Method for preventing titanium lump combustion, nitridation and impurity mixing in titanium sponge production
By injecting oxygen or inert gas into the reaction chamber to treat the titanium lump, the problem of titanium lump combustion and nitride mixing in sponge titanium production is solved, and the stable production of high-quality sponge titanium is achieved.
Patent Information
- Application Number
- CN202510639104.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-05-19
- Publication Date
- 2025-07-29
AI Technical Summary
The prior art is difficult to effectively prevent the combustion and nitride from mixing in titanium sponge in the production of titanium sponge, especially when the titanium lump is removed from the room temperature atmosphere, there is a risk of combustion and nitride generation, which affects product quality.
After vacuum separation and purification, oxygen or a mixture of oxygen and inert gas is injected into the reaction chamber, and introduced into the gap between the furnace cover and the inner wall of the furnace body through the gas valve pipe, inactivate the impurities, and after cooling, open the furnace cover and remove the titanium lump.
Effectively prevent the combustion and nitride generation of titanium lumps when taken out, ensure high-quality production of sponge titanium and reduce the concentration of impurity attachments.
Smart Images
Figure CN120384201A_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of titanium sponge production, and specifically to a method for preventing combustion, nitridation and impurity mixing of titanium ingots during titanium sponge production. Background Art
[0002] During industrial production of titanium ingots, the method of reducing titanium tetrachloride with metallic magnesium in a sealed reaction vessel is often used. The produced titanium ingots contain impurities such as magnesium chloride and need to be purified by vacuum separation. However, titanium ingots are chemically active and will burn violently when contacting air at high temperatures, generating titanium oxides and nitrides. Even at normal temperatures in the atmosphere, the titanium ingots after vacuum separation and purification are prone to burning when encountering a tiny ignition source. The nitrides of titanium generated by this combustion are serious harmful factors during the processes of processing titanium ingots into extended materials, forgings, etc. Therefore, during the manufacture of titanium ingots, the reaction vessel needs to be maintained in an inert gas or vacuum environment, and the titanium sponge ingots in the reaction vessel need to be fully cooled before being taken out of the reaction vessel to prevent their combustion. In the past, there was a method of pre-introducing a certain amount of air into the reaction vessel to inactivate the active impurities and then opening the vessel. However, although this method can prevent combustion to a certain extent, due to the risk of nitrogen in the air causing the formation of titanium nitrides, it is impossible to fundamentally avoid the mixing of nitrides into the titanium ingots. Summary of the Invention
[0003] Aiming at the deficiencies of the prior art, the present invention provides a method for preventing combustion, nitridation and impurity mixing of titanium ingots during titanium sponge production, and solves the problems raised in the above background art.
[0004] To achieve the above objectives, the present invention is realized through the following technical solutions: A method for preventing combustion, nitridation and impurity mixing of titanium ingots during titanium sponge production, the method comprising the following steps: Step 1: Inject titanium tetrachloride into the reaction chamber through a feeding pipe, and titanium tetrachloride reacts with the previously injected metallic magnesium to generate titanium ingots and magnesium chloride; Step 2: Discharge magnesium chloride through a magnesium chloride discharge pipe. After the reduction reaction is completed, titanium ingots containing residual magnesium and magnesium chloride impurities are obtained in the reaction chamber. At this time, the reaction chamber is evacuated to a vacuum and heated by a vacuum pipe, so that magnesium and magnesium chloride are vaporized and then discharged through other gas valve pipes; Step 3: Before opening the furnace lid, inject oxygen or a mixed gas composed of oxygen and an inert gas into the reaction chamber through a new gas valve pipe; Among them, the injection is carried out according to an oxygen amount of 0.05 - 0.15 moles per ton of titanium ingots, and when injecting the mixed gas, a mixed gas containing 0.07 moles of oxygen per ton of titanium ingots is introduced. The inert gas in the mixed gas is argon or helium, and the mixing ratio of oxygen to the inert gas is 1:3 - 5; When injecting oxygen or a mixed gas, the gas is introduced into the gap between the furnace lid and the inner wall of the furnace body; Step 4: After the reaction chamber cools down to room temperature, open the furnace lid and take out the titanium ingot.
[0005] Furthermore, the method is applied to a reaction furnace, which includes a furnace body, and a furnace lid is arranged at the top of the furnace body, and a feeding pipe penetrates through the top of the furnace lid.
[0006] Furthermore, a gas valve pipe is arranged on one side of the feeding pipe, and a vacuum pipe and a magnesium chloride discharge pipe are sequentially arranged on the other side of the feeding pipe, and the number of the gas valve pipes is not one.
[0007] Furthermore, a reaction chamber is opened inside the furnace body.
[0008] The present invention provides a method for preventing the combustion, nitridation and impurity mixing of titanium ingots in the production of titanium sponge, and has the following beneficial effects: 1. In the method for preventing the combustion, nitridation and impurity mixing of titanium ingots in the production of titanium sponge, after the titanium sponge ingots generated by reduction are refined by vacuum separation, oxygen or a mixed gas composed of oxygen and an inert gas is injected into the reaction chamber to inactivate impurities, so that when the titanium ingots are taken out, there will be no situation of impurity ignition and combustion and nitride formation, and high-quality titanium sponge can be stably manufactured. Description of the Drawings
[0009] Figure 1 It is a schematic cross-sectional structure view of the furnace body of the present invention; Figure 2 It is a schematic external structure view of the furnace body of the present invention.
[0010] In the figure: 1, furnace body; 2, furnace lid; 3, feeding pipe; 4, gas valve pipe; 5, vacuum pipe; 6, magnesium chloride discharge pipe; 7, reaction chamber. Detailed Embodiments
[0011] The following further describes in detail the embodiments of the present invention in conjunction with the drawings. The following embodiments are used to illustrate the present invention, but cannot be used to limit the scope of the present invention.
[0012] As Figure 1 - Figure 2 shown, the present invention provides a technical solution: a method for preventing the combustion, nitridation and impurity mixing of titanium ingots in the production of titanium sponge, and the method includes the following steps: Step 1: Inject titanium tetrachloride into the reaction chamber 7 through the feeding pipe 3, and titanium tetrachloride reacts with the previously injected magnesium metal to generate titanium ingots and magnesium chloride; Step 2: Discharge magnesium chloride through the magnesium chloride discharge pipe 6. After the reduction reaction ends, a titanium ingot containing residual magnesium and magnesium chloride impurities is obtained in the reaction chamber 7. At this time, use the vacuum pipe 5 to evacuate the reaction chamber 7 to a vacuum and heat it, so that magnesium and magnesium chloride are vaporized and then discharged through the other gas valve pipe 4; Step 3: Before opening the furnace cover 2, inject oxygen or a mixed gas composed of oxygen and an inert gas into the reaction chamber 7 through the new gas valve pipe 4; Among them, the injection is carried out according to an oxygen amount of 0.05 - 0.15 moles per ton of titanium ingot, and when injecting the mixed gas, the mixed gas containing 0.07 moles of oxygen per ton of titanium ingot is introduced. The inert gas in the mixed gas is argon or helium, and the mixing ratio of oxygen to the inert gas is 1:3 - 5; And when injecting oxygen or the mixed gas, the gas is introduced into the gap between the furnace cover 2 and the inner wall of the furnace body 1; Step 4: After the reaction chamber 7 cools to room temperature, open the furnace cover 2 and take out the titanium ingot.
[0013] The method is applied to a reaction furnace. The reaction furnace includes a furnace body 1, and a furnace cover 2 is provided at the top of the furnace body 1. A feeding pipe 3 penetrates through the top of the furnace cover 2. A gas valve pipe 4 is provided on one side of the feeding pipe 3, and a vacuum pipe 5 and a magnesium chloride discharge pipe 6 are successively provided on the other side of the feeding pipe 3. The number of gas valve pipes 4 is not one, and a reaction chamber 7 is opened inside the furnace body 1; The specific operation is as follows. Inject metallic magnesium and titanium tetrachloride into the reaction chamber 7 through the feeding pipe 3 in sequence. Titanium tetrachloride reacts with metallic magnesium to generate a titanium ingot and magnesium chloride, and then discharge magnesium chloride through the magnesium chloride discharge pipe 6. After the reduction reaction ends, a titanium ingot containing residual magnesium and magnesium chloride impurities is obtained in the reaction chamber 7. At this time, use the vacuum pipe 5 to evacuate the reaction chamber 7 to a vacuum and heat it, so that magnesium and magnesium chloride are vaporized and then discharged through the other gas valve pipe 4, thereby purifying the titanium ingot; Inject oxygen or a mixed gas composed of oxygen and an inert gas into the reaction chamber 7 through the new gas valve pipe 4. Among them, the injection is carried out according to an oxygen amount of 0.05 - 0.15 moles per ton of titanium ingot, and when injecting the mixed gas, the mixed gas containing 0.07 moles of oxygen per ton of titanium ingot is introduced. The inert gas in the mixed gas is argon, helium, etc., and when injecting oxygen or the mixed gas, the gas is introduced into the gap between the furnace cover 2 and the inner wall of the furnace body 1; After the reaction chamber 7 cools to room temperature, open the furnace cover 2 and take out the titanium ingot; Based on the above description, after the sponge titanium ingot generated by reduction is refined by vacuum separation, oxygen or a mixed gas composed of oxygen and an inert gas is injected into the reaction chamber 7 to inactivate the impurities, so that when the titanium ingot is taken out, the situation of impurity ignition and combustion and the formation of nitrides will not occur, and high-quality sponge titanium can be stably manufactured. Example 1:
[0014] After replacing the inside of the reaction chamber 7 with argon, titanium tetrachloride is injected from the feed pipe 3 to react with the metallic magnesium in the reaction chamber 7, generating titanium ingots and magnesium chloride in the reaction chamber 7. Magnesium chloride is discharged from the system through the magnesium chloride discharge pipe 6 in a timely manner. After the reduction reaction ends, titanium ingots containing impurities such as residual magnesium and magnesium chloride are obtained in the reaction chamber 7; The residual magnesium and magnesium chloride contained in the titanium ingots are removed by vacuum separation. After filling the reaction chamber 7 with argon and cooling it to near room temperature, preparations are made to remove the titanium ingots from the reaction chamber 7. Before removing the furnace lid 2 from the reaction chamber 7, oxygen is introduced into the reaction chamber 7 through the gas valve pipe 4 in an amount of 0.10 moles per ton of titanium ingots produced; According to the above method, 10 batches of titanium sponge are manufactured. When removing the titanium ingots from the reaction chamber 7, no cases of ignition and combustion or nitride formation occur, and the nitrogen concentration of the adherents on the surface of the reaction chamber 7 and the titanium ingots is 0.001 - 0.006 wt.%. Example 2:
[0015] Except that a mixed gas of oxygen and an inert gas is introduced into the reaction chamber 7, and the amount of oxygen in the mixed gas is 0.07 moles per ton of titanium ingots produced, other operations are the same as in Example 1. After manufacturing 10 batches of titanium ingots, when removing the titanium ingots from the reaction chamber 7, no cases of ignition and combustion or nitride formation occur either, and the nitrogen concentration of the adherents is 0.001 - 0.007 wt.%.
[0016] Comparative example: Except that air is introduced into the reaction chamber 7, other operations are the same as in Example 2. After manufacturing 10 batches of titanium sponge, when removing the titanium ingots from the reaction chamber 7, the incidence of ignition and combustion is 25%, the incidence of nitride is 100%, and the nitrogen concentration of the adherents is 0.6 - 1.5 wt.%.
[0017] In summary, for the method of preventing the combustion, nitridation, and impurity mixing of titanium ingots in the production of this titanium sponge, during use, first, metallic magnesium and titanium tetrachloride are sequentially injected into the inside of the reaction chamber 7 through the feed pipe 3. Titanium tetrachloride reacts with metallic magnesium to generate titanium ingots and magnesium chloride, and then magnesium chloride is discharged through the magnesium chloride discharge pipe 6. After the reduction reaction ends, titanium ingots containing residual magnesium and magnesium chloride impurities are obtained in the reaction chamber 7. At this time, the inside of the reaction chamber 7 is evacuated to a vacuum and heated using the vacuum pipe 5, so that magnesium and magnesium chloride are vaporized and then discharged through other gas valve pipes 4, thereby purifying the titanium ingots; Oxygen or a mixed gas composed of oxygen and an inert gas is injected into the interior of the reaction chamber 7 through the new gas valve pipe 4, where the amount of oxygen injected is 0.05 - 0.15 moles per ton of titanium ingot, and when injecting the mixed gas, the mixed gas containing 0.07 moles of oxygen per ton of titanium ingot is injected, and the inert gas in the mixed gas is argon, helium, etc.; After the impurities are deactivated due to contact with oxygen or the mixed gas and the temperature drops to room temperature, the furnace lid 2 is opened and the titanium ingot is taken out.
[0018] The embodiments of the present invention are given for purposes of illustration and description, and are not exhaustive or limit the invention to the disclosed form. Many modifications and variations are obvious to those of ordinary skill in the art. The embodiments are chosen and described in order to better illustrate the principles of the invention and its practical application, and to enable those of ordinary skill in the art to understand the invention and design various embodiments with various modifications suitable for a particular purpose.
Claims
1. A method for preventing titanium ingot combustion, nitridation and impurity mixing during titanium sponge production, characterized in that: The method includes the following steps: Step 1: Inject titanium tetrachloride into the reaction chamber (7) through the feeding pipe (3). The titanium tetrachloride reacts with the previously injected metallic magnesium to generate titanium ingots and magnesium chloride. Step 2: Discharge the magnesium chloride through the magnesium chloride discharge pipe (6). After the reduction reaction ends, titanium ingots containing residual magnesium and magnesium chloride impurities are obtained in the reaction chamber (7). At this time, use the vacuum pipe (5) to evacuate the reaction chamber (7) to vacuum and heat it, so that the magnesium and magnesium chloride are vaporized and then discharged through the other gas valve pipe (4). Step 3: Before opening the furnace lid (2), inject oxygen or a mixed gas composed of oxygen and an inert gas into the reaction chamber (7) through the new gas valve pipe (4). Among them, the injection is carried out according to an oxygen amount of 0.05 - 0.15 moles per ton of titanium ingots. When injecting the mixed gas, the mixed gas containing 0.07 moles of oxygen per ton of titanium ingots is introduced. The inert gas in the mixed gas is argon or helium, and the mixing ratio of oxygen to the inert gas is 1:3 - 5. And when injecting oxygen or the mixed gas, the gas is introduced into the gap between the furnace lid (2) and the inner wall of the furnace body (1). Step 4: After the reaction chamber (7) cools to room temperature, open the furnace lid (2) and take out the titanium ingots.
2. A method for preventing the combustion, nitridation and impurity mixing of titanium ingots in titanium sponge production according to claim 1, characterized in that: The method is applied to a reaction furnace. The reaction furnace includes a furnace body (1), and a furnace lid (2) is provided at the top of the furnace body (1). The feeding pipe (3) penetrates through the top of the furnace lid (2).
3. A method for preventing the combustion, nitridation and impurity mixing of titanium ingots in titanium sponge production according to claim 2, characterized in that: One side of the feeding pipe (3) is provided with a gas valve pipe (4), and on the other side of the feeding pipe (3), a vacuum pipe (5) and a magnesium chloride discharge pipe (6) are sequentially arranged. The number of the gas valve pipes (4) is not one.
4. A method for preventing the combustion, nitridation and impurity mixing of titanium ingots in titanium sponge production according to claim 3, characterized in that: A reaction chamber (7) is opened inside the furnace body (1).