CN1161064A - 制备金属和其它元素的方法 - Google Patents

制备金属和其它元素的方法 Download PDF

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CN1161064A
CN1161064A CN95195389A CN95195389A CN1161064A CN 1161064 A CN1161064 A CN 1161064A CN 95195389 A CN95195389 A CN 95195389A CN 95195389 A CN95195389 A CN 95195389A CN 1161064 A CN1161064 A CN 1161064A
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metal
alkaline
halogenide
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titanium
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CN1076759C (zh
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D·R·阿姆斯特朗
S·S·博里斯
R·P·安德森
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Kroftt-Brakston International Inc
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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
    • 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
    • C22B34/1222—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 using a halogen containing agent
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/16—Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/28—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from gaseous metal compounds
    • 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
    • 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
    • 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
    • C22B5/00—General methods of reducing to metals
    • C22B5/02—Dry methods smelting of sulfides or formation of mattes
    • C22B5/04—Dry methods smelting of sulfides or formation of mattes by aluminium, other metals or silicon
    • 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

本发明论述由卤化物或其混合物生产非金属元素或金属或其合金的方法。卤化物或其混合物与足够量的液态碱金属或碱土金属或其混合物相接触，使卤化物转变成非金属或金属或合金，同时保持反应物的温度低于碱金属或碱土金属在大气压下沸点值或低于产生的非金属或金属或其合金的烧结温度。本发明揭示了一种连续式的生产方法，特别适用于钛。

Description

制备金属和其它元素的方法
             发明背景
本发明论述从元素型物质的卤化物生产该元素型物质的方法。它特别适用于其卤化物在还原反应中呈放热反应的那些金属和非金属，尤其适合于钛的制备。本发明将以钛的制备为参考例子来进行描述，但此方法也适用于其它金属和非金属，例如Al、As、Sb、Be、B、Ta、Ge、V、Nb、Mo、Ga、Ir、Os、U和Re。从所有这些元素的卤化物还原成金属时，都产生明显的热。为此应用目的，其元素型物质包括上述的和表1中所列的金属和非金属。
现今，钛的生产是利用四氯化钛的还原反应。四氯化钛是由品位较高的二氧化钛矿石经氯化而得。含金红石的矿石经物理法浓集就可得到氯化所需的进料，而其它二氧化钛的来源如钛铁矿、含钛铁矿以及大部分其它钛的原材料，都需进行化学浓集处理。
采用四氯化钛还原反应制备金属钛时，已试用过一系列还原剂，如氢、碳、钠、钙、铝和镁。四氯化钛的镁还原法已证明是一种工业规模生产金属钛的方法，但是这种间歇式的生产工艺需要较多的物料操作，从而引入污染的可能性，并且在批与批之间也存在质量上的差异。降低生产成本的最可行的办法是发展一种在物料操作中就伴随有还原的连续式还原生产工艺。
目前极需研究一种生产工艺，它能经济地连续生产钛粉末，这种钛粉末不需附加的操作即可适用于粉末冶金或真空-电弧熔融成铸锭。Kroll工艺和Hunter工艺是目前两种以工业规模生产钛的方法。
Kroll工艺是在约1000℃下用镁还原四氯化钛，该工艺是在含惰性气氛(氦或氩)的曲颈缶中间歇式进行的。加入到容器中的镁经加热形成熔融镁浴。室温下的液态四氯化钛在熔融镁浴的上方分散成小滴状。这时液态的四氯化钛在熔融镁浴上方的气相空间蒸发。同时发生表面反应以形成钛和氯化镁。Hunter工艺与Kroll工艺相似，但它是选用钠来代替镁作四氯化钛的还原剂，反应后生成金属钛和氯化钠。
此两工艺的反应均是不可控制的和散现的，并且助长枝状金属钛的增长。钛熔合成包封有一些熔融氯化镁(或氯化钠)的块状物，这种熔合块状物称为钛海绵。金属曲颈缶冷却后，固化的钛海绵破碎、纯化，然后在热氮气流中干燥。通常采用研磨法、喷丸法或离心法来制备钛粉末。常用的技术是先使钛吸收氢以形成脆性海绵，从而便于研磨操作。粉末状的氢化钛形成后，颗粒经脱氢处理以生产可用的产品。把钛海绵加工成可用的形状是困难的，且耗费劳力，也导致产品价格增加1-2倍。
在加工步骤中，一些大至几厘米的海绵颗粒可能会在空气中着火，并转变成氮氧化钛，这种产物在熔融操作中一般不能被破碎。在金属钛中形成的硬质材料夹杂物已被认为是引起喷气发动机灾难性失效而导致飞机坠毁的原因。
上述的工艺过程中，存在一些使钛产品具有高价格的内在因素。间歇式生产本身就耗费投资及劳力，钛海绵也要经大量的附加操作才能制成可用形状的钛，这就提高了价格、增加了工人面临的危险，也加重了间歇式生产中质量控制的困难性。此两工艺均不能利用大的放热反应，因此要为钛的生产输入大量的能量(约6千瓦·时/公斤金属产品)。此外，过程中还产生大量对环境有害的废物。
                        发明概述
本发明的目的是要提供一种生产非金属或金属或其合金的连续式生产方法及系统，同时在投资及运行费用上要优于当今的间歇式生产工艺。
本发明的另一目的是要提供一种利用卤化物的放热还原反应生产非金属或金属的方法和系统，同时要防止金属或非金属在生产设备上发生烧结。
本发明还有一个目的就是要提供一种从非金属或金属的卤化物生产该非金属或金属的方法和系统，同时在工艺和系统中其还原剂可再循环使用，从而大大减少此工艺过程对环境的影响。
本发明包括一些新的特点和部件组合，这些将在下面结合图示进行全面描述，并在所附权利要求中给以特别说明。当然，在细节上可能会有各种变化，但不会违反本发明的实质或损失本发明的任何优点。
                      附图简述
为便于对本发明的理解，在附图上给出了优选实例。结合查看实例及下面的描述，就很容易理解及正确评价本发明，它的构成和操作以及它的许多优点。
图1为流程图，给出从四氯化钛生产金属钛的连续式生产过程的例子。
图2为工艺过程的热平衡流程图，燃烧器中的反应物温度约为300℃。
图3为工艺过程的能量平衡图，燃烧器中的反应物温度约为850℃。
                           发明详述
本发明的工艺过程可依欲还原的过渡金属而选用任何碱金属或碱土金属来实现，在某些情况下，可利用碱金属或碱土金属的组合。此外，任何卤化物或卤化物的组合均可用于本发明，虽然在大部分情况下氯是被优选的卤素，这是因为它最便宜也最易获得。在碱金属或碱土金属中，作为一个例子选用钠，但这并不是一种限制，而仅作为一个例证，因为钠最便宜所以作为优选金属，就如选用氯一样。
关于欲还原的非金属或金属，有可能还原下列表中的单一金属，例如钛或钽、锆；也有可能按所需分子比提供混合的金属卤化物作为工艺过程的进料，以制备有预定组成的合金。表1中例举了每克钠还原可用于本发明的非金属或金属卤化物的反应热。
                           表1
                 原料       反应热(千焦耳/克)
                 TiCl4             10
                 AlCl3              9
                 SbCl3             14
                 BeCl2             10
                 BCl3              12
                 TaCl5             11
                 VCl4              12
                 NbCl5             12
                 MoCl4             14
                 GaCl3             11
                  UF6             10
                  ReF6            17
本工艺的例证是从四氯化钛生产单一金属钛，要再次说明的是这仅为一个例子，并非只限于此。
图1给出了概要流程图。钠和四氯化钛在燃烧器反应室10中进行反应，来自蒸馏塔11的四氯化钛蒸气喷入流动的钠物流中(钠源未给出)，补给钠产生于电解槽12。还原反应为高放热反应，并生成钛和氯化钠的熔融状产物，此反应产物在大量钠物流中冷却。产物的颗粒大小及反应速率由调节四氯化钛蒸气流量、四氯化钛经惰性气(如He或Ar)的稀释程度以及钠流特性和混合参数来控制。燃烧器装有同心喷咀，四氯化钛流经内喷咀，液态钠流经外喷咀，气体与液态得以补充混合，反应产物的温度(与反应热有很大关系)可由钠量来控制，并保持低于产品金属的烧结温度，例如钛的烧结温度约为1000℃。
在反应后的钠主体物流中含有反应产物钛和氯化钠，采用常规的分离设备13和14(例如旋风分离器或颗粒过滤器)可将这些反应产物从钠主体物流中分离出来。有两种分离方案可用于钛和氯化钠体系。
第一种方案是在分离步骤中去除钛和氯化钠。它可通过控制进入燃烧器10的四氯化钛和钠的流量比，以使主体物流的温度保持在能使钛呈固态而氯化钠呈熔融态来实现。此方案中，先去除钛，而主体物流经冷却使氯化钠固化，然后从分离器14中去除氯化钠。此方案中为使四氯化钛蒸馏所需的过程热将从钛分离器13后的主体物流中直接获取。
去除反应产物的第二方案是在燃烧器中维持四氯化钛对钠的较低流量比，使主体钠流温度保持在低于氯化钠的固化温度。此方案中钛和氯化钠同时去除，在颗粒上的氯化钠及任何残留的钠均在其后的水-乙醇洗涤中去除。
分离后的氯化钠再循环至电解槽12，再生处理后所得的钠再返回到主体工艺物流中并进入燃烧器10，所得的氯用于矿石氯化器15中。要指出的是氯化钠电解和接着的矿石氯化均是采用成熟技术来完成的，而这种反应副产物的综合利用及再循环技术在Kroll或Hunter工艺中是不可能实现的，因为其工艺过程是间歇式的，并且钛海绵只是中间产品。采用Kroll或Hunter工艺的生产厂是以购买四氯化钛来生产钛。采用本发明的化学制备工艺就能使这些分离过程一体化，它不仅改善了生产的经济性，而且由于废物流的再循环又大大地减少了对环境的影响。
电解槽12中产生的氯气用于氯化器15中钛矿石(金红石、锐钛矿或钛铁矿)的氯化。在氯化阶段，钛矿石与焦炭混合，并在流化床或其它类型适用的窑式氯化器15中于氯进行化学反应。原材料中所含的二氧化钛经氯化转变成四氯化钛，而氧与焦炭作用生成二氧化碳。矿石中所含的铁和其它杂质金属在氧化过程中也转化为相应的氯化物。生成的氯化钛经冷凝并在蒸馏塔11中蒸馏纯化，纯化后的氯化钛蒸气经再冷凝后送入钛制备器；在此一体化的工艺过程中，四氯化钛蒸气流是直接用于制备过程。
经热交换器16为蒸馏步骤提供过程热后，其主工艺物流的温度经热交换器17调节到燃烧器10所需的温度，然后与再生钠再循环流合并并喷射入燃烧器。当然各种泵、过滤器、捕集肼、监测器等等将按需要采用技术成熟的设备。
参看图2和图3，其分别为低温工艺(图2)和高温工艺(图3)的闭合流程图。这两种工艺的主要差别在于钠进入和离开燃烧器10的温度有所不同。图中同类设备标以同样编号，其用途在图1中已有说明。如图2所示的低温工艺，钠在200℃下以38.4公斤/分的流量进入燃烧器10，来自蒸馏塔11的四氯化钛的压力为2大气压，温度为164℃，经由管线15A的流量为1.1公斤/分。压力高达12大气压也是适用的，主要的是要防止回流，所以至少要选用2大气压以确保通过燃烧器喷咀的物流是处于临界值或受到抑制的。总之，对于图1以及图2和图3所示的工艺流程，主要的是要使来自分离器13的钛处于或低于并且最好是正好低于钛的烧结温度，以排除和防止钛在设备表面固化。这对于目前工业化生产所采用的工艺来说是主要的困难之一。当金属钛的温度保持低于金属钛的烧结温度时，钛就会像现在所描述的那样不会附着在设备壁上，所以就勿需用物理方法来去除钛。这是本发明的重要之处，它可利用足够量的金属钠或稀释气或同时利用二者以控制元素型金属(或合金)产品的温度来实现。
目前所采用的间歇式生产工艺需要用风镐将钛海绵从收集器中敲打下来，并且会遇到钛海绵的硬度问题，因此这不是一项很好的作业。
图3所示的高温工艺表明，钠在750℃下进入蒸馏塔，其流量约为33.4公斤/分。
图2所示的低温工艺中，来自燃烧器的产物的温度约为300℃；而在高温工艺中，其温度约为850℃。很清楚，甚至在高温工艺中，钛的温度也大大低于其烧结温度(约1000℃)，因此这就避免了目前干法工艺的各种缺点。图2和图3中所示的热交换器均标记为20，但其排出的能量值在图2(低温工艺)和图3(高温工艺)中是不一样的，部分原因是由于热交换器20的布局不同。在高温工艺中，热交换器20是安排在氯化钠分离之前，而在低温工艺中，热交换器20是安排在氯化钠分离之后，结果造成了上述的说的不同能量输出。在图2和图3所示的流程中，钠的补给均由管线1 2A供料，钠可来自电解槽1 2或其它一些完全不同的钠源。另外，图2和图3中是各类设计参数的例证，它可用于金属钛的连续生产过程，其可避免目前工业化的间歇式生产过程中的存在的固有问题。
本发明仅以钛的生产作为参考例证，并以四氯化钛作为原料，以钠作为还原金属，但是应理解这只是为了例证目的。本发明完全适用于表1所列的那些金属和非金属的制备，当然还包括铀和铼的氟化物以及其它一些卤化物如溴化物。此外，钠决不是唯一可用的还原剂，这里选用钠作为还原金属是因为其价格便宜又易获得。锂、钾以及钙和其它碱土金属都是适用的，并在热力学上也是可行的。利用热力学表来确定哪些金属能作为上述反应的还原剂是种技术上成熟的方法。本工艺原则上可用于如表1所示的由氯化物或卤化物还原成金属时所发生的高放热反应中。此外，基于本发明的技术成熟性，预计也可利用该工艺来制备合金，只要按所需合金的分子比来选用合适的卤化物进料。这里仅给出了本发明的优选实例，在细节上当然可能会有各种变化，但不会违反本发明的实质或损失本发明的任何优点。

Claims (17)

1、一种由卤化物或其混合物来制备元素型物质或其合金的一种方法，包括将卤化物或其混合物与足够量的液态碱金属或碱土金属或其混合物直接接触，使卤化物转变成元素型物质或合金，同时保持反应产物的温度低于大气压下碱金属或碱土金属的沸点中之较低者，或低于所产生的元素型物质或合金的烧结温度，以防止元素型物质在设备上沉积。
2、权利要求1的方法，其中元素型物质为Ti、Al、Sb、Be、B、Ga、Mo、Nb、Ta和V中的一种或数种。
3、权利要求1的方法，其中元素型物质是Ir、Os、Re和U中的一种或数种。
4、权利要求1的方法，其中碱金属是Na、K和Li中的一种或数种。
5、权利要求1的方法，其中碱土金属是Ca、Sr和Ba中的一种或数种。
6、权利要求1的方法，其中卤化物是Cl、Br和F的一种或数种。
7、权利要求1的方法，其中碱金属是Na和K中的一种或数种；碱土金属是Ca和Ba中的一种或数种；卤化物是Cl和Br中的一种或数种。
8、权利要求1的方法，其中卤化物以蒸气存在，其压力约为2-10大气压，并与液态碱金属或碱土金属或其混合物相接触。
9、权利要求1的方法，其中还包括向卤化物蒸气中引入惰性气体，作为稀释剂和冷源。
10、权利要求9的方法，其中惰性气体为Ar或He。
11、权利要求1的方法，其中要保持反应物的温度低于所制备的元素型物质或合金的烧结温度。
12、一种连续式生产非金属或金属或其合金的方法，包括：提供卤化物蒸气流来源；提供液态碱金属或碱土金属来源；使卤化物蒸气流与液态碱金属或碱土金属或其混合物直接混合，以生成非金属或金属和碱金属或碱土金属的卤化物；所述卤化物蒸气的压力小于2大气压；所述碱金属或碱土金属要有足够的量以保持反应产物的温度低于此碱金属或碱土金属的沸点或低于此非金属或金属或合金的烧结温度，两个低于要同时满足以防止反应产物在设备上的沉积；从反应物中分离固态金属或非金属；将碱金属卤化物或碱土金属的卤化物分解成其组成部分；冷却和再循环碱金属或碱土金属，使其与另外加入的卤化物蒸气起反应。
13、权利要求12的方法，其中卤化物还原成金属或非金属的反应为放热反应。
14、权利要求13的方法，其中卤化物的沸点低于400℃。
15、权利要求14的方法，其中卤化物蒸气流流经同心喷咀的内喷咀，而液态金属流经由内外喷咀形成的环形流道，蒸气流速为声速。
16、权利要求15的方法，其中金属或非金属是TiCl4、AlCl3、SbCl3、BeCl3、BCl3、TaCl5、VCl4、NbCl5、MoCl4、GaCl3、UF6、ReF6中的一种或数种。
17、权利要求12的方法，其中卤化物是Br和Cl中的一种或数种。
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CN1076759C (zh) 2001-12-26
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DE69521432T2 (de) 2002-05-29
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AU686444B2 (en) 1998-02-05
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NO316604B1 (no) 2004-03-08
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KR100241134B1 (ko) 2000-03-02
RU2152449C1 (ru) 2000-07-10
BR9508497A (pt) 1997-12-23
US5779761A (en) 1998-07-14
US20080199348A1 (en) 2008-08-21
NO970444D0 (no) 1997-01-31

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