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1. 发明申请

US20080250901A1 Method of High-Melting-Point Metal Separation and Recovery 审中-公开
标题翻译：高熔点金属分离和回收方法
公开(公告)号：US20080250901A1
公开(公告)日：2008-10-16
申请号：US11886323
申请日：2006-03-08
申请人： Tadashi Ogasawara , Makoto Yamaguchi , Katsunori Dakeshita , Masahiko Hori
发明人： Tadashi Ogasawara , Makoto Yamaguchi , Katsunori Dakeshita , Masahiko Hori
IPC分类号： C22B34/12 , C22B9/02
CPC分类号： C25C3/02 , C22B9/02 , C22B34/1272 , C22B34/1295 , Y02P10/234
摘要： A TiCl4 gas is supplied to a molten CaCl2 liquid held in a reactor vessel 6 through a raw material feed pipe 11, TiCl4 is reduced to produce granular metallic Ti by Ca melted in the CaCl2 liquid. The molten CaCl2 liquid in which Ti granules taken out downward from the reactor vessel 6 is mixed is delivered to a separation process 12, the molten CaCl2 liquid is heated in a heating vessel 15, and separation is generated by a difference in specific gravity, whereby the molten CaCl2 liquid 16 is located in an upper layer while a metallic Ti 17 is located in a lower layer. The metallic Ti 17 in the lower layer is taken out from a high-melting-point metal discharge port 18, and the metallic Ti 17 is solidified to yield an ingot. The molten CaCl2 liquid 16 in the upper layer is delivered to an electrolysis process 13 along with the molten CaCl2 liquid taken out from the reactor vessel 6, and Ca generated by the electrolysis and CaCl2 are returned into the reactor vessel 6. A separation and recovery method of the invention is applied to the separation process 12 in the above production process, and high-quality Ti or Ti alloy is efficiently separated and recovered from the CaCl2-containing molten salt with a small amount of energies.
摘要翻译：将TiCl 4气体通过原料供给管11供给到保持在反应器容器6中的熔融CaCl 2 2液体，TiCl 4 通过在CaCl 2液体中熔化的Ca还原以产生颗粒状金属Ti。将其中从反应器6向下取出的Ti颗粒混合的熔融的CaCl 2 H 2液体被输送到分离过程12中，将熔融的CaCl 2液体加热到加热容器15，并且通过比重差产生分离，由此熔融的CaCl 2液体16位于上层，而金属Ti 17位于下层。下层的金属Ti 17从高熔点金属排出口18取出，使金属Ti 17固化，得到锭。上层的熔融CaCl 2液体16与从反应容器6取出的熔融CaCl 2液体一起被输送到电解过程13，由将电解和CaCl 2 2返回到反应容器6中。本发明的分离和回收方法在上述生产过程中应用于分离过程12，并且从包含CaCl 2的熔融盐中有效地分离和回收高品质的Ti或Ti合金，少量的能量。

2. 发明申请

US20070193411A1 Method For Producing Ti Or Ti Alloy Through Reduction By Ca 失效
标题翻译：通过Ca还原生产Ti或Ti合金的方法
公开(公告)号：US20070193411A1
公开(公告)日：2007-08-23
申请号：US10575225
申请日：2004-10-06
申请人： Tadashi Ogasawara , Makoto Yamaguchi , Masahiko Hori , Toru Uenishi , Katsunori Dakeshita
发明人： Tadashi Ogasawara , Makoto Yamaguchi , Masahiko Hori , Toru Uenishi , Katsunori Dakeshita
IPC分类号： B22F9/20
CPC分类号： C25C3/02 , C22B34/1268 , C22B34/1272 , C22B34/1295
摘要： The present invention is a method for producing Ti or a Ti alloy through reduction of TiCl4 by Ca, which can produce the high-purity metallic Ti or high-purity Ti alloy. A molten salt containing CaCl2 and having Ca dissolved therein is held in a reactor vessel, and a metallic chloride containing TiCl4 is reacted with Ca in the molten salt to generate Ti particles or Ti alloy particles in a molten CaCl2 solution, which allows enhancement of a feed rate of TiCl4 which is of a raw material of Ti, and also allows a continuous operation. Therefore, the high-purity metallic Ti or the high-purity Ti alloy can economically be produced with high efficiency. Further, the method by the present invention eliminates the need of replenishment of expensive metallic Ca and of the operation for separately handling Ca which is highly reactive and difficult to handle.
摘要翻译：本发明是通过Ca还原TiCl 4或Ti合金的方法，其可以生产高纯度金属Ti或高纯Ti合金。将含有CaCl 2 Ca的Ca盐溶解在其中的熔盐保存在反应器容器中，含有TiCl 4的金属氯化物与熔融盐中的Ca反应生成Ti 颗粒或Ti合金颗粒在熔融的CaCl 2溶液中，这样可以提高Ti原料Ti的进料速率，并且还允许连续的操作。因此，可以高效率地经济地制造高纯度金属Ti或高纯Ti合金。此外，本发明的方法消除了对昂贵的金属Ca的补充的需要和用于单独处理高反应性和难以处理的Ca的操作。

3. 发明授权

US07648560B2 Method for producing Ti or Ti alloy through reduction by Ca 失效
标题翻译：通过Ca还原生产Ti或Ti合金的方法
公开(公告)号：US07648560B2
公开(公告)日：2010-01-19
申请号：US10575225
申请日：2004-10-06
申请人： Tadashi Ogasawara , Makoto Yamaguchi , Masahiko Hori , Toru Uenishi , Katsunori Dakeshita
发明人： Tadashi Ogasawara , Makoto Yamaguchi , Masahiko Hori , Toru Uenishi , Katsunori Dakeshita
IPC分类号： C22B34/12 , C25C1/02
CPC分类号： C25C3/02 , C22B34/1268 , C22B34/1272 , C22B34/1295
摘要： The present invention is a method for producing Ti or a Ti alloy through reduction of TiCl4 by Ca, which can produce the high-purity metallic Ti or high-purity Ti alloy. A molten salt containing CaCl2 and having Ca dissolved therein is held in a reactor vessel, and a metallic chloride containing TiCl4 is reacted with Ca in the molten salt to generate Ti particles or Ti alloy particles in a molten CaCl2 solution, which allows enhancement of a feed rate of TiCl4 which is of a raw material of Ti, and also allows a continuous operation. Therefore, the high-purity metallic Ti or the high-purity Ti alloy can economically be produced with high efficiency. Further, the method by the present invention eliminates the need of replenishment of expensive metallic Ca and of the operation for separately handling Ca which is highly reactive and difficult to handle.
摘要翻译：本发明是通过还原TiCl 4来生产Ti或Ti合金的方法，其可以生产高纯度金属Ti或高纯Ti合金。将含有CaCl 2并将Ca溶解在其中的熔融盐保持在反应容器中，含有TiCl 4的金属氯化物与熔融盐中的Ca反应，生成熔融CaCl 2溶液中的Ti粒子或Ti合金粒子，作为原料Ti的TiCl4的进料速度，并且还允许连续操作。因此，可以高效率地经济地制造高纯度金属Ti或高纯Ti合金。此外，本发明的方法消除了对昂贵的金属Ca的补充的需要和用于单独处理高反应性和难以处理的Ca的操作。

4. 发明申请

US20070187255A1 Method for producing ti or ti alloy through reduction by ca 审中-公开
标题翻译：通过还原制备钛或钛合金的方法
公开(公告)号：US20070187255A1
公开(公告)日：2007-08-16
申请号：US10589879
申请日：2005-02-16
申请人： Tadashi Ogasawara , Makoto Yamaguchi , Masahiko Hori , Toru Uenishi , Katsunori Dakeshita
发明人： Tadashi Ogasawara , Makoto Yamaguchi , Masahiko Hori , Toru Uenishi , Katsunori Dakeshita
IPC分类号： C25C3/28
CPC分类号： C22B34/1272 , C22B34/129 , C25C5/04
摘要： The invention is a method for producing Ti or Ti alloys through reduction of TiCl4 by Ca, which can produce high-purity Ti metals or Ti alloys. A molten salt containing CaCl2 and having Ca dissolved therein is held in a reactor cell, electrolysis is performed in the molten salt in the reactor cell, and particulate Ti or Ti alloys are generated in the molten salt by supplying a metallic chloride containing TiCl4 to the molten salt so as to react with Ca generated on a cathode electrode side by the electrolysis, allowing enhancement of a feed rate of TiCl4 as a raw material of Ti, and also a continuous operation. Further, the method by the invention eliminates the need of the separate handling of Ca, because a reducing reaction and an electrolytic reaction can simultaneously proceed in the reactor cell to replenish Ca, consumed in the reducing reaction, by the electrolytic reaction. Accordingly, the production method by the invention can be used as means for efficiently and economically producing high-purity Ti metals or Ti alloys.
摘要翻译：本发明是通过Ca还原TiCl 4制备Ti或Ti合金的方法，其可以生产高纯Ti金属或Ti合金。将含有CaCl 2 Ca的Ca盐溶解在其中的熔融盐保持在反应器电池中，在反应器电池中的熔融盐中进行电解，并且在熔融盐中产生颗粒状的Ti或Ti合金，将含有TiCl 4的金属氯化物供给熔融盐，以便通过电解与在阴极电极侧产生的Ca反应，从而提高TiCl 4的进料速率，作为Ti的原料，也是连续操作。此外，本发明的方法消除了对Ca的单独处理的需要，因为还原反应和电解反应可以在反应器电池中同时进行以补充通过电解反应在还原反应中消耗的Ca。因此，本发明的制造方法可以用作高效且经济地制造高纯度Ti金属或Ti合金的手段。

5. 发明申请

US20090152122A1 Method for electrolyzing molten salt, electrolytic cell, and process for producing ti using said method 审中-公开
标题翻译：使用所述方法电解熔融盐，电解池和制造方法的方法
公开(公告)号：US20090152122A1
公开(公告)日：2009-06-18
申请号：US11991072
申请日：2006-08-22
申请人： Tadashi Ogasawara , Makoto Yamaguchi , Toru Uenishi , Masahiko Hori , Kazuo Takemura , Katsunori Dakeshita
发明人： Tadashi Ogasawara , Makoto Yamaguchi , Toru Uenishi , Masahiko Hori , Kazuo Takemura , Katsunori Dakeshita
IPC分类号： C25B1/26 , C25B9/00 , C25C3/28
CPC分类号： C22B34/129 , C22B5/04 , C22B34/1268 , C25C3/02 , C25C7/005
摘要： The present invention provides a method for electrolyzing molten salt that can enhance the concentration of metal-fog forming metal in the molten salt by carrying out the electrolysis under conditions that the molten salt containing the chloride of metal-fog forming metal is supplied from one end of an electrolytic cell to a space between an anode and a cathode in a continuous or intermittent manner to provide a flow rate in one direction to the molten salt in the vicinity of the surface of the cathode and thus to allow the molten salt to flow in one direction in the vicinity of the surface of the cathode. According to the present invention, while high current efficiency is maintained, only the molten salt enriched with metal-fog forming metal such as Ca can be effectively taken out. Further, this method can easily be carried out by using the electrolytic cell according to the present invention. Furthermore, the application of the method for electrolyzing molten salt according to the present invention to the production of Ti by Ca reduction can realize the production of metallic Ti with high efficiency. Thus, the method for electrolyzing molten salt, the electrolytic cell, and the process for producing Ti, each according to the present invention, can be effectively utilized in the production of Ti by Ca reduction.
摘要翻译：本发明提供了一种电解熔融盐的方法，该方法可以通过在从一端供给含有金属雾形成金属的氯化物的熔融盐的条件下进行电解，从而提高熔融盐中金属雾形成金属的浓度的电解池以连续或间歇的方式连接到阳极和阴极之间的空间，以在阴极表面附近向熔融盐提供沿一个方向的流速，从而允许熔融盐流入在阴极表面附近的一个方向。根据本发明，在保持高电流效率的同时，仅有效地除去富含金属雾形成金属如Ca的熔盐。此外，该方法可以通过使用根据本发明的电解槽容易地进行。另外，通过将本发明的熔盐电解方法应用于通过Ca还原生产Ti，可以实现高效率地生产金属Ti。因此，根据本发明的电解熔融盐，电解槽和制造Ti的方法的方法可以有效地用于通过Ca还原生产Ti。

6. 发明申请

US20070181435A1 Method for producing ti or ti alloy through reduction by ca (as amended) 审中-公开
标题翻译：通过ca还原制备钛或钛合金的方法（经修改）
公开(公告)号：US20070181435A1
公开(公告)日：2007-08-09
申请号：US10589949
申请日：2005-02-01
申请人： Tadashi Ogasawara , Makoto Yamaguchi , Masahiko Hori , Toru Uenishi , Katsunori Dakeshita
发明人： Tadashi Ogasawara , Makoto Yamaguchi , Masahiko Hori , Toru Uenishi , Katsunori Dakeshita
IPC分类号： C25C3/28
CPC分类号： C25C3/28 , C22B5/04 , C22B34/1268 , C22B34/129
摘要： The method by the invention in which a molten salt is held in a reactor cell 1 to perform electrolysis in the molten salt of the reactor cell, the molten salt containing CaCl2 while Ca being dissolved in the molten salt, and Ti or Ti alloys are generated in the molten salt by supplying a metallic chloride containing TiCl4 into the molten salt such that the metallic chloride containing TiCl4 is caused to react with Ca generated on a cathode electrode side by the electrolysis, makes it possible to produce the high-purity Ti metals or Ti alloy. Furthermore, the reactor cell 1 includes a membrane 4 which partitions an inside of the reactor cell into a side of an anode electrode 2 and a side of a cathode electrode 3, and the membrane 4 blocks the movement of Ca generated on the cathode electrode side in the reactor cell toward the anode electrode side while permitting the molten salt to flow in the reactor cell, which allows a back reaction by Ca to be effectively suppressed. When an electroconductive porous material is used as a cathode electrode, productivity can further be improved.
摘要翻译：本发明的方法，其中将熔融盐保持在反应器电池1中以在反应器电池的熔融盐中进行电解，所述熔融盐含有CaCl 2，同时Ca溶解在熔融盐中，并且在熔融盐中产生Ti或Ti合金，通过向熔融盐中加入含有TiCl 4的金属氯化物，使含有TiCl 4的金属氯化物反应通过电解在阴极电极侧产生的Ca，可以生产高纯Ti金属或Ti合金。此外，反应器电池1包括将反应器单元的内部分隔成阳极电极2和阴极电极3的一侧的膜4，并且膜4阻挡在阴极电极侧产生的Ca的移动在反应器电池中朝向阳极电极侧，同时允许熔融盐在反应器电池中流动，这允许有效地抑制Ca的反向反应。当使用导电多孔材料作为阴极时，可进一步提高生产率。

7. 发明申请

US20100089204A1 Process for Producing Ti and Apparatus Therefor 审中-公开
标题翻译：生产钛的方法及其设备
公开(公告)号：US20100089204A1
公开(公告)日：2010-04-15
申请号：US11992162
申请日：2006-08-22
申请人： Tadashi Ogasawara , Makoto Yamaguchi , Toru Uenishi , Masahiko Hori , Kazuo Takemura , Katsunori Dakeshita
发明人： Tadashi Ogasawara , Makoto Yamaguchi , Toru Uenishi , Masahiko Hori , Kazuo Takemura , Katsunori Dakeshita
IPC分类号： C22B34/12
CPC分类号： C25C3/28 , C22B34/1272 , C22B34/129 , C22B34/1295 , C25C3/02 , C25C7/005 , C25C7/06
摘要： A process for producing Ti, comprising a reduction step of reacting TiCl4 with Ca in a CaCl2-containing molten salt having the Ca dissolved therein to thereby form Ti particles, a separation step of separating the Ti particles formed in said molten salt from said molten salt and an electrolysis step of electrolyzing the molten salt so as to increase the Ca concentration, wherein the molten salt increased in Ca concentration in the electrolysis step is introduced into a regulating cell to thereby render the Ca concentration of the molten salt constant and thereafter the molten salt is used for the reduction of TiCl4 in the reduction step. In the present invention, the Ca concentration of the molten salt to be fed to the corresponding reduction vessel can be inhibited from fluctuating and, at the same time, can maintain high concentration levels. Further, a large volume of the molten salt can be treated continuously. Therefore, the reduction reaction of TiCl4 can be efficiently performed, and the process can be effectively utilized in the production of Ti by Ca reduction as a production process for realizing Ti production on an industrial scale.
摘要翻译：一种制备Ti的方法，包括在溶解有Ca的含CaCl 2的熔融盐中使TiCl4与Ca反应从而形成Ti颗粒的还原步骤，将在所述熔融盐中形成的Ti颗粒与所述熔融盐分离的分离步骤以及电解电解步骤，电解所述熔融盐以增加所述Ca浓度，其中将所述电解步骤中的Ca浓度升高的所述熔融盐引入调节池中，从而使所述熔融盐的Ca浓度恒定，盐在还原步骤中用于还原TiCl4。在本发明中，可以抑制供给到相应的还原容器的熔融盐的Ca浓度的波动，同时可以保持高浓度水平。此外，可以连续地处理大量的熔融盐。因此，可以有效地进行TiCl 4的还原反应，并且通过Ca还原可以有效地利用Ti的制造，作为实现工业规模的Ti生产的制造方法。

8. 发明申请

US20080053838A1 Method for Production of Metal by Molten-Salt Electrolysis and Method for Production of Titanium Metal 审中-公开
标题翻译：熔盐电解生产金属的方法及钛金属生产方法
公开(公告)号：US20080053838A1
公开(公告)日：2008-03-06
申请号：US11576891
申请日：2005-10-05
申请人： Masanori Yamaguchi , Yuichi Ono , Susumu Kosemura , Eiji Nishimura , Tadashi Ogasawara , Makoto Yamaguchi , Masahiko Hori , Toru Uenishi
发明人： Masanori Yamaguchi , Yuichi Ono , Susumu Kosemura , Eiji Nishimura , Tadashi Ogasawara , Makoto Yamaguchi , Masahiko Hori , Toru Uenishi
IPC分类号： C25C3/28
CPC分类号： C25C3/02 , C22B34/129 , C25B1/26 , C25C3/28
摘要： A method for production of metal by molten-salt electrolysis is a method for production of metal by molten-salt electrolysis which is performed by filling molten salt of a metal chloride in an electrolysis vessel having an anode and a cathode, and a molten salt which reduces solubility of the metal in the molten salt is used.
摘要翻译：通过熔盐电解生产金属的方法是通过熔盐电解生产金属的方法，其通过在具有阳极和阴极的电解容器中填充金属氯化物的熔融盐和熔融盐来进行，使用熔融盐中金属的溶解度降低。

9. 发明申请

US20070295167A1 Method for Producing Ti or Ti Alloy Through Reduction by Ca 审中-公开
标题翻译：通过Ca还原生产Ti或Ti合金的方法
公开(公告)号：US20070295167A1
公开(公告)日：2007-12-27
申请号：US10590863
申请日：2004-10-13
申请人： Tadashi Ogasawara , Makoto Yamaguchi , Masahiko Hori , Toru Uenishi , Kazuo Takemura
发明人： Tadashi Ogasawara , Makoto Yamaguchi , Masahiko Hori , Toru Uenishi , Kazuo Takemura
IPC分类号： C22B34/12 , C25C3/28
CPC分类号： C22B34/1272 , C22B5/04 , C22B34/129 , C22B34/1295 , Y02P10/212
摘要： A mixed molten salt containing CaCl2 and NaCl is held in the reactor cell 1 at a temperature not more than 600° C. TiCl4 which is of a Ti raw material is introduced into the reactor cell 1 while Na is introduced into the reactor cell 1. Na introduced into the reactor cell 1 is replaced by Ca, Ca is dissolved in the molten salt, Ca reduces TiCl4 introduced into the reactor cell 1, and thereby Ti particles are generated. The generated Ti particles are introduced to a separation cell 2 along with the molten salt, and the Ti particles and Na are separated from the molten salt. The residual molten salt is introduced to an electrolytic cell 3 to generate Na by high-temperature electrolysis at the temperature more than 600° C. The generated Na is returned to the reactor cell 1 to replenish Na consumed in the reactor cell 1. The highly reactive Ca is not directly handled, and Na which is easy to handle is used in a circulating manner. Therefore, the Ti or Ti alloy can economically be produced by Ca reduction.
摘要翻译：将含有CaCl 2 N 2和NaCl的混合熔融盐在不高于600℃的温度下保持在反应器电池1中。Ti原料的TiCl 4为引入反应器电池1中，同时将Na引入反应器电池1中。引入反应器电池1的Na被Ca替代，Ca溶解在熔融盐中，Ca使引入反应器电池1的TiCl 4导致，从而产生Ti颗粒。所产生的Ti颗粒与熔融盐一起被引入分离池2中，并将Ti颗粒和Na与熔融盐分离。将残留的熔融盐引入电解槽3中，通过在600℃以上的高温下进行高温电解而生成Na。将所生成的Na返回到反应器电池1，补充反应器电池1中消耗的Na。高反应性Ca不能直接处理，易于处理的Na以循环方式使用。因此，Ti或Ti合金可经济地通过Ca还原产生。

10. 发明申请

US20060219053A1 Method and apparatus for producing metal 审中-公开
标题翻译：用于生产金属的方法和设备
公开(公告)号：US20060219053A1
公开(公告)日：2006-10-05
申请号：US10569602
申请日：2004-07-14
申请人： Tadashi Ogasawara , Makoto Yamaguchi , Masahiko Hori , Toru Uenishi
发明人： Tadashi Ogasawara , Makoto Yamaguchi , Masahiko Hori , Toru Uenishi
IPC分类号： C22B34/00 , C22B34/12
CPC分类号： C25C3/02 , C22B5/04 , C22B34/1268 , C22B34/129 , C25B1/26
摘要： The present invention relates to a method for producing a metal by a direct oxide reduction process with Ca. A CaCl2-based molten salt containing Ca is held in a reduction chamber 1, a metal oxide is introduced into the molten salt in the reduction chamber 1, and the metal oxide is reduced with the Ca in the molten salt to form said metal. The metal formed in the molten salt is separated from the molten salt in a separation means 2, and the molten salt deprived of the metal is introduced into a chlorination chamber 7 and subjected to chlorination treatment with chlorine gas to eliminate the byproduct CaO in the molten salt. The molten salt after chlorination treatment is introduced into an electrolysis chamber 8 and electrolyzed for the formation of Ca and chlorine from CaCl2, and the thus-formed Ca or Ca-containing molten salt is transferred from the electrolysis chamber 8 to the reduction chamber 1. The chlorine obtained in the electrolysis chamber 8 is used in the chlorination chamber 7. Thus, the present invention provides a metal production method and an apparatus wherein high levels of productivity are obtained and the product metal can be inhibited from carbon contamination due to CaO, without any generation of CO2 from the production process, while their being based on the direct oxide reduction process comprising the step of reducing a metal oxide with Ca.
摘要翻译：本发明涉及通过直接氧化还原法制备金属的方法。含有CaCl 2的基于Ca的熔融盐保持在还原室1中，金属氧化物被引入到还原室1中的熔融盐中，并且金属氧化物与Ca中的Ca还原熔融盐形成所述金属。在熔融盐中形成的金属与分离装置2中的熔融盐分离，将不含金属的熔融盐引入氯化室7中，并用氯气进行氯化处理，以消除熔融的盐。将氯化处理后的熔融盐引入电解室8中，电解，从CaCl 2 2形成Ca和氯，将由此形成的含Ca或Ca的熔融盐从电解室8到还原室1。在氯化室7中使用电解室8中得到的氯。因此，本发明提供了一种金属制造方法和装置，其中获得了高水平的生产率，并且可以抑制产品金属由于CaO而导致的碳污染，而不会从生产中产生CO 2 而它们基于直接氧化还原方法，包括用Ca.还原金属氧化物的步骤。

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