CN109371262B - Method for recovering titanium element in titanium alloy waste by using aluminum liquid - Google Patents
Method for recovering titanium element in titanium alloy waste by using aluminum liquid Download PDFInfo
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- CN109371262B CN109371262B CN201811533625.9A CN201811533625A CN109371262B CN 109371262 B CN109371262 B CN 109371262B CN 201811533625 A CN201811533625 A CN 201811533625A CN 109371262 B CN109371262 B CN 109371262B
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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
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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
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/005—Preliminary treatment of scrap
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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
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/001—Dry processes
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/026—Alloys based on aluminium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/06—Making non-ferrous alloys with the use of special agents for refining or deoxidising
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C21/00—Alloys based on aluminium
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- 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
The invention discloses a method for recovering titanium element in titanium alloy waste by using aluminum liquid, which comprises the following steps: (1) crushing titanium alloy waste and removing impurities to obtain titanium alloy waste powder; (2) mixing the titanium alloy waste powder, potassium fluoroaluminate, potassium fluotitanate, magnesium powder and aluminum powder, and cold-pressing into a titanium blank; (3) and pressing the titanium blank into the aluminum melt, continuously stirring, and casting to form the aluminum-titanium intermediate alloy. The invention adopts industrial titanium alloy waste as a titanium source in the aluminum alloy, fully separates out titanium element in the titanium alloy through the complex molten salt reaction interaction of the titanium alloy waste, potassium fluoroaluminate, potassium fluotitanate, magnesium powder, aluminum powder and high-temperature aluminum liquid, and then dissolves the titanium element in the titanium alloy in aluminum to form an aluminum-titanium intermediate alloy, thereby achieving the purposes of fully absorbing the titanium element in the titanium alloy waste and effectively recycling the titanium element, and the recovery rate of the titanium element in the titanium alloy waste reaches more than 70 percent.
Description
Technical Field
The invention relates to a method for recovering metal waste, in particular to a method for recovering titanium element in titanium alloy waste by using aluminum liquid.
Background
The titanium alloy has the advantages of high strength, low density, corrosion resistance, no magnetism and the like, and is widely applied to the fields of aerospace, ships, chemical engineering, sports and the like. Chinese patents (200810232605.8, 201710029041.7 and 201610500892.0) disclose treatment modes of the residual materials, wherein the titanium alloy residual materials are mainly crushed into chip-shaped and small-particle-shaped forms, mixed with sponge titanium, pressed into electrode blocks and then welded, and subjected to vacuum consumable electrode furnace (VAR) remelting recovery or preparation of other brands of titanium alloys.
Titanium is the most common crystal grain refining additive in industrial aluminum alloy, and can refine aluminum alloy crystal grains, improve the density of castings, and reduce the shrinkage porosity and cracks of the castings, thereby improving the mechanical properties of the aluminum alloy castings. At present, titanium in the aluminum alloy is mainly added in the mode of aluminum-titanium intermediate alloy and titanium-containing composite salt, and the methods have the defects of high cost, large power consumption and the like. The aluminum-titanium intermediate alloy adopts pure aluminum and pure titanium as raw materials, is formed by smelting in vacuum, and has higher production cost. Chinese patent (201110073393.5) discloses a method for preparing titanium additive, which is prepared by mixing high-purity titanium powder and fluxing agent, but the cost is high by using the high-purity titanium powder as the titanium additive to directly process. Chinese patent 201210421567.7 discloses a method for preparing an aluminum-titanium alloy, but the method adopts pure titanium and pure aluminum added into pure magnesium to carry out molten salt reaction, but the melting point of titanium reaches more than 1700 ℃, and the melting points of aluminum and magnesium are lower than 700 ℃, so that the process is complex and the cost is high.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects and shortcomings in the background art and provide a method for recovering titanium element in titanium alloy waste by using aluminum liquid.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
a method for recovering titanium element in titanium alloy waste by using aluminum liquid comprises the following steps:
(1) crushing titanium alloy waste and removing impurities to obtain titanium alloy waste powder;
(2) mixing the titanium alloy waste powder, potassium fluoroaluminate, potassium fluotitanate, magnesium powder and aluminum powder, and cold-pressing into a titanium blank;
(3) and pressing the titanium blank into the aluminum melt, continuously stirring, and casting to form the aluminum-titanium intermediate alloy.
In the above method, preferably, in the step (2), the titanium alloy waste powder is 50 to 70 parts by weight, the potassium fluoroaluminate is 20 to 30 parts by weight, the potassium fluorotitanate is 5 to 10 parts by weight, the aluminum powder is 1 to 5 parts by weight, and the magnesium powder is 1 to 5 parts by weight. The raw materials added in the invention can generate molten salt reaction in the aluminum melt, thereby dissolving the titanium element in the titanium alloy in the aluminum liquid.
In the above method, preferably, in the step (3), the aluminum is heated to 750-800 ℃ to be melted, and then the titanium blank is pressed into the aluminum melt, stirred for more than 30min, and cast and formed to form the aluminum-titanium intermediate alloy.
In the above method, preferably, the pulverization is performed by pulverizing the titanium alloy scrap into titanium alloy scrap powder of 50 to 100 mesh. The applicant finds that the titanium alloy powder with the granularity less than 50 meshes can cause insufficient recovery of titanium, and the fine powder with the granularity more than 100 meshes can cause the titanium alloy powder to be oxidized into titanium oxide in the high-temperature melting process, so that the titanium element in the alloy is difficult to recover.
Preferably, the impurity removal treatment comprises magnetic separation for removing iron and soaking for removing chlorine.
In the above method, preferably, the soaking for dechlorination is to soak in an acidic solution or an alkaline solution, and after dechlorination, the material is dehydrated and vacuum-dried.
In the method, the titanium alloy waste preferably comprises one or more of titanium leftover materials and titanium cutting materials formed in industrial processing.
The invention adopts the industrial titanium alloy waste as the titanium source in the aluminum melt, and fully recycles the titanium element in the titanium alloy waste, thereby greatly reducing the cost of the titanium source, and the prepared aluminum-titanium intermediate alloy can be used as a grain refiner of aluminum alloy and can be used as a refining additive when other aluminum alloy grains are refined.
Compared with the prior art, the invention has the advantages that:
(1) the invention adopts industrial titanium alloy waste as a titanium source in the aluminum alloy, fully separates out titanium element in the titanium alloy through the complex molten salt reaction interaction of the titanium alloy waste, potassium fluoroaluminate, potassium fluotitanate, magnesium powder, aluminum powder and high-temperature aluminum liquid, and then dissolves the titanium element in the titanium alloy in aluminum to form an aluminum-titanium intermediate alloy, thereby achieving the purposes of fully absorbing the titanium element in the titanium alloy waste and effectively recycling the titanium element, and the recovery rate of the titanium element in the titanium alloy waste reaches more than 70 percent. And other elements except titanium in the titanium alloy waste are subjected to degassing refining in the molten aluminum in the form of a complex molten salt compound to form inclusions, and then the inclusions are separated from the molten aluminum.
(2) The titanium alloy intermediate alloy is prepared by cold-pressing titanium alloy waste powder, potassium fluoroaluminate, potassium fluotitanate, magnesium powder and aluminum powder into a titanium blank and then pressing the titanium blank into an aluminum melt.
(3) The invention has simple production process and high safety and reliability, forms the aluminum-titanium intermediate alloy which can be practically and industrially applied, and provides a new and cheap way and method for adding the titanium element in the industrial aluminum alloy.
Detailed Description
In order to facilitate an understanding of the present invention, the present invention will be described more fully and in detail with reference to the preferred embodiments, but the scope of the present invention is not limited to the specific embodiments below.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
In the following examples, the recovery rate of titanium element is (melt mass × titanium element mass fraction)/(added titanium element mass) × 100%, where titanium element mass fraction refers to the mass fraction of titanium element in the cast aluminum-titanium intermediate alloy, and added titanium element mass refers to the mass of titanium element in the titanium billet added to the melt.
Example 1:
a method for recovering titanium element in titanium alloy waste by using aluminum liquid comprises the following steps:
(1) crushing, crushing and screening leftover waste of Ti-6Al-4V titanium alloy to obtain waste titanium alloy powder of 50 meshes;
(2) carrying out magnetic separation on titanium alloy waste powder to remove iron, then soaking in a 3% hydrochloric acid solution to remove chlorine impurities, dehydrating, and carrying out vacuum drying treatment;
(3) uniformly mixing 50 parts by weight of the titanium alloy waste powder treated in the step (2) with 30 parts by weight of potassium fluoroaluminate, 10 parts by weight of potassium fluotitanate, 5 parts by weight of magnesium powder and 5 parts by weight of aluminum powder, and cold-pressing to obtain a titanium blank;
(4) melting pure aluminum at 800 ℃, pressing the titanium blank into an aluminum melt, stirring for 30min, and then casting to form to obtain the aluminum-titanium intermediate alloy.
Through chemical composition analysis and calculation, the recovery rate of the titanium element in the titanium alloy waste is 70%, the mass fraction of the titanium element in the aluminum-titanium intermediate alloy is 0.4%, and the aluminum-titanium intermediate alloy containing the titanium element can be used as a grain refiner in industrial aluminum alloy production.
Example 2:
a method for recovering titanium element in titanium alloy waste by using aluminum liquid comprises the following steps:
(1) titanium alloy cutting waste with the chemical components of Ti-5.5Al-4.5V-0.3Fe is crushed, crushed and screened to prepare 100-mesh titanium alloy waste powder;
(2) carrying out magnetic separation and iron removal on titanium alloy waste powder, then soaking in a 4% nitric acid solution to remove chlorine impurities, dehydrating, and carrying out vacuum drying treatment;
(3) mixing 70 parts by weight of titanium alloy waste powder with 22 parts by weight of potassium fluoroaluminate, 5 parts by weight of potassium fluotitanate, 2.5 parts by weight of magnesium powder and 2.5 parts by weight of aluminum powder, and cold-pressing to obtain a titanium blank;
(4) melting pure aluminum at 750 ℃, pressing the titanium blank into the melt, stirring for 40min, and then casting to form to obtain the aluminum-titanium intermediate alloy.
Through chemical composition analysis and calculation, the recovery rate of the titanium element in the titanium alloy waste is 80%, and the mass fraction of the titanium element in the aluminum-titanium intermediate alloy is 0.5%.
Example 3:
a method for recovering titanium element in titanium alloy waste by using aluminum liquid comprises the following steps:
(1) crushing, crushing and screening titanium alloy cutting waste with a chemical composition of Ti-5Al-3Sn-1Zr-0.5Mo to prepare titanium alloy waste powder with the particle size of 80 meshes;
(2) carrying out magnetic separation and iron removal on titanium alloy waste powder, then soaking the titanium alloy waste powder in a 3% acetic acid solution to remove chlorine impurities, dehydrating and carrying out vacuum drying treatment;
(3) mixing 65 parts by weight of titanium alloy waste powder with 20 parts by weight of potassium fluoroaluminate, 7.5 parts by weight of potassium fluotitanate, 3 parts by weight of magnesium powder and 4.5 parts by weight of aluminum powder, and cold-pressing to obtain a titanium blank;
(4) melting pure aluminum at 780 ℃, pressing the titanium blank into an aluminum melt, stirring for 60min, and then casting to form to obtain the aluminum-titanium intermediate alloy.
Through chemical composition analysis and calculation, the recovery rate of the titanium element in the titanium alloy waste is 85%, the mass fraction of the titanium element in the aluminum-titanium intermediate alloy is 1.0%, and the aluminum-titanium intermediate alloy can be used as an aluminum-titanium intermediate alloy additive in the aluminum alloy industry and as a grain refiner of the aluminum alloy.
Example 4:
a method for recovering titanium element in titanium alloy waste by using aluminum liquid comprises the following steps:
(1) crushing, crushing and screening the titanium alloy cutting waste material with the chemical composition of Ti-6Al-1Zr-2Mo to prepare 100-mesh titanium alloy waste material powder;
(2) carrying out magnetic separation and iron removal on titanium alloy waste powder, then soaking in a 4% nitric acid solution to remove chlorine impurities, dehydrating, and carrying out vacuum drying treatment;
(3) uniformly mixing 68 parts by weight of titanium alloy waste powder with 25 parts by weight of potassium fluoroaluminate, 5 parts by weight of potassium fluotitanate, 1 part by weight of magnesium powder and 1 part by weight of aluminum powder, and cold-pressing to obtain a titanium blank;
(4) melting pure aluminum at 770 ℃, pressing the titanium blank into an aluminum melt, stirring for 60min, and then casting to form to obtain the aluminum-titanium intermediate alloy.
Through chemical composition analysis and calculation, the recovery rate of the titanium element in the titanium alloy waste is 80%, and the mass fraction of the titanium element in the aluminum-titanium intermediate alloy is 0.45%.
Claims (4)
1. A method for recovering titanium element in titanium alloy waste by using aluminum liquid is characterized by comprising the following steps:
(1) crushing titanium alloy waste and removing impurities to obtain titanium alloy waste powder; the crushing refers to crushing the titanium alloy waste into 50-100 meshes of titanium alloy waste powder;
(2) mixing the titanium alloy waste powder, potassium fluoroaluminate, potassium fluotitanate, magnesium powder and aluminum powder, and cold-pressing into a titanium blank; the titanium alloy waste powder comprises, by weight, 50-70 parts of titanium alloy waste powder, 20-30 parts of potassium fluoroaluminate, 5-10 parts of potassium fluotitanate, 1-5 parts of aluminum powder and 1-5 parts of magnesium powder;
(3) firstly heating the aluminum to 750-800 ℃ for melting, then pressing the titanium blank into the aluminum melt, stirring for more than 30min, and casting and forming to form the aluminum-titanium intermediate alloy.
2. The method of claim 1, wherein the impurity removal treatment comprises magnetic separation iron removal and soaking chlorine removal.
3. The method of claim 2, wherein the dechlorination is followed by a dehydration and vacuum drying operation of the material.
4. The method of claim 1, wherein the titanium alloy scrap comprises one or more of titanium scrap and titanium cuttings formed during industrial processing.
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| CN101775499B (en) * | 2010-02-05 | 2011-04-06 | 新星化工冶金材料(深圳)有限公司 | Purification method of Al-Ti-B alloy melt |
| CN104278176B (en) * | 2013-07-01 | 2016-09-21 | 中国科学院金属研究所 | A kind of preparation method of high-quality Al-5Ti-1B intermediate alloy |
| RU2567768C2 (en) * | 2013-09-27 | 2015-11-10 | Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Курганский государственный университет" | Method of alloy production based on titanium from water suspension of particles of ore containing compounds of titanium, and device of its implementation |
| CN103773979B (en) * | 2014-03-04 | 2016-03-30 | 哈尔滨理工大学 | The method of aluminium titanium master alloy prepared by a kind of regeneration titanium bits or titanium scrap stock |
| CN104911376B (en) * | 2015-07-17 | 2017-01-04 | 东北大学 | Two sections of aluminothermic reduction Titaniums or titanium-aluminium alloy by-product are without the method for titanium cryolite |
| CN107586984B (en) * | 2017-09-07 | 2019-11-26 | 哈尔滨理工大学 | Al-Ti-C alloy and preparation method thereof |
| CN108220601A (en) * | 2018-02-11 | 2018-06-29 | 沈阳北冶冶金科技有限公司 | A kind of preparation method of titanium alloy |
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