CN115094249B - Application method of reduction distillation heating furnace for reducing packaging density of titanium sponge - Google Patents
Application method of reduction distillation heating furnace for reducing packaging density of titanium sponge Download PDFInfo
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- CN115094249B CN115094249B CN202210816186.2A CN202210816186A CN115094249B CN 115094249 B CN115094249 B CN 115094249B CN 202210816186 A CN202210816186 A CN 202210816186A CN 115094249 B CN115094249 B CN 115094249B
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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
- C22B34/1263—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 metallic titanium from titanium compounds, e.g. by reduction
- C22B34/1268—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 metallic titanium from titanium compounds, e.g. by reduction using alkali or alkaline-earth metals or amalgams
- C22B34/1272—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 metallic titanium from titanium compounds, e.g. by reduction using alkali or alkaline-earth metals or amalgams reduction of titanium halides, e.g. Kroll process
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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
- C22B5/00—General methods of reducing to metals
- C22B5/02—Dry methods smelting of sulfides or formation of mattes
- C22B5/04—Dry methods smelting of sulfides or formation of mattes by aluminium, other metals or silicon
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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
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Abstract
The utility model relates to a reduction distillation heating furnace for reducing the packaging density of titanium sponge and a use method thereof. The reduction distillation heating furnace comprises a heating furnace body, a cooling furnace body, a vacuum system and a central temperature measuring tube; a closed hot end reactor is arranged in the heating furnace body, a closed cooling reactor is arranged in the cooling furnace body, and the hot end reactor is communicated with the cooling reactor; the hot end reactor is internally provided with a titanium sponge lump after reduction; the reading end of the central temperature measuring tube is arranged outside the furnace body, and the sensing end is arranged in the center of the titanium lump inside the furnace body. When the utility model is used, the heating and cooling time is prolonged, and the phase change time of the sponge titanium from the low-temperature alpha type to the high-temperature beta type or from the high-temperature beta type to the low-temperature alpha type is prolonged. Avoiding the occurrence of the phenomena of rapid expansion and contraction of the surface of the titanium sponge caused by rapid temperature rise or cooling. The packaging density of the titanium sponge produced by the heating furnace can meet the requirements of pressing titanium sponge ingots in downstream working procedures and casting the titanium ingots by adopting a vacuum consumable furnace.
Description
Technical Field
The utility model relates to the technical field of industrial kilns, in particular to a use method of a reduction distillation heating furnace for reducing the packaging density of titanium sponge.
Background
Titanium and titanium alloy have the characteristics of high strength, corrosion resistance and the like. Has important application in the fields of military industry, aerospace, deep sea detection, chemical medical treatment and the like. Titanium sponge is used as an important raw material for titanium alloy processing, and is mostly prepared by adopting a magnesia-thermal reduction method in industrial production, and along with the utility model of a U furnace-reversing steam furnace by adopting the magnesia-thermal reduction method, the production furnace type continuously develops towards the large-scale direction, and currently 5 tons, 6 tons, 7 tons, 8 tons, 10 tons, 12 tons, 15 tons and the like are known. The large furnace type production of the titanium sponge does have the advantages of reducing the cost, improving the labor intensity and the like, but the production of the titanium lump has the reasons of larger dead weight, heavy dead weight, imperfect process and the like. The packaging density of the sponge titanium produced in a large furnace type is larger, and the packaging density of the sponge titanium cannot meet the requirements of ingot pressing and vacuum consumable furnace casting of titanium ingots in subsequent processing. Domestic high-end titanium alloy processing manufacturers have long been very important in looking at this index. Although China is the largest production country of the sponge titanium worldwide, the country is not the strong production country of the sponge titanium, more foreign exchange import high-end sponge titanium is required to be spent every year to meet the demands of domestic high-end users.
Disclosure of Invention
The utility model aims to provide a use method of a reduction distillation heating furnace for reducing the packaging density of titanium sponge, which changes the technical defect that the process steps of the large-sized reduction distillation furnace for titanium sponge cannot be accurately controlled in the process of distillation heating and cooling, so that the produced product is rough and the requirement of the downstream working procedure in industrial production on the material precision cannot be met.
In order to achieve the above purpose, the technical scheme adopted by the utility model is as follows:
the application method of the reduction distillation heating furnace for reducing the packaging density of the titanium sponge comprises a heating furnace body, a cooling furnace body, a vacuum system and a central temperature measuring tube; the method is characterized in that: the heating furnace body is internally provided with a closed hot-end reactor, the cooling furnace body is internally provided with a closed cooling reactor, and the hot-end reactor is communicated with the cooling reactor through a passage pipe; the hot end reactor is internally provided with a titanium sponge lump after reduction; a ventilation system is arranged on the heating furnace body; the outlet end of the vacuum system is provided with a valve which is connected to a closed cooling reactor in the cooling furnace through a pipeline; the reading end of the central temperature measuring tube is arranged outside the closed heating furnace body, and the induction end is arranged in the center of the titanium lump inside the heating furnace body.
The ventilation system comprises an upper air outlet, a middle air outlet, an upper air inlet and a lower air inlet, wherein the upper air outlet and the middle air outlet are respectively arranged at the upper part and the middle part of the heating furnace body, and a blind plate is arranged at the joint of the upper air outlet and the middle air outlet and the heating furnace body; the upper air inlet and the lower air inlet are arranged at the lower part of the heating furnace body, and a valve is arranged at the joint of the upper air inlet and the lower air inlet and the heating furnace body.
The upper part of the hot end reactor is provided with a sealing cover, the upper part of the cooling reactor is provided with a sealing cover, and the sealing cover is provided with through holes corresponding to different pipelines and devices; the aisle tube is provided with an aisle tube heater.
The bottoms of the hot end reactor and the cooling reactor are provided with a sieve plate.
The application method of the reduction distillation heating furnace for reducing the packaging density of the titanium sponge is characterized by comprising the following steps of:
s1, closing blind plates and valves of all air inlets and outlets of a reduction distillation heating furnace;
step S2: the signal source of the central temperature measuring tube is communicated;
step S3: and (5) transmitting power to the heating furnace and controlling the temperature rise.
Step S4, keeping constant temperature at a high temperature state of 845-855 ℃, starting a vacuum system, and vacuumizing the inside and the outside of the hot-end reactor;
step S5, finishing constant temperature after keeping constant temperature for 2.5 to 3.5 hours, and further heating for multiple times to keep constant temperature until distillation is finished;
s6, turning off a power supply of the heating furnace, naturally cooling the heating furnace, and continuously vacuumizing the inside and the outside of the hot-end reactor;
step S7: when the temperature is reduced to 860-890 ℃, stopping vacuumizing the inside and outside of the hot end reactor, and filling argon into the hot end reactor for protection;
step S8: opening the blind plates of the upper air inlet, the lower air inlet, the upper air outlet and the middle air outlet for cooling, and adjusting the opening and closing degree of the blind plates to control the temperature falling speed;
step S9: when the temperature is reduced to below 850 ℃, discharging the furnace.
Step S4: maintaining constant temperature when power transmission is heated to 850 ℃;
the step S5 is as follows: keeping the temperature at 850 ℃ for 3 hours, continuously heating, and controlling the temperature to be 5 ℃ from 850 ℃ to 900 ℃ every hour, and keeping the temperature at 900 ℃ for 2 hours; heating to 10 ℃ from 900 ℃ to 1000 ℃ in each hour; keeping the temperature at 1000 ℃ until the distillation is finished;
step S7: stopping evacuating the inside and outside of the reactor after the temperature of the heating furnace is reduced to 880 ℃;
step S8: adjusting the opening of the blind plate to ensure that the temperature reduction speed of the heating furnace is less than or equal to 20 ℃/hour;
step S9: and when the temperature is lower than 800 ℃, discharging.
The reading end of the central temperature measuring tube of the reduction distillation heating furnace is arranged outside the furnace body of the heating furnace, so that the reaction process is convenient to control at any time, the temperature rising rhythm of the large-scale sponge titanium distillation heating furnace in the distillation temperature rising process and the temperature falling rhythm after the distillation process are finished are controllable, and the time for rising and falling the temperature is prolonged when the utility model is used, so that the phase change time of the sponge titanium from the low-temperature alpha type to the high-temperature beta type or from the high-temperature beta type to the low-temperature alpha type is prolonged. Thus, the phenomenon of rapid expansion and shrinkage of the surface of the titanium sponge caused by rapid temperature rise or cooling is avoided, and the packaging density of the titanium sponge produced by adopting the reduction distillation heating furnace and the application method thereof can meet the requirements of pressing titanium sponge ingots in downstream processes and melting and casting titanium ingots by adopting a vacuum consumable furnace.
Drawings
Fig. 1 is a schematic structural view of the present utility model.
Wherein: 1-a vacuum system; 2-valve; 3-a pipeline; 4-cooling the furnace body; 5-cooling the reactor;
distilling the condensate; 7-aisle tubes; 8-aisle tube heaters; 9-a central temperature measuring tube;
titanium lump; 11-hot end reactor; 12-heating the furnace body; 13-an upper air outlet;
a middle air outlet; 15-sieve plates; 16-an upper air inlet; 17-a lower air inlet.
Description of the embodiments
The following description of the embodiments of the present utility model will be made more fully hereinafter with reference to the accompanying drawings, in which it is evident that the embodiments described are only some, but not all embodiments of the utility model. All other embodiments, which can be made by those skilled in the art based on the embodiments of the utility model without making any inventive effort, are intended to be within the scope of the utility model.
As shown in FIG. 1, the reduction distillation heating furnace for reducing the packaging density of the titanium sponge comprises a heating furnace body 12, a cooling furnace body 4, a vacuum system 1 and a central temperature measuring tube 9; a closed hot end reactor 11 is arranged in the heating furnace body, a closed cooling reactor 5 is arranged in the cooling furnace body, and the hot end reactor is communicated with the cooling reactor through a passage pipe 7; the hot end reactor is internally provided with a reduced titanium sponge lump 10, and the cooling reactor is internally provided with a distillation condensate 6; the upper air outlet 13 and the middle air outlet 14 are respectively arranged on the heating furnace body 12 and in the middle, and blind plates are arranged at the joints of the upper air outlet 13 and the middle air outlet 14 and the heating furnace body 12; the lower part of the heating furnace body is provided with an upper air inlet 16 and a lower air inlet 17, and the joint of the upper air inlet 16 and the lower air inlet 17 and the heating furnace body 12 is provided with a valve. The outlet end of the vacuum system 1 is provided with a valve 2, and the valve 2 is connected to a closed cooling reactor in the cooling furnace through a pipeline 3. The reading end of the central temperature measuring tube is arranged outside the closed heating furnace body, and the induction end is arranged in the center of the titanium lump inside the heating furnace body. The upper part of the hot end reactor is provided with a sealing cover, the upper part of the cooling reactor is provided with a sealing cover, and the sealing cover is provided with through holes corresponding to different pipelines and devices. The aisle tube 7 is externally provided with an aisle tube heater 8. The bottom of the hot end reactor and the bottom of the cooling reactor are provided with a sieve plate 15.
Example 1. When the utility model is actually used, the temperature rising process is firstly carried out, S1, the blind plates and the valves of all air inlets and outlets of the reduction distillation heating furnace are closed, S2: the signal source of the central temperature measuring tube is communicated; s3: and (5) transmitting power to the heating furnace and controlling the temperature rise. And S4, maintaining constant temperature when power is transmitted and the temperature is raised to 850 ℃, starting a vacuum system, and vacuumizing the inside and the outside of the hot-end reactor.
Then carrying out distillation reaction S5, keeping the constant temperature of 850 ℃ for 3 hours, continuing to heat, and controlling the temperature to rise by 5 ℃ from 850 ℃ to 900 ℃ every hour, and keeping the constant temperature of 900 ℃ for 2 hours; heating to 10 ℃ from 900 ℃ to 1000 ℃ in each hour; constant temperature at 1000 ℃ until distillation is finished.
Finally, cooling, namely turning off a power supply of the heating furnace to naturally cool the heating furnace, and continuously vacuumizing the inside and the outside of the hot-end reactor; s7: when the temperature of the heating furnace is reduced to 880 ℃, stopping evacuating the inside and the outside of the reactor, and filling argon into the hot-end reactor for protection; s8: opening the blind plates of the upper air inlet, the lower air inlet, the upper air outlet and the middle air outlet for cooling, and adjusting the opening and closing degree of the blind plates to control the temperature falling speed so that the temperature falling speed of the heating furnace is less than or equal to 5 ℃/h; s9: when the temperature is reduced to 800 ℃, discharging the furnace.
Step S4, keeping constant temperature at 845 ℃, starting a vacuum system, and vacuumizing the inside and the outside of the hot-end reactor; s5, finishing constant temperature after keeping constant temperature for 2.5 hours, and further heating for multiple times to keep constant temperature until distillation is finished; step S7: when the temperature is reduced to 860 ℃, stopping vacuumizing the inside and outside of the hot-end reactor, and filling argon into the hot-end reactor for protection; step S9: when the temperature is reduced to 850 ℃, discharging the furnace. The other steps are the same as in example 1.
Step S4, keeping constant temperature at 855 ℃, starting a vacuum system, and vacuumizing the inside and the outside of the hot-end reactor; s5, finishing constant temperature after keeping constant temperature for 3.5 hours, and further heating for multiple times to keep constant temperature until distillation is finished; step S7: when the temperature is reduced to 890 ℃, stopping vacuumizing the inside and outside of the hot end reactor, and filling argon into the hot end reactor for protection; step S9: and when the temperature is reduced to 820 ℃, discharging. The other steps are the same as in example 1.
The utility model is based on theory: the transition temperature of two allotropic forms of titanium is 882.5 ℃, and when the titanium contains oxygen, nitrogen, carbon and other impurities, the temperature of the titanium is correspondingly increased. And the volume increase upon conversion from α -Ti to β -Ti was 5.5%. The reaction temperature is controlled, so that the phase change time of the sponge titanium from low-temperature alpha type to high-temperature beta type or from high-temperature beta type to low-temperature alpha type is prolonged, the phenomenon of rapid expansion and contraction of the surface of the sponge titanium caused by rapid heating or cooling can be avoided, the packaging density of the sponge titanium is reduced, and the requirements of ingot pressing and vacuum consumable furnace casting of the titanium ingot in subsequent processing are met.
According to the utility model, the ventilation system device is added on the heating furnace of the steaming furnace, so that the aim of controlling the controllable cooling of the steaming furnace is fulfilled; through increasing titanium lump center temperature measuring device, can effectively measure the center temperature that titanium lump, because the titanium sponge thermal conductivity performance is relatively poor, its titanium lump surface temperature and the temperature in center have great difference in temperature. Therefore, the temperature of the whole titanium lump can be objectively reflected by using the center temperature as the control temperature. The utility model controls the temperature rise and fall mode by a special way: the temperature is controlled to rise by 5 ℃ from 850 ℃ to 900 ℃ per hour, and the temperature is controlled to rise by 10 ℃ per hour from 900 ℃ to 1000 ℃. When the temperature is reduced, a vacuum cooling mode is adopted, the temperature reduction of 10-20 ℃ per hour is controlled in a section of 1000-880 ℃ under the state of continuously evacuating the reactor, the temperature reduction of less than or equal to 5 ℃ per hour is controlled in a section of 880-850 ℃, the vacuum system is closed after the temperature is lower than 880 ℃, and meanwhile argon is filled into the reactor for protection.
The ventilation system arranged on the heating furnace can be used for adjusting the air inlet quantity, so that the temperature requirements of the heating furnace in different periods can be effectively controlled. The upper sealing cover of the hot-end reactor is provided with a central temperature measuring tube for measuring the temperature of the center of the titanium lump. In the using process, a unique heating and cooling control mode is adopted: when heating, the temperature is controlled to rise by 5 ℃ from 850 ℃ to 900 ℃ in each hour, and the temperature is controlled to rise by 10 ℃ from 900 ℃ to 1000 ℃ in each hour; when the temperature is reduced, the temperature is reduced by 10-20 ℃ per hour in the section of 1000-880 ℃ under the state of continuously evacuating the reactor, the temperature is reduced by less than or equal to 5 ℃ per hour in the section of 880-850 ℃, the vacuum system is closed after the temperature is lower than 880 ℃, argon is filled into the reactor for protection, the opening of a blind plate is regulated, and the tapping work can be carried out below 850 ℃.
Although embodiments of the present utility model have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the utility model, the scope of which is defined in the appended claims and their equivalents.
Claims (2)
1. The application method of the reduction distillation heating furnace for reducing the packaging density of the titanium sponge comprises a heating furnace body, a cooling furnace body, a vacuum system and a central temperature measuring tube; the method is characterized in that: the heating furnace body is internally provided with a closed hot-end reactor, the cooling furnace body is internally provided with a closed cooling reactor, and the hot-end reactor is communicated with the cooling reactor through a passage pipe; the hot end reactor is internally provided with a titanium sponge lump after reduction; a ventilation system is arranged on the heating furnace body; the outlet end of the vacuum system is provided with a valve which is connected to a closed cooling reactor in the cooling furnace through a pipeline; the reading end of the central temperature measuring tube is arranged outside the closed heating furnace body, and the induction end is arranged in the center of the titanium lump inside the heating furnace body;
the ventilation system comprises an upper air outlet, a middle air outlet, an upper air inlet and a lower air inlet, wherein the upper air outlet and the middle air outlet are respectively arranged at the upper part and the middle part of the heating furnace body, and a blind plate is arranged at the joint of the upper air outlet and the middle air outlet and the heating furnace body; the upper air inlet and the lower air inlet are arranged at the lower part of the heating furnace body, and a valve is arranged at the joint of the upper air inlet and the heating furnace body;
the upper part of the hot end reactor is provided with a sealing cover, the upper part of the cooling reactor is provided with a sealing cover, the sealing cover is provided with through holes corresponding to different pipelines and devices, and the aisle tube is externally provided with an aisle tube heater;
the bottoms of the hot end reactor and the cooling reactor are provided with a sieve plate;
the using method of the reduction distillation heating furnace comprises the following steps:
s1, closing blind plates and valves of all air inlets and outlets of a reduction distillation heating furnace;
step S2: the signal source of the central temperature measuring tube is communicated;
step S3: feeding power to the heating furnace and controlling the temperature rise;
step S4, keeping constant temperature at a high temperature state of 845-855 ℃, starting a vacuum system, and vacuumizing the inside and the outside of the hot-end reactor;
step S5, finishing constant temperature after keeping constant temperature for 2.5 to 3.5 hours, and further heating for multiple times to keep constant temperature until distillation is finished;
s6, turning off a power supply of the heating furnace, naturally cooling the heating furnace, and continuously vacuumizing the inside and the outside of the hot-end reactor;
step S7: when the temperature is reduced to 860-890 ℃, stopping vacuumizing the inside and outside of the hot end reactor, and filling argon into the hot end reactor for protection;
step S8: opening the blind plates of the upper air inlet, the lower air inlet, the upper air outlet and the middle air outlet for cooling, and adjusting the opening and closing degree of the blind plates to control the temperature falling speed;
step S9: when the temperature is reduced to below 850 ℃, discharging the furnace.
2. The method for using a reducing distillation heating furnace according to claim 1, wherein:
step S4: maintaining constant temperature when power transmission is heated to 850 ℃;
the step S5 is as follows: keeping the temperature at 850 ℃ for 3 hours, continuously heating, and controlling the temperature to be 5 ℃ from 850 ℃ to 900 ℃ every hour, and keeping the temperature at 900 ℃ for 2 hours; heating to 10deg.C from 900-1000deg.C per hour, and keeping constant temperature at 1000deg.C until distillation is completed;
step S7: stopping evacuating the inside and outside of the reactor after the temperature of the heating furnace is reduced to 880 ℃;
step S8: adjusting the opening of the blind plate to ensure that the temperature reduction speed of the heating furnace is less than or equal to 20 ℃/hour;
step S9: and when the temperature is lower than 800 ℃, discharging.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210816186.2A CN115094249B (en) | 2022-07-12 | 2022-07-12 | Application method of reduction distillation heating furnace for reducing packaging density of titanium sponge |
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| CN202210816186.2A CN115094249B (en) | 2022-07-12 | 2022-07-12 | Application method of reduction distillation heating furnace for reducing packaging density of titanium sponge |
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| CN115821069B (en) * | 2022-12-07 | 2023-06-16 | 云南国钛金属股份有限公司 | Temperature control method for rotor-grade titanium sponge inverted U-shaped distillation process |
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