CN112030009A - Device and method for producing titanium sponge with low nitrogen and oxygen impurity content and low Brinell hardness - Google Patents
Device and method for producing titanium sponge with low nitrogen and oxygen impurity content and low Brinell hardness Download PDFInfo
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- CN112030009A CN112030009A CN202010894751.8A CN202010894751A CN112030009A CN 112030009 A CN112030009 A CN 112030009A CN 202010894751 A CN202010894751 A CN 202010894751A CN 112030009 A CN112030009 A CN 112030009A
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
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- 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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- 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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- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
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Abstract
The invention belongs to the technical field of titanium sponge production, and particularly discloses a device for producing low-nitrogen-oxygen-impurity-content and low-Brinell-hardness titanium sponge and a method for producing low-nitrogen-oxygen-impurity-content and low-Brinell-hardness titanium sponge, wherein the device can effectively control the pressure in a reaction container after being implanted into a corresponding existing control program. After this a device for producing low nitrogen oxygen impurity content low brinell hardness titanium sponge is implanted corresponding current control procedure, when the reduction process of production titanium sponge, but feed back to the controller through pressure detector real-time detection reaction intracavity pressure, the controller is inflated to the reaction intracavity according to reaction intracavity pressure control air inlet valve again, perhaps control pressure release valve is opened and is carried out the pressure release, with the pressure in the effective control reaction vessel, ensure going on smoothly of reduction process, and can avoid the titanium sponge in the air pollution reaction vessel, thereby can produce low nitrogen oxygen impurity content, the titanium sponge of low brinell hardness.
Description
Technical Field
The invention belongs to the technical field of titanium sponge production, and particularly relates to a device and a method for producing titanium sponge with low nitrogen and oxygen impurity content and low Brinell hardness.
Background
The titanium sponge is used as an important raw material for preparing titanium and titanium alloy, and the nitrogen-oxygen impurity content and the Brinell hardness of the titanium sponge have obvious influence on the processing yield and the final service performance of titanium and titanium alloy parts. In order to avoid adverse effects of nitrogen-oxygen impurities in the titanium sponge on the application performance of titanium and titanium alloy materials, titanium material processing enterprises prefer to select low-nitrogen, low-oxygen and low-Brinell hardness titanium sponge as a raw material.
Currently, the magnesium thermal method is used industrially to prepare titanium sponge. Researches on nitrogen and oxygen impurity sources and control measures in the titanium sponge show that the air tightness and process pressure conditions of the reduction distillation furnace serving as a reaction container have direct influence on the nitrogen and oxygen impurities in the titanium sponge. In the reduction process, the positive pressure of the reaction vessel should be ensured all the time to avoid air pollution to the titanium sponge in the reaction vessel. The reaction vessel has good air tightness so as to prevent air from entering the condensing tank to pollute the titanium sponge in the vacuum distillation process; at the end of the distillation, the condensation tank should be filled with argon rapidly to avoid air inflow. In addition, under the condition that the air tightness of the condensing tanks is the same, the vacuum distillation period is shortened, so that the air inflow is favorably reduced, and the nitrogen and oxygen content of the titanium sponge is favorably reduced.
However, in the existing titanium sponge production equipment, the air tightness of the reaction container is general, the pressure control in the reaction container is not good, the produced titanium sponge often has the problems of high nitrogen and oxygen content, high Brinell hardness and the like, and the problems cannot meet the requirement of the national standard GB/T2524-2019 on 0ALow nitrogen oxygen impurity content of the grade low brookfield hardness titanium sponge nitrogen oxygen impurity content and brookfield hardness requirements.
Disclosure of Invention
The invention aims to provide a device for producing titanium sponge with low nitrogen and oxygen impurity content and low Brinell hardness, which can effectively control the pressure in a reaction container after being implanted into a corresponding existing control program.
The technical scheme adopted by the invention for solving the technical problems is as follows: the device for producing the sponge titanium with low nitrogen and oxygen impurity content and low Brinell hardness comprises a reaction container with a reaction cavity and a controller; the top of the reaction container is provided with a reaction container cover, the reaction container cover is provided with a pressure detection port, an air inlet and a pressure relief port which are respectively communicated with the reaction cavity, the pressure detection port is provided with a pressure detector, the air inlet is provided with an air inlet valve and is connected with an air source through the air inlet valve, and the pressure relief port is provided with a pressure relief valve; the pressure detector, the air inlet valve and the pressure relief valve are respectively electrically connected with the controller.
Furthermore, a magnesium chloride discharge structure is arranged at the bottom of the reaction container and comprises a magnesium chloride discharge port arranged at the bottom of the reaction container and a magnesium chloride discharge valve connected with the magnesium chloride discharge port through a flange, and the magnesium chloride discharge valve is a valve with a thimble.
Further, a titanium tetrachloride adding port communicated with the reaction cavity is arranged on the reaction container cover, and a titanium tetrachloride adding pipe is arranged at the titanium tetrachloride adding port.
Further, the device also comprises a condensation tank; the reaction container cover is of an upper-lower double-flange structure and comprises an upper flange and a lower flange, the reaction container cover is connected with a bottom flange of the condensation tank in a sealing mode through the upper flange, and the reaction container cover is connected with a top flange of the reaction container in a sealing mode through the lower flange.
Further, a first cooling channel is arranged in a bottom flange of the condensing tank, and a second cooling channel is arranged in a top flange of the reaction vessel; and sealing rings are arranged between a bottom flange and an upper flange of the condensing tank and between a lower flange and a top flange of the reaction vessel.
Further, a cooling spraying device is arranged at the top of the condensing tank, and a spray water collecting jacket is sleeved outside the condensing tank; the top of the condensing tank is also provided with a vacuum pipeline communicated with the inner cavity of the condensing tank, and a vacuum pump is arranged on the vacuum pipeline; a first vacuum detection port is arranged on a pipeline section of the vacuum pipeline between the vacuum pump and the condensation tank, and a second vacuum detection port communicated with an inner cavity of the condensation tank is arranged on the reaction container cover.
Further, a heat insulating member is provided between the reaction vessel and the condensation tank, and the heat insulating member is located above the titanium tetrachloride inlet.
The invention also provides a method for producing the sponge titanium with low nitrogen and oxygen impurity content and low Brinell hardness, which adopts the device for producing the sponge titanium with low nitrogen and oxygen impurity content and low Brinell hardness to produce the sponge titanium.
Further, the method for producing the titanium sponge with low nitrogen and oxygen impurity content and low Brinell hardness comprises a reduction step;
a reduction step: the method comprises the following steps of loading raw materials into a reaction cavity for reduction, simultaneously monitoring the pressure in the reaction cavity in real time through a pressure detector and feeding back to a controller, and when the pressure in the reaction cavity is lower than 5kPa, controlling an air inlet valve to be opened by the controller to fill argon into the reaction cavity until the pressure in the reaction cavity is higher than 5 kPa; when the pressure in the reaction cavity is higher than 30kPa, the controller controls the pressure relief valve to open for pressure relief until the pressure in the reaction cavity is lower than 30 kPa.
Further, the method for producing the titanium sponge with low nitrogen and oxygen impurity content and low Brinell hardness further comprises discharging Mg and MgCl2A step of (1), a distillation step and a product take-out step;
discharging Mg and MgCl2The steps of (1): after the reduction is finished, opening a magnesium chloride discharge valve to remove the residual liquid-phase Mg and MgCl in the reaction chamber2Discharging the reaction vessel, opening a magnesium chloride discharge valve, and simultaneously controlling an air inlet valve to open by a controller to fill argon into the reaction cavity so that the pressure in the reaction cavity is higher than 30 kPa;
a distillation step: residual liquid phase Mg and MgCl2After the discharge is finished, when the pressure in the reaction cavity is more than 15kPa, the titanium tetrachloride feeding pipe is taken down, and meanwhile, the controller controls the air inlet valve to be opened to fill argon into the reaction cavity, so that the pressure in the reaction cavity is higher than 15 kPa; then, a condensation tank is arranged on the reaction container, and a heat insulation component is arranged between the condensation tank and the reaction container; finally, closing a vacuum pipeline on the condensing tank, and then carrying out positive pressure leak detection on the reaction container to ensure that no leak point exists; in the distillation processControlling the distillation temperature in the reaction container to be 900-1020 ℃, then opening a cooling spray device to spray CaCl with the temperature of-20-0 ℃ and the concentration of 20-35 wt%2Liquid and ensure CaCl2The temperature of the liquid at the liquid outlet of the spray water collecting jacket is less than or equal to 40 ℃ until the distillation is finished;
a product taking-out step: after distillation is finished, stopping power transmission, closing the vacuum pipeline, closing the cooling spray device, respectively filling argon from the first vacuum detection port and the second vacuum detection port, and stopping argon filling when the pressure in the reaction cavity reaches 15 kPa; and after the temperature of the outer wall of the reaction container is lower than 50 ℃, removing the condensing tank and the heat insulation component, then taking down the cover of the reaction container, and taking out the prepared titanium sponge product from the reaction cavity.
The invention has the beneficial effects that: after this a device for producing low nitrogen oxygen impurity content low brinell hardness titanium sponge is implanted corresponding current control procedure, when the reduction process of production titanium sponge, but feed back to the controller through pressure detector real-time detection reaction intracavity pressure, the controller is inflated to the reaction intracavity according to reaction intracavity pressure control air inlet valve again, perhaps control pressure release valve is opened and is carried out the pressure release, with the pressure in the effective control reaction vessel, ensure going on smoothly of reduction process, and can avoid the titanium sponge in the air pollution reaction vessel, thereby can produce low nitrogen oxygen impurity content, the titanium sponge of low brinell hardness.
Drawings
FIG. 1 is a schematic diagram of the structure of one embodiment of the apparatus for producing titanium sponge with low nitrogen and oxygen impurity content and low Brinell hardness in accordance with the present invention;
FIG. 2 is an enlarged view of a portion of FIG. 1 at A;
FIG. 3 is a schematic structural diagram of another embodiment of the apparatus for producing titanium sponge having low nitrogen and oxygen impurity content and low Brinell hardness in accordance with the present invention;
FIG. 4 is an enlarged view of a portion of FIG. 3 at B;
labeled as: the reaction vessel 100, the second cooling channel 101, the reaction chamber 110, the raw material support plate 111, the reaction vessel cover 120, the pressure detector 121, the air inlet valve 122, the pressure relief valve 123, the titanium tetrachloride inlet 124, the titanium tetrachloride inlet tube 125, the upper flange 126, the lower flange 127, the second vacuum detection port 128, the magnesium chloride discharge structure 130, the magnesium chloride discharge port 131, the magnesium chloride discharge valve 132, the thimble 133, the condensation tank 200, the first cooling channel 201, the cooling shower device 210, the shower water collection jacket 211, the vacuum pipe 220, the first vacuum detection port 221, the vacuum pump 230, the sealing ring 300, and the heat insulation member 400.
Detailed Description
The invention will be further described with reference to the accompanying drawings.
Referring to fig. 1 and 2, the apparatus for producing titanium sponge with low nitrogen-oxygen impurity content and low brinell hardness comprises a reaction vessel 100 having a reaction chamber 110, and a controller; a reaction container cover 120 is arranged at the top of the reaction container 100, a pressure detection port, an air inlet and a pressure relief port which are respectively communicated with the reaction cavity 110 are arranged on the reaction container cover 120, a pressure detector 121 is arranged at the pressure detection port, an air inlet valve 122 is arranged at the air inlet and is connected with an air source through the air inlet valve 122, and a pressure relief valve 123 is arranged at the pressure relief port; the pressure detector 121, the intake valve 122 and the pressure relief valve 123 are respectively electrically connected to the controller.
After the device for producing the titanium sponge with low nitrogen-oxygen impurity content and low Brinell hardness is implanted into a corresponding existing control program, in the reduction stage of producing the titanium sponge, the pressure in the reaction cavity 110 can be detected in real time through the pressure detector 121 and fed back to the controller, if the pressure in the reaction cavity 110 does not meet the requirement, the controller can control the air inlet valve 122 to inflate the reaction cavity 110 according to the pressure in the reaction cavity 110, or control the pressure relief valve 123 to open for pressure relief, so that the pressure in the reaction cavity 110 is regulated to meet the reduction requirement, the smooth operation of the reduction process is ensured, and the titanium sponge in the reaction container 100 can be prevented from being polluted by air. The reduction stage generally requires maintaining the pressure in the reaction chamber 110 at 5 to 30 kPa.
Wherein the reaction vessel 100 is one of the main components of the apparatus, which has a distillation function, preferably a reduction distillation furnace; a raw material support plate 111 is generally disposed in the reaction chamber 110 of the reaction vessel 100. The pressure detector 121 may be various, for example: pressure sensors, pressure gauges, etc.; both the intake valve 122 and the pressure relief valve 123 are electrically actuated valves.
Specifically, the reaction container cover 120 is provided with a titanium tetrachloride inlet 124 communicated with the reaction chamber 110, and a titanium tetrachloride inlet tube 125 is arranged at the titanium tetrachloride inlet 124.
In order to facilitate the removal of liquid-phase Mg and MgCl remaining after the reaction2To shorten the production cycle, as shown in fig. 1, a magnesium chloride discharge structure 130 is disposed at the bottom of the reaction vessel 100, the magnesium chloride discharge structure 130 includes a magnesium chloride discharge port 131 disposed at the bottom of the reaction vessel 110 and a magnesium chloride discharge valve 132 flanged with the magnesium chloride discharge port 131, and the magnesium chloride discharge valve 132 is a valve with a thimble 133. The magnesium chloride discharge port 131 and the magnesium chloride discharge valve 132 are connected by welding, and the magnesium chloride discharge valve 132 is opened by moving a needle 133 of the magnesium chloride discharge valve 132 downward to realize the remaining liquid-phase Mg and MgCl2And (4) discharging.
As a preferred embodiment of the present invention, as shown in fig. 3 and 4, the apparatus for producing titanium sponge with low nitrogen and oxygen impurity content and low brinell hardness further comprises a condensing tank 200; the reaction vessel cover 120 has an upper and lower double flange structure, and includes an upper flange 126 and a lower flange 127, the reaction vessel cover 120 is hermetically connected to the bottom flange of the condensation tank 200 via the upper flange 126, and the reaction vessel cover 120 is hermetically connected to the top flange of the reaction vessel 100 via the lower flange 127. The device is used in the distillation stage for producing the titanium sponge.
In order to improve the sealing effect, as shown in fig. 4 again, a first cooling channel 201 is provided in the bottom flange of the condensation tank 200, and a second cooling channel 101 is provided in the top flange of the reaction vessel 100; sealing rings 300 are disposed between the bottom flange of the condensation tank 200 and the upper flange 126, and between the lower flange 127 and the top flange of the reaction vessel 100. The gasket 300 may be of various types, preferably a nitrile rubber type gasket.
Specifically, a cooling spray device 210 is arranged at the top of the condensation tank 200, and a spray water collecting jacket 211 is sleeved outside the condensation tank 200; the top of the condensation tank 210 is also provided with a vacuum pipeline 220 communicated with the inner cavity of the condensation tank, and a vacuum pump 230 is arranged on the vacuum pipeline 220; a first vacuum detection port 221 is formed on a pipe section of the vacuum pipe 220 between the vacuum pump 230 and the condensation tank 200, and a second vacuum detection port 128 communicated with an inner cavity of the condensation tank 200 is formed on the reaction container cover 120. The lower end of the shower water collecting jacket 211 is typically sealingly connected to a bottom flange of the condensate tank 200.
In order to prevent the titanium tetrachloride inlet 124 from being clogged, as shown in fig. 3, a heat insulating member 400 is provided between the reaction container 100 and the condensation tank 200, and the heat insulating member 400 is located above the titanium tetrachloride inlet 124. The heat insulating member 400 is mainly made of a material having a low heat conductive capability, and a tapered through hole is generally formed in the middle thereof.
The invention also provides a method for producing the sponge titanium with low nitrogen and oxygen impurity content and low Brinell hardness, which adopts the device for producing the sponge titanium with low nitrogen and oxygen impurity content and low Brinell hardness to produce the sponge titanium. During production, in the reduction process, the pressure in the reaction cavity 110 can be controlled in real time, and the nitrogen and oxygen content of the titanium sponge is prevented from increasing due to the fact that air flows into the reaction container 100; after the reduction is completed, the liquid-phase Mg and MgCl remained at the bottom of the reaction chamber 110 can be discharged through the magnesium chloride discharge structure 1302The Mg and the MgCl are ensured to be discharged completely as much as possible2The distillation stage is high-efficiency distillation, so that the distillation period is favorably shortened; by providing the heat insulating member 400, the titanium tetrachloride introduction port 124 can be prevented from being clogged; meanwhile, the cooling liquid is sprayed by the cooling spraying device 210 for cooling, so that the distillation period can be further shortened, and the nitrogen-oxygen impurity content of the titanium sponge can be reduced; the vacuum degree can be detected through the first vacuum detection port 221 and the second vacuum detection port 128, argon can be filled, and the reaction container 100 can be quickly filled with argon after distillation is finished, so that the increase of the nitrogen and oxygen impurity content of the titanium sponge caused by air inflow is avoided.
Specifically, the method for producing the titanium sponge with low nitrogen and oxygen impurity content and low Brinell hardness comprises a reduction step; the reduction step is to TiCl4Performing magnesium heatingReduction, before this, the reaction vessel 100 is generally assembled, the titanium tetrachloride inlet tube 125 is installed at the titanium tetrachloride inlet 124, and the connection is generally separated by a graphite gasket; the raw material support plate 111 is installed at the lower portion of the reaction chamber 110, and is generally fixed by welding; then the reaction vessel cover 120 is arranged at the top of the reaction vessel 100, and a sealing ring 300 is arranged between the reaction vessel cover 120 and the reaction vessel 100; finally, a magnesium chloride discharge valve 132 is connected to the magnesium chloride discharge port 131; after the assembly is finished, air tightness detection is required, specifically, positive pressure leak detection is carried out, and air tightness of assembly equipment is guaranteed; then, carrying out leakage test under the vacuum degree of 40Pa to ensure that the leakage is less than 0.2 Pa/min;
a reduction step: the raw materials are loaded into the reaction cavity 110 for reduction, meanwhile, the pressure in the reaction cavity 110 is monitored in real time through the pressure detector 121 and fed back to the controller, when the pressure in the reaction cavity 110 is lower than 5kPa, the controller controls the air inlet valve 122 to be opened to fill argon into the reaction cavity 100 until the pressure in the reaction cavity 110 is higher than 5 kPa; when the pressure in the reaction chamber 110 is higher than 30kPa, the controller controls the pressure relief valve 123 to open for pressure relief until the pressure in the reaction chamber 110 is lower than 30 kPa.
Specifically, the method for producing the titanium sponge with low nitrogen and oxygen impurity content and low Brinell hardness further comprises discharging Mg and MgCl2A step of (1), a distillation step and a product take-out step;
discharging Mg and MgCl2The steps of (1): after the reduction is finished, the magnesium chloride discharge valve 132 is opened to allow the residual liquid-phase Mg and MgCl in the reaction chamber 1102Discharging the reaction vessel 100, opening the magnesium chloride discharge valve 132, and simultaneously controlling the gas inlet valve 122 to open by the controller to fill argon gas into the reaction chamber 110, so that the pressure in the reaction chamber 110 is higher than 30 kPa;
a distillation step: residual liquid phase Mg and MgCl2After the discharge is finished, when the pressure in the reaction chamber 110 is more than 15kPa, taking down the titanium tetrachloride feeding pipe 125, and simultaneously controlling the air inlet valve 122 to open by the controller to fill argon into the reaction chamber 110, so that the pressure in the reaction chamber 110 is higher than 15 kPa; then, the condensation tank 200 is installed on the reaction vessel 100, and the condensation tank 200 and the reaction vessel 100 are installedA heat insulating member 400 is interposed; finally, the vacuum pipeline 220 on the condensation tank 200 is closed, and then positive pressure leak detection is carried out on the reaction container 100 to ensure that no leak point exists; in the distillation process, the distillation temperature in the reaction container 100 is controlled to be 900-1020 ℃, and then the cooling spray device 210 is opened to spray CaCl with the injection temperature of-20-0 ℃ and the concentration of 20-35 wt%2Liquid and ensure CaCl2The temperature of the liquid at the liquid outlet of the spray water collecting jacket 211 is less than or equal to 40 ℃ until the distillation is finished;
a product taking-out step: after distillation is finished, power transmission is stopped, the vacuum pipeline 220 is closed, the cooling spray device 210 is turned off, argon gas is respectively filled from the first vacuum detection port 221 and the second vacuum detection port 128, and the argon filling is stopped when the pressure in the reaction cavity 110 reaches 15 kPa; after the temperature of the outer wall of the reaction vessel 100 is lower than 50 ℃, the condensing tank 200 and the heat insulation member 400 are removed, the reaction vessel cover 120 is removed, and the prepared titanium sponge product is taken out of the reaction chamber 100.
Claims (10)
1. An apparatus for producing titanium sponge with low nitrogen-oxygen impurity content and low Brinell hardness, comprising a reaction vessel (100) having a reaction chamber (110), characterized in that: the device also comprises a controller; the top of the reaction container (100) is provided with a reaction container cover (120), the reaction container cover (120) is provided with a pressure detection port, an air inlet and a pressure relief port which are respectively communicated with the reaction cavity (110), the pressure detection port is provided with a pressure detector (121), the air inlet is provided with an air inlet valve (122) and is connected with an air source through the air inlet valve (122), and the pressure relief port is provided with a pressure relief valve (123); the pressure detector (121), the air inlet valve (122) and the pressure relief valve (123) are respectively electrically connected with the controller.
2. The apparatus for producing titanium sponge having low nitrogen-oxygen impurity content and low Brinell hardness as claimed in claim 1, wherein: the bottom of the reaction vessel (100) is provided with a magnesium chloride discharge structure (130), the magnesium chloride discharge structure (130) comprises a magnesium chloride discharge port (131) arranged at the bottom of the reaction vessel (110) and a magnesium chloride discharge valve (132) connected with the magnesium chloride discharge port (131) in a flange mode, and the magnesium chloride discharge valve (132) is a valve with a thimble (133).
3. The apparatus for producing titanium sponge with low nitrogen-oxygen impurity content and low Brinell hardness as claimed in claim 1 or 2, wherein: the reaction container cover (120) is provided with a titanium tetrachloride adding port (124) communicated with the reaction cavity (110), and a titanium tetrachloride adding pipe (125) is arranged at the titanium tetrachloride adding port (124).
4. The apparatus for producing titanium sponge having low nitrogen-oxygen impurity content and low Brinell hardness as claimed in claim 3, wherein: also comprises a condensation tank (200); the reaction container cover (120) is of an upper-lower double-flange structure and comprises an upper flange (126) and a lower flange (127), the reaction container cover (120) is connected with a bottom flange of the condensing tank (200) in a sealing mode through the upper flange (126), and the reaction container cover (120) is connected with a top flange of the reaction container (100) in a sealing mode through the lower flange (127).
5. The apparatus for producing titanium sponge having low nitrogen-oxygen impurity content and low Brinell hardness as claimed in claim 4, wherein: a first cooling channel (201) is arranged in a bottom flange of the condensing tank (200), and a second cooling channel (101) is arranged in a top flange of the reaction container (100); sealing rings (300) are arranged between a bottom flange and an upper flange (126) of the condensation tank (200) and between a lower flange (127) and a top flange of the reaction vessel (100).
6. The apparatus for producing titanium sponge having low nitrogen-oxygen impurity content and low Brinell hardness as claimed in claim 4, wherein: a cooling spray device (210) is arranged at the top of the condensation tank (200), and a spray water collecting jacket (211) is sleeved outside the condensation tank (200); the top of the condensation tank (210) is also provided with a vacuum pipeline (220) communicated with the inner cavity of the condensation tank, and a vacuum pump (230) is arranged on the vacuum pipeline (220); a first vacuum detection port (221) is formed in a pipeline section of the vacuum pipeline (220) between the vacuum pump (230) and the condensation tank (200), and a second vacuum detection port (128) communicated with an inner cavity of the condensation tank (200) is formed in the reaction container cover (120).
7. The apparatus for producing titanium sponge having low nitrogen-oxygen impurity content and low Brinell hardness as claimed in claim 4, wherein: a heat insulation part (400) is arranged between the reaction container (100) and the condensing tank (200), and the heat insulation part (400) is positioned on the upper side of the titanium tetrachloride adding opening (124).
8. The method for producing the sponge titanium with low nitrogen and oxygen impurity content and low Brinell hardness is characterized by comprising the following steps: use of the apparatus for the production of titanium sponge with low nitrogen-oxygen impurity content and low Brinell hardness as claimed in any one of claims 1 to 7 for the production of titanium sponge.
9. The process for producing titanium sponge having low nitrogen oxygen impurity content and low brinell hardness as claimed in claim 8 wherein: comprises a reduction step;
a reduction step: the method comprises the steps of loading raw materials into a reaction cavity (110) for reduction, simultaneously monitoring the pressure in the reaction cavity (110) in real time through a pressure detector (121) and feeding back the pressure to a controller, and when the pressure in the reaction cavity (110) is lower than 5kPa, controlling an air inlet valve (122) to be opened by the controller to fill argon into the reaction cavity (100) until the pressure in the reaction cavity (110) is higher than 5 kPa; when the pressure in the reaction chamber (110) is higher than 30kPa, the controller controls the pressure relief valve (123) to open for pressure relief until the pressure in the reaction chamber (110) is lower than 30 kPa.
10. The process for producing titanium sponge having low nitrogen oxygen impurity content and low brinell hardness as claimed in claim 9 wherein: also includes discharging Mg and MgCl2A step of (1), a distillation step and a product take-out step;
discharging Mg and MgCl2The steps of (1): after the reduction is finished, opening a magnesium chloride discharge valve (132) to remove the liquid-phase Mg and MgCl remained in the reaction chamber (110)2Discharging the reaction vessel (100), opening the magnesium chloride discharge valve (132), and simultaneously controlling the gas inlet valve (122) to open to fill argon gas into the reaction chamber (110) by the controller, so that the pressure in the reaction chamber (110) is higher than 30kPa；
A distillation step: residual liquid phase Mg and MgCl2After the discharge is finished, when the pressure in the reaction cavity (110) is more than 15kPa, the titanium tetrachloride feeding pipe (125) is taken down, and meanwhile, the controller controls the air inlet valve (122) to be opened to fill argon into the reaction cavity (110), so that the pressure in the reaction cavity (110) is higher than 15 kPa; then, a condensation tank (200) is installed on the reaction vessel (100), and a heat insulating member (400) is provided between the installed condensation tank (200) and the reaction vessel (100); finally, closing a vacuum pipeline (220) on the condensing tank (200), and then carrying out positive pressure leak detection on the reaction container (100) to ensure that no leak point exists; in the distillation process, the distillation temperature in the reaction container (100) is controlled to be 900-1020 ℃, and then the cooling spray device (210) is opened to spray CaCl with the injection temperature of-20-0 ℃ and the concentration of 20-35 wt%2Liquid and ensure CaCl2The temperature of the liquid at the liquid outlet of the spray water collecting jacket (211) is less than or equal to 40 ℃ until the distillation is finished;
a product taking-out step: after distillation is finished, power transmission is stopped, the vacuum pipeline (220) is closed, the cooling spray device (210) is turned off, argon is respectively filled from the first vacuum detection port (221) and the second vacuum detection port (128), and the argon filling is stopped when the pressure in the reaction cavity (110) reaches 15 kPa; after the temperature of the outer wall of the reaction container (100) is lower than 50 ℃, the condensing tank (200) and the heat insulation part (400) are disassembled, then the reaction container cover (120) is taken down, and the prepared titanium sponge product is taken out from the reaction cavity (100).
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010894751.8A CN112030009B (en) | 2020-08-31 | 2020-08-31 | Device and method for producing titanium sponge with low nitrogen and oxygen impurity content and low Brinell hardness |
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| CN202010894751.8A CN112030009B (en) | 2020-08-31 | 2020-08-31 | Device and method for producing titanium sponge with low nitrogen and oxygen impurity content and low Brinell hardness |
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| CN112030009B CN112030009B (en) | 2022-07-19 |
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Effective date of registration: 20230922 Address after: 617000 Taoyuan street, East District, Panzhihua, Sichuan Province, No. 90 Patentee after: PANGANG GROUP PANZHIHUA IRON & STEEL RESEARCH INSTITUTE Co.,Ltd. Patentee after: Chengdu advanced metal material industry technology Research Institute Co.,Ltd. Address before: 617000 Taoyuan street, East District, Panzhihua, Sichuan Province, No. 90 Patentee before: PANGANG GROUP PANZHIHUA IRON & STEEL RESEARCH INSTITUTE Co.,Ltd. |