Method for preparing TA1 or TA2 round ingot by using TA1 residual waste material
Through magnetic separation, classification, acid-base washing and electron beam cold bed refining, the problem of low utilization rate of TA1 metal waste material is solved, and the efficient preparation of TA1 and TA2 ingots is achieved, and the yield and production efficiency of titanium alloys are improved.
Patent Information
- Application Number
- CN202411778212.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-05
- Publication Date
- 2025-03-11
AI Technical Summary
The utilization rate of TA1 metal waste is low, and the secondary utilization cost is high, resulting in waste of resources. The existing technology has problems such as complex process and many metallurgical defects.
TA1 or TA2 round ingots are prepared by magnetic separation, sorting by color, acid-base washing, adding titanium agent and pressing them into ingots, and finally undergoing electron beam cold bed refining to prepare TA1 or TA2 round ingots.
The efficient utilization of TA1 waste materials is achieved, the yield of TA1 and TA2 titanium alloys is improved, high-density inclusions are avoided, and production efficiency and strength are ensured.
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of metal material processing, and in particular to a method for preparing TA1 or TA2 round ingots by utilizing TA1 waste materials. Background Art
[0002] Panxi area is an important base of titanium resources in China, with rich vanadium-titanium magnetite resources. Panxi area accounts for 91% of the national titanium resource reserves and 35.2% of the global titanium resource reserves. Therefore, Panxi area has developed many titanium industries, including sponge titanium production and the manufacture of industrial pure titanium. TA1 is an industrial pure titanium material, which has many excellent properties in industrial production, such as low density, high strength, good corrosion resistance, good heat resistance, etc. Its excellent properties make it widely used in many fields such as aerospace, chemical industry, and medical treatment. However, after industrial cutting, TA1 metal often produces a large amount of residual waste.
[0003] At present, the utilization rate of TA1 scrap materials is relatively low, the cost of secondary utilization is high, and it also causes waste of resources; the background reasons for this situation are mainly the following: First, the processing technology of TA1 metal is relatively high, and the scrap materials after cutting are often difficult to reuse directly, and need to be reprocessed or recycled; secondly, there is a lack of effective technology and management methods for the recycling and reuse of scrap materials, resulting in high recycling costs and low efficiency; this situation not only has a negative impact on the economic benefits of the enterprise, but also does not conform to the concept of sustainable development. Improving the utilization rate of TA1 metal scrap materials and reducing the cost of secondary utilization have become issues that need to be urgently addressed in the current industrial field.
[0004] In the prior art, CN118835105A discloses a method for preparing TA2 ingots from TA1 block waste by VAR smelting through a titanium tube oxygenation process, the method comprising the following steps: step 1, classifying, collecting and storing the TA1 block waste generated in the production process of TA1 brand products, including plate edges, rod heads, risers and runners; step 2, alkali washing and acid washing the TA1 block waste stored in step 1 to obtain the treated TA1 block waste; step 3, performing appearance inspection and chemical composition confirmation on the TA1 block waste treated in step 2; step 4, calculating the required TiO2 powder to be added according to the chemical composition requirements of the target product TA2 ingot, then loading the TiO2 powder into the TA1 titanium tube and sealing it, then welding the sealed TA1 titanium tube with the TA1 block waste after inspection and confirmation in step 3 to prepare bundled electrodes, and performing VAR smelting to obtain TA2 ingots. The TA1 block residue and the TA1 titanium tube with TiO2 powder added are recycled by VAR smelting to obtain TA2 ingots. The chemical composition of the TA2 ingot meets the requirements of GB / T 3620.1-2016 "Titanium and Titanium Alloy Grades and Chemical Compositions". The TA1 block residue is effectively recycled and smelted into TA2 ingots, which reduces the production cost of titanium materials and is conducive to the promotion of large-scale application of titanium materials. However, this method has the following problems: 1. In the pretreatment process, the TiO2 powder is required to be loaded into the TA1 titanium tube and sealed, and the TA1 titanium tube is required to be large and cumbersome and inconvenient; 2. It is extremely difficult to prepare bundled electrodes with irregular TA1 block residues and TA1 titanium tubes. Even if electrodes are made, the VAR smelting process is difficult to stabilize; 3. The TA2 ingot obtained by VAR smelting is prone to metallurgical defects, which are difficult to eliminate by homogenization or hot working, limiting the use of TA2 ingots, especially limiting the requirement that TA2 bears a certain load. Summary of the invention
[0005] The present invention provides a method for preparing TA1 or TA2 ingots by utilizing TA1 waste materials, which has the advantages of short process, high yield, simple process and avoidance of high-density inclusions.
[0006] The technical solution of the present invention to solve the above technical problems is as follows: A method for preparing TA1 or TA2 ingots using TA1 waste material comprises the following steps: Step 1): magnetic separation, iron removal, collection and storage of TA1 block residues generated during the production process of TA1 brand products; the TA1 block residues include plate edges, rod heads, risers and runners; Step 2): Classify the TA1 block waste materials in step 1) by color, and perform component detection on each classification of the TA1 block waste materials; Step 3): The TA1 block waste material of any classification in step 2) is subjected to alkali washing and / or acid washing to obtain acid-alkali washed TA1 waste material; Step 4): According to the chemical composition requirements of the target product TA1 or TA2 and the component detection results of step 2), a titanium agent is added to the acid-base washed TA1 residue, and the mixture is pressed into an ingot to obtain a mixed waste ingot; or, the acid-base washed TA1 residue and the titanium agent are pressed into ingots respectively to obtain a single waste ingot and a titanium agent ingot; Step 5): The single waste ingot and the titanium agent ingot of step 4) are placed in layers and subjected to electron beam cold bed refining, or the mixed waste ingot of step 4) is subjected to electron beam cold bed refining to obtain TA1 ingot or TA2 ingot; wherein, the electron beam cold bed refining performs two-stage scanning, the first stage scanning is a large-range grid surface scanning, and the parameters are controlled as follows: 20-50KW, vacuum 0.01-0.08Pa, and time 100-160min; the second stage scanning is a grid scanning, and the parameters are controlled as follows: 90-120KW, vacuum 0.005-0.01Pa, and time 60-100min.
[0007] The present invention can prepare TA1 ingots and TA2 ingots by using TA1 waste materials, and the prepared titanium alloy products meet the performance requirements for grades TA1 and TA2 in GB2965-2007 "Titanium and Titanium Alloy Bars".
[0008] In a specific embodiment of the present invention, in step 2), the classification is carried out according to the surface gloss of the TA1 block residue being silvery white metallic color, blue and purple red.
[0009] In a specific embodiment of the present invention, in step 2), the surface of the TA1 block residue is free of oil stains.
[0010] In a specific embodiment of the present invention, in step 2), the requirements for component detection are: Ti ≥ 99wt%, Fe ≤ 0.20wt%, O ≤ 0.18wt%, and the single content of other impurity elements ≤ 0.1wt%.
[0011] In a specific embodiment of the present invention, in step 3), the alkali washing is performed by using an alkali washing agent at 400-470° C. for 60-120 min and drying.
[0012] In a specific embodiment of the present invention, the alkaline cleaning agent is a mixture of sodium hydroxide and sodium carbonate in a mass ratio of 1: (1-2).
[0013] In a specific embodiment of the present invention, in step 3), the pickling is performed by using a pickling solution prepared by mixing water, nitric acid and hydrofluoric acid in a volume ratio of 92:5:3 for 60 to 120 minutes and then drying.
[0014] In a specific embodiment of the present invention, in step 4), the titanium agent is any one of titanium sponge, titanium hydride, titanium dioxide or any combination thereof.
[0015] In a specific embodiment of the present invention, the amount of titanium dioxide used is 0.1-0.5 kg, and the amount of titanium sponge and / or titanium hydride used is 5-100 kg per 100 kg of acid-base washed TA1 residue.
[0016] In a specific embodiment of the present invention, in step 4), the single waste ingot and the titanium agent ingot are placed in layers, and the single waste ingot is placed above the titanium agent ingot.
[0017] The beneficial effects of the present invention are: 1. The process of the present invention is simple, the utilization rate of TA1 waste material is high, and the yield rate of titanium alloys with grades TA1 and TA2 is high; 2. The method of the present invention can avoid high-density inclusions of TA1 / TA2 and ensure the production efficiency and strength of TA1 / TA2. DETAILED DESCRIPTION
[0018] To make the purpose, technical solution and advantages of the present invention clearer, the technical solution of the present invention will be described in detail below. Obviously, the described embodiments are only part of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments of the present invention, all other implementation methods obtained by ordinary technicians in this field without creative work belong to the scope of protection of the present invention.
[0019] A method for preparing TA1 or TA2 ingots using TA1 waste material comprises the following steps: Step 1): magnetic separation, iron removal, collection and storage of TA1 block residues generated during the production process of TA1 brand products; the TA1 block residues include plate edges, rod heads, risers and runners; Step 2): Classify the TA1 block waste materials in step 1) by color, and perform component detection on each classification of the TA1 block waste materials; Step 3): The TA1 block waste material of any classification in step 2) is subjected to alkali washing and / or acid washing to obtain acid-alkali washed TA1 waste material; Step 4): According to the chemical composition requirements of the target product TA1 or TA2 and the component detection results of step 2), a titanium agent is added to the acid-base washed TA1 residue, and the mixture is pressed into an ingot to obtain a mixed waste ingot; or, the acid-base washed TA1 residue and the titanium agent are pressed into ingots respectively to obtain a single waste ingot and a titanium agent ingot; Step 5): The single waste ingots and the titanium agent ingots of step 4) are placed in layers and subjected to electron beam cold bed refining, or the mixed waste ingots of step 4) are subjected to electron beam cold bed refining to obtain TA1 / TA2 round ingots; wherein, the electron beam cold bed refining performs two-stage scanning, the first stage scanning is a large-range grid surface scanning, and the parameters are controlled as follows: 20~50KW, vacuum 0.01~0.08Pa, time 100~160min; the second stage scanning is a grid scanning, and the parameters are controlled as follows: 90~120KW, vacuum 0.005~0.01Pa, time 60~100min.
[0020] In some examples, in step 2), the classification is performed based on the surface gloss of the TA1 block residues being silvery white metallic, blue and purple red.
[0021] In some examples, in step 2), the surface of the TA1 block residue is free of oil stains.
[0022] In some examples, in step 2), the requirements for component detection are: Ti ≥ 99wt%, Fe ≤ 0.20wt%, O ≤ 0.18wt%, and the single content of other impurity elements ≤ 0.1wt%.
[0023] In some examples, in step 3), the alkali washing is performed using an alkali washing agent at 400-470° C. for 60-120 min and then drying.
[0024] In some examples, the alkaline cleaning agent is a mixture of sodium hydroxide and sodium carbonate in a mass ratio of 1: (1-2).
[0025] In some examples, in step 3), the pickling is performed by using a pickling solution prepared by mixing water, nitric acid and hydrofluoric acid in a volume ratio of 92:5:3 for 60 to 120 minutes, followed by drying.
[0026] In some examples, in step 4), the titanium agent is titanium dioxide.
[0027] In some examples, the amount of titanium dioxide used is 0.1-0.5 g per 100 g of acid-base washed TA1 residue.
[0028] In some examples, in step 4), the titanium agent is any one of titanium sponge, titanium hydride, titanium dioxide, or any combination thereof.
[0029] In some examples, the amount of titanium dioxide used is 0.1-0.5 kg, and the amount of titanium sponge and / or titanium hydride used is 5-100 kg per 100 kg of acid-base washed TA1 residue.
[0030] In some examples, in step 4), the single waste material ingot and the titanium agent ingot are placed in layers, and the single waste material ingot is placed above the titanium agent ingot.
[0031] To further demonstrate the effect of the method of the present invention in improving the recovery rate of TA1 waste materials, the following examples are provided: Example 1 This embodiment provides a method for preparing TA1 ingots using TA1 waste materials, comprising the following steps: 1. Collect and store blocky waste materials such as plate edges, rod heads, risers and runners generated during the processing of TA1 brand products; 2. According to the silver-white metallic color, blue and purple-red color of titanium alloy scrap, deep learning is carried out to complete the color recognition, classification and composition detection of TA1 block scrap; after classification, the mass ratio of silver-white metallic color, blue and purple-red TA1 scrap is 3:1:1; 3. The silvery white metallic and blue residual materials are washed with a molten alkaline solution at 450°C for 60 minutes and then dried; wherein the alkaline solution is a solid made by mixing sodium hydroxide and sodium carbonate in a mass ratio of 2:3 and melting at 450°C; 4. Use pickling solution to pickle the residual waste for 80 minutes, filter and dry; the pickling solution is prepared by mixing water, nitric acid and hydrofluoric acid in a volume ratio of 92:5:3; 5. Element detection was performed on the TA1 scrap after pickling. In terms of weight percentage, the components of the TA1 scrap were: titanium 99.2wt%, iron 0.26wt%, carbon 0.05wt%, and oxygen 0.17wt%. 6. Take the waste material after pickling, add 20kg of sponge titanium block material to every 100kg of waste material, press the waste material into waste material ingots, and press the sponge titanium into sponge titanium ingots; 7. Put the pressed titanium sponge ingot and the single waste ingot into the cooling bed furnace. The material distribution method is: the lower layer is titanium sponge ingot, and the upper layer is waste ingot; 8. The laid materials are refined by electron beam cold bed with cold cathode electron gun to obtain TA1 round ingots with a diameter of 200 mm. The electron beam cold bed adopts two-stage scanning as much as possible. The first stage scanning is grid large-scale surface scanning, and the parameters are controlled as follows: 20-50KW, vacuum 0.03Pa, and time 100min; the second stage scanning is grid scanning, and the parameters are controlled as follows: 90-120KW, vacuum 0.003Pa, and time 60min.
[0032] The composition of the TA1 ingot prepared in this embodiment is: 99.5wt% titanium, 0.21wt% iron, 0.06wt% carbon, and 0.17wt% oxygen.
[0033] The utilization rate of the TA1 waste material in this embodiment is 83.7%.
[0034] Example 2 This embodiment provides a method for preparing TA1 ingots using TA1 waste materials, comprising the following steps: 1. Collect and store blocky waste materials such as plate edges, rod heads, risers and runners generated during the processing of TA1 brand products; 2. According to the silver-white metallic color, blue and purple-red color of titanium alloy scraps, deep learning is carried out to complete the color recognition, classification and composition detection of TA1 block scraps; after classification, the mass ratio of silver-white metallic color, blue and purple-red TA1 scraps is 1:2:1; 3. Wash the silvery white metallic and blue TA1 waste materials with molten alkaline solution at 450°C for 70 minutes and dry them; wherein the alkaline solution is a solid prepared by mixing sodium hydroxide and sodium carbonate in a mass ratio of 2:3 and melting at 450°C; 4. Use pickling solution to pickle the residual waste for 80 minutes, filter and dry; the pickling solution is prepared by mixing water, nitric acid and hydrofluoric acid in a volume ratio of 92:5:3; 5. Element detection was performed on the TA1 scrap after pickling. In terms of weight percentage, the components of the TA1 scrap were: titanium 99.3wt%, iron 0.24wt%, carbon 0.05wt%, and oxygen 0.18wt%. 6. Take the waste material after pickling, add 30kg of sponge titanium block material for every 100kg of waste material, press the waste material into single waste material ingots, and press the sponge titanium into sponge titanium ingots; 7. Put the pressed titanium sponge ingots and waste ingots into the cooling furnace. The material distribution method is: the lower layer is titanium sponge blocks, and the upper layer is waste ingots; 8. The laid materials are refined by electron beam cold bed with cold cathode electron gun to obtain TA1 round ingots with a diameter of 200 mm. The electron beam cold bed adopts two-stage scanning as much as possible. The first stage scanning is grid large-scale surface scanning, and the parameters are controlled as follows: 20-50KW, vacuum 0.03Pa, and time 100min; the second stage scanning is grid scanning, and the parameters are controlled as follows: 90-120KW, vacuum 0.003Pa, and time 60min.
[0035] The composition of the TA1 ingot prepared in this embodiment is: 99.3wt% titanium, 0.19wt% iron, 0.06wt% carbon, and 0.22wt% oxygen.
[0036] The utilization rate of the TA1 waste material in this embodiment is 74.1%.
[0037] Example 3 This embodiment provides a method for preparing TA1 ingots using TA1 waste materials, comprising the following steps: 1. Collect and store blocky waste materials such as plate edges, rod heads, risers and runners generated during the processing of TA1 brand products; 2. Based on the silver-white metallic color, blue color and purple-red color of titanium alloy scraps, deep learning was performed to complete the color recognition, classification and composition detection of TA1 block scraps; after classification, the mass ratio of silver-white metallic color, blue color and purple-red scraps was 1:3:1; 3. Wash the TA1 waste material with a molten alkaline washing liquid at 450°C for 70 minutes and dry it; wherein the alkaline washing liquid is a solid made by mixing sodium hydroxide and sodium carbonate in a mass ratio of 2:3 and melting it at 450°C; 4. Use pickling solution to pickle the residual waste for 80 minutes, filter and dry; the pickling solution is prepared by mixing water, nitric acid and hydrofluoric acid in a volume ratio of 92:5:3; 5. Perform element detection on the TA1 scrap after pickling. In terms of weight percentage, the components of the TA1 scrap are: titanium 99.1wt%, iron 0.24wt%, carbon 0.05wt%, oxygen 0.20wt%; 6. Take the residual waste after pickling, add 20kg of titanium sponge and 5kg of titanium hydride for every 100kg of residual waste, press the residual waste into residual waste ingots, and mix the titanium sponge and titanium hydride to press into mixed titanium agent ingots; 7. Put the pressed mixed titanium ingots and waste ingots into the cooling furnace, and place them in the following way: the lower layer is the mixed titanium ingots, and the upper layer is the waste ingots; 8. The laid materials are refined by electron beam cold bed with cold cathode electron gun to obtain TA1 round ingots with a diameter of 200 mm. The electron beam cold bed adopts two-stage scanning as much as possible. The first stage scanning is grid large-scale surface scanning, and the parameters are controlled as follows: 20-50KW, vacuum 0.05Pa, and time 120min; the second stage scanning is grid scanning, and the parameters are controlled as follows: 90-120KW, vacuum 0.005Pa, and time 80min.
[0038] The composition of the TA1 ingot prepared in this embodiment is: 99.3wt% titanium, 0.18wt% iron, 0.06wt% carbon, and 0.19wt% oxygen.
[0039] The utilization rate of the TA1 waste material in this embodiment is 81.4%.
[0040] Example 4 This embodiment provides a method for preparing TA1 ingots using TA1 waste materials, comprising the following steps: 1. Collect and store blocky waste materials such as plate edges, rod heads, risers and runners generated during the processing of TA1 brand products; 2. According to the silver-white metallic color, blue and purple-red color of titanium alloy scraps, deep learning is carried out to complete color recognition, classification and component detection of TA1 block scraps; after classification, the mass ratio of silver-white metallic color, blue and purple-red scraps is 1:3:1; 3. The silvery white metallic and blue TA1 waste materials are washed with a molten alkaline solution at 450°C for 70 minutes and then dried; wherein the alkaline solution is a solid made by mixing sodium hydroxide and sodium carbonate in a mass ratio of 2:3 and melting at 450°C; 4. Use pickling solution to pickle the residual waste for 80 minutes, filter and dry; the pickling solution is prepared by mixing water, nitric acid and hydrofluoric acid in a volume ratio of 92:5:3; 5. Perform element detection on the TA1 scrap after pickling. In terms of weight percentage, the components of the TA1 scrap are: titanium 99.1wt%, iron 0.24wt%, carbon 0.05wt%, oxygen 0.16wt%; 6. Take the residual waste after pickling, add 15kg of sponge titanium for every 100kg of residual waste, press the residual waste into residual waste ingots, and press the sponge titanium into sponge titanium ingots; 7. Put the pressed titanium sponge ingots and waste ingots into the cooling bed furnace. The material distribution method is: the lower layer is titanium sponge ingots, and the upper layer is waste ingots; 8. The laid materials are refined by electron beam cold bed with cold cathode electron gun to obtain TA1 round ingots with a diameter of 200 mm. The electron beam cold bed adopts two-stage scanning as much as possible. The first stage scanning is grid large-scale surface scanning, and the parameters are controlled as follows: 20-50KW, vacuum 0.05Pa, and time 120min; the second stage scanning is grid scanning, and the parameters are controlled as follows: 90-120KW, vacuum 0.005Pa, and time 80min.
[0041] The composition of the TA1 ingot prepared in this embodiment is: 99.3wt% titanium, 0.20wt% iron, 0.06wt% carbon, and 0.19wt% oxygen.
[0042] The utilization rate of the TA1 waste material in this embodiment is 83.8%.
[0043] Example 5 This embodiment provides a method for preparing TA2 ingots using TA1 scrap material, comprising the following steps: 1. Collect and store blocky waste materials such as plate edges, rod heads, risers and runners generated during the processing of TA1 brand products; 2. Titanium alloy scraps are deeply learned according to silver-white metallic color, blue and purple-red, and TA1 block scraps are color identified, classified and component tested; after classification, the mass ratio of silver-white metallic color, blue and purple-red scraps is 1:2:1; 3. Wash the blue and purple TA1 waste materials with molten alkaline solution at 450°C for 60 minutes and dry them; wherein the alkaline solution is a solid made by mixing sodium hydroxide and sodium carbonate in a mass ratio of 2:3 and melting at 450°C; 4. Perform appearance inspection and element detection on the TA1 waste material after alkali washing. The components of the TA1 waste material are as follows: 99.2wt% titanium, 0.28wt% iron, 0.05wt% carbon, and 0.18wt% oxygen, by weight percentage; add 20kg titanium sponge and 0.44kg titanium dioxide to every 100kg of the waste material, press the waste material into waste material ingots, and mix the titanium sponge with the two samples and press them into mixed titanium agent ingots; 5. Put the pressed mixed titanium ingots and waste ingots into the cooling furnace, and the material distribution method is: the lower layer is the mixed titanium ingots, and the upper layer is the waste ingots; 6. The laid materials are subjected to electron beam cold bed refining with a cold cathode electron gun to obtain TA2 ingots; the electron beam cold bed adopts two-stage scanning as much as possible, the first stage of scanning is a large-scale grid surface scanning, and the parameters are controlled as follows: 20-50KW, vacuum 0.03Pa, time 100min; the second stage of scanning is a grid scanning, and the parameters are controlled as follows: 90-120KW, vacuum 0.003Pa, time 60min.
[0044] The composition of the TA2 ingot prepared in this embodiment is: 99.0wt% titanium, 0.22wt% iron, 0.06wt% carbon, and 0.24wt% oxygen. The utilization rate of TA1 waste material is 81.9%.
[0045] Example 6 This embodiment provides a method for preparing TA2 ingots using TA1 scrap material, comprising the following steps: 1. Collect and store blocky waste materials such as plate edges, rod heads, risers and runners generated during the processing of TA1 brand products; 2. Deep learning was performed on titanium alloy scrap materials according to silver-white metallic color, blue and purple-red, and color recognition, classification and composition detection of TA1 block scrap materials were completed; after classification, the mass ratio of silver-white metallic color, blue and purple-red scrap materials was 1:1:3; 3. Wash the blue and purple TA1 waste materials with molten alkaline solution at 450°C for 60 minutes and dry them; the alkaline solution is a solid made by mixing sodium hydroxide and sodium carbonate in a mass ratio of 2:3 and melting at 450°C; 4. Perform appearance inspection and element detection on the TA1 waste material after alkali washing. The components of the TA1 waste material are as follows: titanium 99.2wt%, iron 0.21wt%, carbon 0.05wt%, oxygen 0.21wt% by weight; 5. Add 20kg of titanium sponge and 0.44kg of titanium dioxide to every 100kg of waste material, press the waste material into waste material ingots, and mix the titanium sponge and titanium dioxide and press them into mixed titanium agent ingots; 6. Put the pressed mixed titanium ingots and waste ingots into the cooling furnace, and the material distribution method is: the lower layer is the mixed titanium ingots, and the upper layer is the waste ingots; 7. The laid materials are subjected to electron beam cold bed refining with a cold cathode electron gun to obtain TA2 ingots; the electron beam cold bed adopts two-stage scanning as much as possible, the first stage of scanning is a large-scale grid surface scanning, and the parameters are controlled as follows: 20-50KW, vacuum 0.05Pa, time 120min; the second stage of scanning is a grid scanning, and the parameters are controlled as follows: 90-120KW, vacuum 0.005Pa, time 80min.
[0046] The composition of the TA2 ingot prepared in this embodiment is: 99.0wt% titanium, 0.18wt% iron, 0.06wt% carbon, and 0.24wt% oxygen.
[0047] In this embodiment, the utilization rate of TA1 waste material is 82.2%.
[0048] Example 7 1. Collect and store blocky waste materials such as plate edges, rod heads, risers and runners generated during the processing of TA1 brand products; 2. Deep learning was performed on titanium alloy scrap materials according to silver-white metallic color, blue and purple-red, and color recognition, classification and composition detection of TA1 block scrap materials were completed; after classification, the mass ratio of silver-white metallic color, blue and purple-red scrap materials was 1:1:3; 3. Wash the blue and purple TA1 waste materials with molten alkaline solution at 450°C for 60 minutes and dry them; wherein the alkaline solution is a solid made by mixing sodium hydroxide and sodium carbonate in a mass ratio of 2:3 and melting at 450°C; 4. Perform appearance inspection and element detection on the TA1 waste material after alkali washing. The components of the TA1 waste material are as follows: titanium 99.2wt%, iron 0.21wt%, carbon 0.05wt%, oxygen 0.22wt% by weight; 5. Add 15kg of titanium sponge and 0.3kg of titanium dioxide to every 100kg of waste material, press the waste material into waste material ingots, and mix the titanium sponge and titanium dioxide and press them into mixed titanium agent ingots; 6. Put the pressed mixed titanium ingots and waste ingots into the cooling furnace, and the material distribution method is: the lower layer is the mixed titanium ingots, and the upper layer is the waste ingots; 7. The laid materials are subjected to electron beam cold bed refining with a cold cathode electron gun to obtain TA2 ingots; the electron beam cold bed adopts two-stage scanning as much as possible, the first stage of scanning is a large-scale grid surface scanning, and the parameters are controlled as follows: 20-50KW, vacuum 0.05Pa, time 120min; the second stage of scanning is a grid scanning, and the parameters are controlled as follows: 90-120KW, vacuum 0.005Pa, time 80min.
[0049] The composition of the TA2 ingot prepared in this embodiment is: 99.0wt% titanium, 0.20wt% iron, 0.06wt% carbon, and 0.24wt% oxygen.
[0050] In this embodiment, the utilization rate of TA1 waste material is 84.6%.
[0051] Example 8 1. Collect and store blocky waste materials such as plate edges, rod heads, risers and runners generated during the processing of TA1 brand products; 2. Deep learning is performed on titanium alloy scrap materials according to silver-white metallic color, blue and purple-red, and color recognition, classification and component detection of TA1 block scrap materials are completed. After classification, the mass ratio of silver-white metallic color, blue and purple-red scrap materials is 1:1:3; 3. Wash the blue and purple TA1 waste materials with molten alkaline solution at 450°C for 60 minutes and dry them; the alkaline solution is a solid made by mixing sodium hydroxide and sodium carbonate in a mass ratio of 2:3 and melting at 450°C; 4. Perform appearance inspection and element detection on the TA1 waste material after alkali washing. The components of the TA1 waste material are as follows: titanium 99.2wt%, iron 0.21wt%, carbon 0.05wt%, oxygen 0.22wt% by weight; 5. Add 10kg of titanium sponge and 0.26kg of titanium dioxide to every 100kg of waste material, mix the waste material, titanium sponge and titanium dioxide, and press them into mixed waste material ingots; 6. The mixed waste ingots are subjected to electron beam cold bed refining with a cold cathode electron gun to obtain TA2 round ingots; wherein, the electron beam cold bed adopts two-stage scanning as much as possible, the first stage scanning is a large-scale grid surface scanning, and the parameters are controlled as follows: 20-50KW, vacuum 0.05Pa, time 120min; the second stage scanning is a grid scanning, and the parameters are controlled as follows: 90-120KW, vacuum 0.005Pa, time 80min.
[0052] The composition of the TA2 ingot prepared in this embodiment is: 99.0wt% titanium, 0.20wt% iron, 0.06wt% carbon, and 0.24wt% oxygen.
[0053] In this embodiment, the utilization rate of TA1 waste material is 88.6%.
Claims
1. A method for preparing TA1 or TA2 ingots using TA1 waste material, characterized in that: The following steps are involved: Step 1): magnetic separation, iron removal, collection and storage of TA1 block residues generated during the production process of TA1 brand products; the TA1 block residues include plate edges, rod heads, risers and runners; Step 2): Classify the TA1 block waste materials in step 1) by color, and perform component detection on each classification of the TA1 block waste materials; Step 3): The TA1 block waste material of any classification in step 2) is subjected to alkali washing and / or acid washing to obtain acid-alkali washed TA1 waste material; Step 4): According to the chemical composition requirements of the target product TA1 or TA2 and the component detection results of step 2), a titanium agent is added to the acid-base washed TA1 residue, and the mixture is pressed into an ingot to obtain a mixed waste ingot; or, the acid-base washed TA1 residue and the titanium agent are pressed into ingots respectively to obtain a single waste ingot and a titanium agent ingot; Step 5): The single waste ingots and the titanium agent ingots of step 4) are placed in layers and subjected to electron beam cold bed refining, or the mixed waste ingots of step 4) are subjected to electron beam cold bed refining to obtain TA1 / TA2 round ingots; wherein, the electron beam cold bed refining performs two-stage scanning, the first stage scanning is a large-range grid surface scanning, and the parameters are controlled as follows: 20~50KW, vacuum 0.01~0.08Pa, time 100~160min; the second stage scanning is a grid scanning, and the parameters are controlled as follows: 90~120KW, vacuum 0.005~0.01Pa, time 60~100min.
2. The method according to claim 1, characterized in that: Step 2), the classification is based on the surface gloss of the TA1 block residue being silvery white metallic, blue and purple red.
3. The method according to claim 1, characterized in that: Step 2), the surface of the TA1 block residue is free of oil stains.
4. The method according to claim 1, characterized in that: Step 2), the requirements for component detection are: Ti ≥ 99wt%, Fe ≤ 0.3wt%, O ≤ 0.18wt%, and the single content of other impurity elements ≤ 0.1wt%.
5. The method according to claim 1, characterized in that: Step 3), the alkali washing is performed by using an alkali washing agent at 400-470° C. for 60-120 minutes and drying.
6. The method according to claim 2, characterized in that: The alkaline cleaning agent is a mixture of sodium hydroxide and sodium carbonate in a mass ratio of 1: (1-2).
7. The method according to claim 1, characterized in that: Step 3), the pickling is carried out by using a pickling solution prepared by mixing water, nitric acid and hydrofluoric acid in a volume ratio of 92:5:3 for pickling for 60 to 120 minutes and drying.
8. The method according to claim 1, characterized in that: Step 4), the titanium agent is any one or any combination of titanium sponge, titanium hydride, and titanium dioxide.
9. The method according to claim 8, characterized in that: For every 100 kg of acid-base washed TA1 residue, the amount of titanium dioxide used is 0.1-0.5 kg, and the amount of sponge titanium and / or titanium hydride used is 5-100 kg.
10. The method according to claim 1, characterized in that: Step 4), the single waste ingot and the titanium agent ingot are placed in layers, and the single waste ingot is placed above the titanium agent ingot.