TWI694155B - Method for directly producing titanium and titanium alloy by using titanium dioxide - Google Patents
Method for directly producing titanium and titanium alloy by using titanium dioxide Download PDFInfo
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Abstract
本發明公開了一種利用二氧化鈦直接生產鈦及鈦合金的方法,所述方法是利用化學活性大於鈦的活潑金屬與二氧化鈦在高溫下直接發生化學反應,本發明可直接由二氧化鈦生產鈦及鈦合金,不僅生產成本可得到顯著降低,而且反應過程清潔環保,不存在污染問題,尤其是無需中間提純處理,產量高,生產工藝簡單,易於實現規模化。The invention discloses a method for directly producing titanium and titanium alloys by using titanium dioxide. The method is to use a reactive metal with a chemical activity greater than titanium to directly react with titanium dioxide at high temperature. The invention can directly produce titanium and titanium alloys from titanium dioxide. Not only the production cost can be significantly reduced, but the reaction process is clean and environmentally friendly, there is no pollution problem, especially without intermediate purification treatment, high output, simple production process, easy to achieve scale.
Description
本發明是相關於金屬材料製備,特別是相關於一種利用二氧化鈦直接生產鈦及鈦合金的方法。The invention relates to the preparation of metal materials, in particular to a method for directly producing titanium and titanium alloys using titanium dioxide.
鈦是20世紀50年代發展起來的一種重要的結構金屬,鈦合金因具有強度高、耐蝕性好、耐熱性高等特點而被廣泛用於各個領域。鈦和鈦合金以其比重小,塑性好,比強度和熱強性高,低溫性能好,抗腐蝕性優良,以及同人體組織有良好的親合性等優越的性能,成為最重要的工程材料之一。近幾十年以來,隨著技術的發展,鈦和鈦合金的作用越來越重要,在航太、航空、航海等部門它們是產業發展的基礎材料、關鍵材料,在化工、石化、醫療、機械等行業它們也有重要作用。現在,鈦和鈦合金已大量用於製作導彈、火箭、飛船等航天器的殼體,飛機的殼體、機翼和引擎葉片,輪船、軍艦、潛艇的殼體,海水淡化裝置、化工反應器、管道、容器,人造牙齒、骨骼、關節、夾板,以及儀表、精密機械、高爾夫球頭、眼鏡框、鐘錶、首飾和裝飾品。此外,鈦還用於製作超導材料、貯氫材料、吸氣材料、壓電材料和形狀記憶合金等重要的功能材料。Titanium is an important structural metal developed in the 1950s. Titanium alloys are widely used in various fields because of their high strength, good corrosion resistance, and high heat resistance. Titanium and titanium alloys have become the most important engineering materials because of their small specific gravity, good plasticity, high specific strength and thermal strength, good low temperature performance, excellent corrosion resistance, and good affinity with human tissues. one. In recent decades, with the development of technology, the role of titanium and titanium alloys has become more and more important. In aerospace, aviation, nautical and other sectors, they are the basic materials and key materials for industrial development, in chemical, petrochemical, medical, They also play an important role in industries such as machinery. At present, titanium and titanium alloys have been widely used in the production of shells for missiles, rockets, spacecraft and other spacecraft, aircraft shells, wings and engine blades, shells for ships, warships, submarines, seawater desalination devices, chemical reactors , Pipes, containers, artificial teeth, bones, joints, splints, as well as instruments, precision machinery, golf balls, eyeglass frames, watches, jewelry, and decorations. In addition, titanium is also used to make important functional materials such as superconducting materials, hydrogen storage materials, getter materials, piezoelectric materials and shape memory alloys.
目前,金屬鈦的主流生產工藝為克羅爾(Kroll)工藝,主要是採用金屬Mg還原TiCl4 工序、真空分離工序製造金屬鈦。該工藝由三部分組成:一是由含鈦礦物質制取精TiCl4 ;二是鎂還原TiCl4 生產海綿鈦的還原工序;三是真空蒸餾、提純和鎂的再生。在還原工序中,液態TiCl4 從反應器上方加入並流經熔融Mg發生還原,在反應器底部沉積得到海綿Ti;真空分離工序主要是除去其中夾雜的Mg單質和還原產物MgCl2 。雖然該工藝可制得高純度的金屬鈦,但該工藝由於熱還原過程長、工序複雜、不能連續生產等原因使鈦生產成本居高不下,加之生產過程中的環境污染,大大制約了鈦的廣泛應用。因此,研發一種既可以大幅度降低生產成本,且清潔環保、易於實現工業化的生產鈦及鈦合金的方法,將具有重要經濟價值和社會意義。At present, the mainstream production process of metallic titanium is the Kroll process, which mainly uses metallic Mg to reduce TiCl 4 process and vacuum separation process to manufacture metallic titanium. The process consists of three parts: one is the preparation of refined TiCl 4 from titanium-containing minerals; the second is the reduction process of producing titanium sponge with TiCl 4 reduced by magnesium; the third is vacuum distillation, purification and magnesium regeneration. In the reduction process, liquid TiCl 4 is added from above the reactor and flows through the molten Mg to be reduced, and sponge Ti is deposited at the bottom of the reactor; the vacuum separation process is mainly to remove the Mg element contained therein and the reduced product MgCl 2 . Although this process can produce high-purity metal titanium, the process has high production costs due to the long thermal reduction process, complex procedures, and continuous production. The environmental pollution during the production process has greatly restricted the titanium widely used. Therefore, it is of great economic value and social significance to develop a method for producing titanium and titanium alloys that can greatly reduce production costs, is clean and environmentally friendly, and is easy to realize industrialization.
針對習知技術存在的上述問題和需求,本發明的目的是提供一種利用二氧化鈦直接生產鈦及鈦合金的方法,以實現低成本、清潔環保的工業化生產鈦及鈦合金。In view of the above-mentioned problems and needs in the conventional technology, the object of the present invention is to provide a method for directly producing titanium and titanium alloys using titanium dioxide, so as to realize low-cost, clean and environmentally friendly industrial production of titanium and titanium alloys.
為實現上述發明目的,本發明採用的技術方案如下:In order to achieve the above-mentioned object of the invention, the technical scheme adopted by the present invention is as follows:
一種利用二氧化鈦直接生產鈦及鈦合金的方法,所述方法是利用化學活性大於鈦的活潑金屬與二氧化鈦在高溫下直接發生化學反應;所述高溫是指能使活潑金屬或/和二氧化鈦熔化的溫度。鈦是重要的國防和工業材料,一直是世界科技研究的重點。但由於二氧化鈦的鈦和氧之間的化學鍵非常牢固,導致化學性質非常穩定,無法直接生成金屬鈦,所以利用二氧化鈦直接生成金屬鈦已經成為人類材料科學的世界難題。所以現在就只能採用金屬鎂還原四氯化鈦,得到海綿金屬鈦。但四氯化鈦的生產成本非常高,並且在生產過程中會產生嚴重的污染。本發明採用的直接生產鈦的方法,首次破解了人類直接利用二氧化鈦生成金屬鈦的材料學的技術瓶頸。A method for directly producing titanium and titanium alloys using titanium dioxide. The method is to use a reactive metal that has a chemical activity greater than titanium to directly react with titanium dioxide at a high temperature; the high temperature refers to a temperature that can melt the active metal or/and titanium dioxide. . Titanium is an important national defense and industrial material and has always been the focus of scientific research in the world. However, because the chemical bond between titanium and oxygen of titanium dioxide is very strong, resulting in very stable chemical properties, it is impossible to directly generate titanium metal, so the direct generation of titanium metal using titanium dioxide has become a world problem in human materials science. So now we can only use metal magnesium to reduce titanium tetrachloride to get sponge metal titanium. However, the production cost of titanium tetrachloride is very high, and serious pollution will occur during the production process. The method for directly producing titanium adopted by the present invention, for the first time, breaks the technical bottleneck of materials science in which humans directly use titanium dioxide to generate metallic titanium.
一種實施方案,使活潑金屬與二氧化鈦按化學反應方程式的計量比發生化學反應,得到金屬鈦。In one embodiment, the active metal and titanium dioxide are chemically reacted according to the stoichiometric ratio of the chemical reaction equation to obtain metallic titanium.
作為優選方案,使活潑金屬與過量二氧化鈦發生化學反應,得到高純度金屬鈦。因為此種情形下可保證活潑金屬全部參與化學反應,從而保證得到的金屬鈦裡面沒有活潑金屬。As a preferred solution, the active metal is chemically reacted with excess titanium dioxide to obtain high-purity metal titanium. Because in this case, it can be ensured that all active metals participate in the chemical reaction, thereby ensuring that there is no active metal in the obtained titanium.
一種實施方案,使過量活潑金屬與二氧化鈦發生化學反應,得到鈦合金。鈦的用途非常廣泛,其中一個用途之一就是以鈦與活潑金屬形成鈦合金。採用這種方案可以直接得到鈦與活潑金屬的合金,而不需要將純鈦與活潑金屬再進行熔化生成合金。In one embodiment, the excessively active metal reacts with titanium dioxide to obtain a titanium alloy. Titanium has a wide range of uses. One of its uses is to form titanium alloys with titanium and active metals. With this scheme, the alloy of titanium and active metal can be directly obtained without melting the pure titanium and active metal to form an alloy.
一種實施方案,先將形成目標鈦合金所需要的其他組分加入活潑金屬中,然後使其與二氧化鈦發生化學反應,得到所需鈦合金。因為鈦合金種類非常多,如果採用本方案可以一步就形成所需的鈦合金。In one embodiment, the other components needed to form the target titanium alloy are first added to the active metal, and then chemically reacted with titanium dioxide to obtain the desired titanium alloy. Because there are many types of titanium alloys, if this solution is adopted, the desired titanium alloy can be formed in one step.
一種實施方案,先將形成目標鈦合金所需要的其他組分加入二氧化鈦中,然後使活潑金屬與其發生化學反應,得到所需鈦合金。因為鈦合金種類非常多,如果採用本方案可以一步就形成所需的鈦合金。In one embodiment, the other components needed to form the target titanium alloy are first added to titanium dioxide, and then the active metal is chemically reacted with it to obtain the desired titanium alloy. Because there are many types of titanium alloys, if this solution is adopted, the desired titanium alloy can be formed in one step.
一種實施方案,先使部分熔融態活潑金屬與熔融態二氧化鈦發生化學反應,然後補加固態活潑金屬。由於所述化學反應是放熱反應,先使部分熔融態活潑金屬與熔融態二氧化鈦發生化學反應,在反應過程中會釋放出大量的熱,通過補加固態活潑金屬可以提高產量,降低加熱能耗。In one embodiment, a part of the molten active metal and the molten titanium dioxide are chemically reacted, and then the solid active metal is added. Since the chemical reaction is an exothermic reaction, a part of the molten active metal and the molten titanium dioxide undergo a chemical reaction, and a large amount of heat will be released during the reaction. By adding solid active metal, the output can be increased and the heating energy consumption can be reduced.
同樣,也可以先使部分熔融態活潑金屬與部分熔融態二氧化鈦發生化學反應,然後補加固態二氧化鈦。Similarly, the partially molten active metal and partially molten titanium dioxide can be chemically reacted, and then solid titanium dioxide can be added.
同樣,可以先使部分熔融態活潑金屬與部分熔融態二氧化鈦發生化學反應,然後補加固態活潑金屬和固態二氧化鈦。這種方法不僅可以節省加熱能耗,還可以使化學反應連續進行,達到連續生產。Similarly, the partially molten active metal and the partially molten titanium dioxide can be chemically reacted, and then the solid active metal and the solid titanium dioxide can be added. This method can not only save heating energy consumption, but also make the chemical reaction continue to achieve continuous production.
一種實施方案,上述活潑金屬包括但不限於金屬鎂、鋁等,其中優選金屬鋁,因為鋁在與二氧化鈦反應過程中會釋放出大量的熱能,從而可保持化學反應的持續進行,尤其是鋁的沸點高,可保證在化學反應過程中不會發生氣化產生污染問題。In one embodiment, the above-mentioned active metals include, but are not limited to, metal magnesium, aluminum, etc. Among them, metal aluminum is preferred, because aluminum will release a large amount of thermal energy during the reaction with titanium dioxide, which can keep the chemical reaction continuing, especially aluminum The high boiling point can ensure that the gasification will not cause pollution during the chemical reaction.
所述化學反應優選在無氧條件下進行,例如:在惰性氣氛下或真空下進行。因為剛生產出來的鈦非常活潑,容易與氧發生化學反應,通過無氧環境保證產品的品質。The chemical reaction is preferably carried out under oxygen-free conditions, for example, under an inert atmosphere or under vacuum. Because the newly produced titanium is very active, it is easy to chemically react with oxygen, and the quality of the product is guaranteed through an oxygen-free environment.
所述化學反應優選在攪拌下進行,特別是在反應過程中補加固態二氧化鈦、活潑金屬時。The chemical reaction is preferably carried out under stirring, especially when solid titanium dioxide and active metals are added during the reaction.
與習知技術相比,本發明具有如下顯著性有益效果: 1、可直接由二氧化鈦生產鈦及鈦合金,生產工藝簡單,易於實現規模化,且生產成本得到顯著降低; 2、直接由活潑金屬與二氧化鈦進行化學反應,反應過程清潔環保,不存在污染問題。 3、由於可直接生產得到金屬鈦及鈦合金,無需中間提純處理,因此產量高,操作簡單。Compared with the conventional technology, the present invention has the following significant beneficial effects: 1. Titanium and titanium alloys can be directly produced from titanium dioxide. The production process is simple, easy to achieve scale, and the production cost is significantly reduced; 2. Directly from active metals Chemical reaction with titanium dioxide, the reaction process is clean and environmentally friendly, there is no pollution problem. 3. Since the metal titanium and titanium alloy can be directly produced without intermediate purification treatment, the output is high and the operation is simple.
下面結合實施例和附圖對本發明技術方案做進一步詳細、完整地說明。The technical solutions of the present invention will be further described in detail and completely in conjunction with the embodiments and the drawings.
實施例1Example 1
參照第1圖所示,本實施例提供的一種利用二氧化鈦直接生產鈦及鈦合金的方法,是採用間歇式生產工藝,即:先將活潑金屬鋁2放置在坩堝1裡,通過加熱使活潑金屬鋁2熔化成液態及將二氧化鈦5放置在坩堝4裡加熱至其熔化成液態;然後開啟閥門3使液態金屬鋁2加入到坩堝4裡,使液態金屬鋁2與液態二氧化鈦5發生化學反應,由於鈦的比重比生成的三氧化二鋁大,鈦位於坩堝的底部,開啟出料口6可將產生的鈦從坩堝4裡放出。Referring to FIG. 1, a method for directly producing titanium and titanium alloys using titanium dioxide is provided in this embodiment, which adopts a batch production process, that is, firstly placing an
若液態金屬鋁2與液態二氧化鈦5是按化學計量比發生化學反應,則得到金屬鈦;若使液態二氧化鈦5稍稍過量,則可保證液態金屬鋁2充分反應完全,從而得到高純度金屬鈦;若使液態金屬鋁2過量,則會使過量的液態金屬鋁2與形成的金屬鈦形成鈦鋁合金,從而得到鈦鋁合金。If the
若要生產與發生反應的活潑金屬不同元素的鈦合金,例如鈦鐵合金,可通過先使液態金屬鋁2與液態二氧化鈦5按化學計量比發生化學反應得到金屬鈦,然後加入與形成的金屬鈦為化學計量比的金屬鐵,從而直接得到鈦鐵合金;也可以,先將化學計量比的金屬鐵加入液態二氧化鈦5中,然後向其中加入化學計量比的液態金屬鋁2,攪拌使其發生反應,從而直接得到鈦鐵合金。If you want to produce a titanium alloy with different elements of the active metal that reacts, such as a ferro-titanium alloy, you can first obtain a metal titanium by chemically reacting
由於純鈦的熔點為1678℃,而鈦合金的熔點一般會低於1678℃,二氧化鈦的熔點為1850℃,因此反應得到的金屬鈦或鈦合金也為液態,因而可以由坩堝4的底部出料口6排出。Since the melting point of pure titanium is 1678°C, while the melting point of titanium alloys is generally lower than 1678°C, and the melting point of titanium dioxide is 1850°C, the metal titanium or titanium alloy obtained by the reaction is also liquid, so it can be discharged from the bottom of
實施例2Example 2
參照第2圖所示,本實施例提供的一種利用二氧化鈦直接生產鈦及鈦合金的方法,是採用連續式生產工藝,即:先將活潑金屬鋁2A放置在坩堝1A裡,加熱使其熔化成液態以及將二氧化鈦2B放置在坩堝1B裡,加熱使其熔化成液態,然後開啟計量閥門3A和3B,使液態金屬鋁2A與液態二氧化鈦2B加入到反應坩堝4裡,在攪拌7作用下發生化學反應。Referring to FIG. 2, a method for directly producing titanium and titanium alloys using titanium dioxide is provided in this embodiment, which uses a continuous production process, that is, first placing
可使液態金屬鋁2A與液態二氧化鈦2B按化學計量比加入到反應坩堝4裡發生化學反應;也可先加入部分液態金屬鋁2A與全量的液態二氧化鈦2B至反應坩堝4裡發生化學反應,然後補加餘量的金屬鋁粉至反應坩堝4裡,使繼續反應。因為液態金屬鋁2A與液態二氧化鈦2B為放熱反應,這樣可以充分利用反應熱維持繼續反應,以節約能耗。The
另外,在此需要說明的是,本發明所述化學反應優選在無氧條件下進行,例如:在惰性氣氛下或真空下進行,以避免發生氧化反應而影響產品純度和產量。In addition, it should be noted here that the chemical reaction of the present invention is preferably carried out under oxygen-free conditions, for example, under an inert atmosphere or under vacuum, so as to avoid the occurrence of oxidation reactions that affect product purity and yield.
最後需要在此指出的是:以上僅是本發明的部分優選實施例,不能理解為對本發明保護範圍的限制,本領域中具有通常知識者根據本發明的上述內容做出的一些非本質的改進和調整均屬於本發明的保護範圍。Finally, it should be pointed out here that: The above are only some of the preferred embodiments of the present invention, which cannot be understood as a limitation to the protection scope of the present invention, and some non-essential improvements made by those with ordinary knowledge in the art based on the above content of the present invention And adjustments belong to the protection scope of the present invention.
1、1A、1B、4‧‧‧坩堝2、2A‧‧‧鋁2B‧‧‧二氧化鈦3、3A、3B‧‧‧閥門5‧‧‧二氧化鈦6‧‧‧出料口7‧‧‧攪拌1. 1A, 1B, 4‧‧‧‧
第1圖是實施例1提供的一種利用二氧化鈦直接生產鈦及鈦合金的間歇式生產工藝流程示意圖。 第2圖是實施例2提供的一種利用二氧化鈦直接生產鈦及鈦合金的連續式生產工藝流程示意圖。FIG. 1 is a schematic diagram of a batch production process flow for directly producing titanium and titanium alloy using titanium dioxide provided in Example 1. FIG. Figure 2 is a schematic diagram of a continuous production process flow for directly producing titanium and titanium alloys using titanium dioxide provided in Example 2.
無no
1、4‧‧‧坩堝 1. 4‧‧‧‧Crucible
2‧‧‧鋁 2‧‧‧Aluminum
3‧‧‧閥門 3‧‧‧Valve
5‧‧‧二氧化鈦 5‧‧‧ Titanium dioxide
6‧‧‧出料口 6‧‧‧Discharge port
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CNCN201710711128.2 | 2017-08-18 |
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CN110343867A (en) * | 2018-04-03 | 2019-10-18 | 上海广谋能源技术开发有限公司 | A method of titanium or titanium alloy is directly produced using high titanium slag |
CN110343874A (en) * | 2018-04-03 | 2019-10-18 | 上海广谋能源技术开发有限公司 | A method of titanium or titanium alloy is directly produced using titanium ore |
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CN101967531A (en) * | 2010-10-21 | 2011-02-09 | 东北大学 | Method for preparing high-titanium iron by step-by-step metal thermal reduction |
CN104131128A (en) * | 2014-07-21 | 2014-11-05 | 东北大学 | Aluminum thermal self-propagating-injection depth reduction based method for preparing ferro-titanium |
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BR8402087A (en) * | 1984-05-04 | 1985-12-10 | Vale Do Rio Doce Co | PROCESS OF OBTAINING METALLIC TITANIUM FROM ANASTASIA CONCENTRATE, BY ALUMINOTERMIA AND MAGNESIOTERMIA |
US6117208A (en) * | 1998-04-23 | 2000-09-12 | Sharma; Ram A. | Molten salt process for producing titanium or zirconium powder |
CN100469910C (en) * | 2006-07-17 | 2009-03-18 | 中国科学院过程工程研究所 | Direct titanium alloy producing process with titanium containing mineral |
CN101487066B (en) * | 2009-03-03 | 2011-05-04 | 北京金坤宏宇矿业科技有限公司 | Industrial production method for directly producing iron and vanadium-titanium-aluminum alloy from iron concentrate |
CN101709381A (en) * | 2009-12-16 | 2010-05-19 | 段广学 | Method for producing high-titanium iron |
CN102921953A (en) * | 2012-10-31 | 2013-02-13 | 昆明理工大学 | Method of preparing metal titanium powder through TiO2 |
CN103555974B (en) * | 2013-10-24 | 2016-03-09 | 攀枝花学院 | Magnalium method produces high ferrotitanium alloy |
CN103911537B (en) * | 2014-03-31 | 2016-09-14 | 承德天大钒业有限责任公司 | A kind of aluminum vanadium ferrochrome titanium intermediate alloy and preparation method thereof |
CN105543516B (en) * | 2015-12-17 | 2017-06-13 | 东北大学 | The method that aluminothermic reduction titanium dioxide prepares aluminium titanium mother alloy in fused-salt medium |
CN107586971A (en) * | 2017-08-18 | 2018-01-16 | 王武生 | A kind of method that titanium or titanium alloy is directly produced using titanium dioxide |
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CN101967531A (en) * | 2010-10-21 | 2011-02-09 | 东北大学 | Method for preparing high-titanium iron by step-by-step metal thermal reduction |
CN104131128A (en) * | 2014-07-21 | 2014-11-05 | 东北大学 | Aluminum thermal self-propagating-injection depth reduction based method for preparing ferro-titanium |
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