前所述的用于实施Armstrong工艺的反应器110类型具有，仅仅用作例子，四氯化钛入口111和钠入口112，用于进行如前所述的反应，出口113将得到的浆液从反应中去除.
重力分离室117为截头圆锥形，具有供较轻的液态金属例如钠排出的出口118，以及供较重的不需要的组成物(在该例中为氯化钠)排出的底部出口119.在排出管线116和重力分离室117之间提供适当的阀，如阀121所示，阀122位于容器105和钠进口112之间的排出管线116内.另一阀123位于容器105和重力分离室117的氯化钠出口之间，最后阀124位于反应器110和容器105之间.
在本系统100中，当熔化的盐在适当的例如高于氯化钠熔点例如850℃的温度下流经滤板115并携带过量熔融钠时，滤板115收集金属颗粒物，当在过滤器115上积聚了滤饼时，熔融钠从中置换出来.液态钠和液态盐的组合流出容器105.关闭阀122并打开阀121，使材料通过适当泵(未示出)移至重力分离室117.在重力分离室117中，液态金属钠漂浮，液体盐形成位于分离室117底部的较重层并被分离出来，其表示为钠在分离室顶部通过管线118被吸取并回收(如果需要，在冷却后)至反应器110的钠入口.通过阀123将盐回收至容器105.反应器110可以通过阀124与系统隔开，从而在预定时间之后，反应器可以与系统分开，并转至另一分离模块，而液体盐用于置换容器105中存在的以及钛颗粒物中的液态钠，所述钛颗粒物在过滤器115上形成滤饼.
尽管此处公开的分离系统为间歇式操作，但是阀门的装设可以进行连续分离并同时使反应器不断运行.两个或多个分离系统10、80或100的简单系统允许反应器连续生产Armstrong反应的产物.
尽管参照钛和钠进行了描述，但是任意碱金属或碱土金属或它们的不同组合可以用作还原剂金属.可以使用任意卤化物或卤化物的任意组合作为注入液态金属，从而发生放热反应的蒸汽.出于经济原因，优选钠或镁，最优选钠.出于其它原因，还优选四氯化钛以及钒和铝的氯化物，从而得到钛粉末或不同的钛合金，钛6∶4合金为目前使用的最优选的钛合金.6∶4钛合金为6％铝、4％钒，而剩余的为钛，这是本领域所公知的。
尽管所公开的被认为是本发明的优选实施方案，但是应理解，可以在不偏离本发明的精神或者不损害本发明的优势的情况下，对细节作出各种修改.

Claims (12)

1.一种将金属颗粒物从浆液中分离出来的方法，所述浆液由液态金属、金属颗粒物和盐颗粒物的原始成分构成，其中所述液态金属的原始组成物为碱金属或碱土金属或其混合物，所述金属颗粒物为Ti或Ti合金，所述盐颗粒物是所述液态金属的卤化物，所述方法包括除去至少部分液态金属以浓缩金属和盐颗粒物，使液态金属或原始盐颗粒物液体或其混合物在高于原始盐颗粒物或其混合物的熔点的温度下通过所述浓缩的金属和盐颗粒物，从而进一步浓缩金属颗粒物，之后将金属颗粒物从剩余的原始组成物中分离出来.
2.如权利要求1所述的方法，其中当从浆液中除去至少部分液态金属时，形成凝胶.
3.如权利要求1所述的方法，其中在对金属颗粒物进一步浓缩的过程中，液体原始盐颗粒物或其混合物的温度低于金属颗粒物的烧结温度。
4.如权利要求1所述的方法，其中原始盐颗粒物为低共熔混合物，或者为NaCl和CaCl2的低共熔混合物.
5.如权利要求1所述的方法，其中所述Ti合金包括6重量％Al，4重量％V，其它为Ti。
6.如权利要求1所述的方法，其中所述金属颗粒物为Ti或Ti合金、液态金属为Na、盐颗粒物为NaCl或为NaCl和CaCl2的低共熔混合物.
7.一种将金属颗粒物从浆液中分离出来的方法，所述浆液由液态金属、金属颗粒物和盐颗粒物的原始成分构成，其中所述液态金属的原始组成物为碱金属或碱土金属或其混合物，所述金属颗粒物为Ti或Ti合金，所述盐颗粒物是所述液态金属的卤化物，所述方法包括将原始组成物的浆液引入其中包括液体盐的容器中，由于液态金属最轻、金属颗粒物最重，存在着密度差异，因此在该容器中分层，金属颗粒物的浓度朝着容器底部不断增加，将液态金属从容器中除去，将浓缩的金属颗粒物和某些液态盐从容器中分离，将盐从金属颗粒物中过滤出来，之后，对从金属颗粒物中分离出的盐进行冷却并水洗。
8.如权利要求7所述的方法，其中所述液体盐与盐颗粒物相同。
9.如权利要求7所述的方法，其中所述液体盐为低共熔混合物，或者为所述盐颗粒物的低共熔混合物.
10.如权利要求9所述的方法，其中所述低共熔混合物含有Na和CaCl2。
11.如权利要求10所述的方法，其中所述液态金属为Na或Mg。
12.如权利要求7所述的方法，其中所述液态金属通过抽吸的方式从容器中除去，从而防止金属颗粒物与液态金属一起被除去。
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US20100282023A1 (en) 2010-11-11
CA2497999A1 (en) 2004-03-18
US20060123950A1 (en) 2006-06-15
CN1681951A (zh) 2005-10-12
AU2003273279B2 (en) 2007-05-03
US7632333B2 (en) 2009-12-15
WO2004022800A1 (en) 2004-03-18
EA200500463A1 (ru) 2005-10-27
EA006616B1 (ru) 2006-02-24
AU2003273279A1 (en) 2004-03-29

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