CN115821069B - Temperature control method for rotor-grade titanium sponge inverted U-shaped distillation process - Google Patents
Temperature control method for rotor-grade titanium sponge inverted U-shaped distillation process Download PDFInfo
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Abstract
The invention discloses a temperature control method for a rotor-level titanium sponge inverted U-shaped distillation process, which comprises the following steps of 1) dividing a heating zone of a cylindrical distillation furnace into an A zone, a B zone, a C zone, a D zone and an E zone from top to bottom; 2) Dividing an A zone, a B zone and a C zone, wherein the D zone and the E zone are controllable independent heating zones; the invention can solve the problems of hard core part, excessive chlorine element, different product hardness, unstable smelting process and substandard performance of the titanium sponge core part, so as to meet the use requirements of the field of rotor-grade titanium sponge.
Description
Technical Field
The invention relates to the technical field of titanium sponge smelting engineering, in particular to a temperature control method for a rotor-level inverted U-shaped distillation process of titanium sponge.
Background
The sponge titanium in China is developed at a high speed for more than ten years, the capacity of the low-end and medium-end is seriously excessive, and the capacity of the high-end sponge titanium is insufficient. In particular to a high-quality rotor-grade titanium sponge, which is seriously insufficient in supply and is basically imported. The main expression of the method is that the surface and the inner components of the products of a single heat are uneven, the fluctuation of the components of the products of different heat is large, and the components of the products of multiple heat are not reproducible. The root cause is that the process in the production process is different, the same heating temperature is adopted in different temperature areas, so that the temperature of the area with less materials is easily overhigh, and the temperature of the area with materials is insufficient. The problems that the temperature field is discontinuous in the distillation process, or the surface temperature and the inside temperature are different, the discharge port with loose surface is melted and closed due to the overhigh surface temperature, so that distilled volatile matters cannot be discharged in time or the discharge period is long, the titanium sponge core is hard or chlorine element exceeds standard, and the like are solved. Further affecting the hardness of the products obtained by the subsequent crushing of the titanium sponge, and the smelting process is unstable. The performance of the subsequent materials does not reach the standard, and the use requirements of the high-end field are not met.
Disclosure of Invention
The invention provides a temperature control method for a rotor-level titanium sponge inverted U-shaped distillation process.
The scheme of the invention is as follows:
a temperature control method for a rotor-grade titanium sponge inverted U-shaped distillation process comprises the following steps:
1) Dividing a heating area of a cylindrical distillation furnace into an A area, a B area, a C area, a D area and an E area from top to bottom;
2) Dividing an A zone, a B zone and a C zone, wherein the D zone and the E zone are controllable independent heating zones;
3) After the reduction process is finished, closing a chlorine inlet switch, opening an argon gas charging switch, charging the argon gas atmosphere in the inner container furnace filled with the titanium sponge round titanium lump to 5+/-0.5 kPa, and then maintaining the pressure for 5 minutes; the leakage amount is less than or equal to 10Pa/min, the reduction furnace is connected with the cooler through the inverted U-shaped connecting pipe, after the edge connection is finished, a valve of the U-shaped connecting pipe is opened, the cooler is vacuumized through the vacuum pump set, the vacuum pump set is closed after the vacuum pump set is vacuumized to 50+/-5 Pa;
4) Then distilling by a cylindrical distillation furnace, heating the A area, the B area, the C area, the D area and the E area to 650 ℃ simultaneously, keeping the B area and the C area at constant temperature, heating the A area at 5 ℃/min, after 60min, keeping the A area at 950 ℃ for 2 h; heating the zone B, after 64min, maintaining the temperature of the zone B at 970 ℃ for 2 h; heating the C area, after 64min, maintaining the temperature of the C area at 970 ℃ for 2 h; heating the zone D, after 64min, maintaining the temperature of the zone D at 970 ℃ for 2 h; heating the E area, after 64min, maintaining the E area at 970 ℃ for 2 h; at the moment, the area A, the area B, the area C and the area D are all at 970 ℃, and the temperature of the area E is maintained for 5 to 20 hours;
5) After the temperature of the area A, the area B, the area C and the area D and the area E reach 970 ℃, controlling the area A, the area B, the area C, the area D and the area E to perform counting periodic heating control taking 3h as a unit; wherein the first counting is that the area A and the area C stop heating; stopping heating the zone B and the zone D during the second counting, and recovering heating the zone A and the zone C; stopping heating the A area, the C area and the E area during the third counting, and recovering heating the B area and the D area; stopping heating the B area and the D area and recovering heating the A area, the C area and the E area during the fourth counting; stopping heating the zone A, the zone C and the zone E when counting for the fifth time, and recovering heating the zone B and the zone D; stopping heating the zone B and the zone D and recovering heating the zone A, the zone C and the zone E during the sixth counting; stopping heating in the seventh zone A, the seventh zone C and the seventh zone E, and recovering heating in the seventh zone B and the seventh zone D;
6) After the periodic heating control is completed, continuously heating and preserving the temperature of the A area, the B area, the C area, the D area and the E area for 20-30 hours, wherein the temperature of the A area is controlled to 950 ℃, and the temperatures of the B area, the C area, the D area and the E area are controlled to 960-980 ℃;
7) Vacuum pumps are started to vacuumize the cooler, so that the vacuum degree of the A area, the B area, the C area, the D area and the E area is less than or equal to 4Pa, the vacuumizing is stopped, the temperature of the A area is kept unchanged at 950 ℃, the temperatures of the B area, the C area, the D area and the E area are subjected to secondary temperature rise, and the temperature rise is controlled to be 1020-1040 ℃; the heat preservation time is 50-60 h;
8) After the heat preservation time is up, closing the A area, the B area, the C area, the D area and the E area for heating; the distillation pot was purged back with argon, and the pressure of the purged back was shown to be 10 to 20kPa.
As an preferable technical scheme, the controllable independent heating zone in the step 2) is one of a heating resistance mode or an independent heating unit mode controlled by a PLC.
As a preferable technical scheme, the heating temperature deviation in the step 5) is within +/-5 ℃.
As a preferable technical scheme, in the step 6), the temperature difference of the B area, the C area, the D area and the E area is controlled to be 970.
As a preferable technical scheme, in the step 7), the temperatures of the B area, the C area, the D area and the E area are controlled at 1030 ℃.
Due to the adoption of the technical scheme, the temperature control method for the inverted U-shaped distillation process of the rotor-level titanium sponge comprises the following steps of: 1) Dividing a heating area of a cylindrical distillation furnace into an A area, a B area, a C area, a D area and an E area from top to bottom;
2) Dividing an A zone, a B zone and a C zone, wherein the D zone and the E zone are controllable independent heating zones;
3) After the reduction process is finished, closing a chlorine inlet switch, opening an argon gas charging switch, charging the argon gas atmosphere in the inner container furnace filled with the titanium sponge round titanium lump to 5+/-0.5 kPa, and then maintaining the pressure for 5 minutes; the leakage amount is less than or equal to 10Pa/min, the reduction furnace is connected with the cooler through the inverted U-shaped connecting pipe, after the edge connection is finished, a valve of the U-shaped connecting pipe is opened, the cooler is vacuumized through the vacuum pump set, the vacuum pump set is closed after the vacuum pump set is vacuumized to 50+/-5 Pa;
4) Then distilling by a cylindrical distillation furnace, heating the A area, the B area, the C area, the D area and the E area to 650 ℃ simultaneously, keeping the B area and the C area at constant temperature, heating the A area at 5 ℃/min, after 60min, keeping the A area at 950 ℃ for 2 h; heating the zone B, after 64min, maintaining the temperature of the zone B at 970 ℃ for 2 h; heating the C area, after 64min, maintaining the temperature of the C area at 970 ℃ for 2 h; heating the zone D, after 64min, maintaining the temperature of the zone D at 970 ℃ for 2 h; heating the E area, after 64min, maintaining the E area at 970 ℃ for 2 h; at the moment, the area A, the area B, the area C and the area D are all at 970 ℃, and the temperature of the area E is maintained for 5 to 20 hours;
5) After the temperature of the area A, the area B, the area C and the area D and the area E reach 970 ℃, controlling the area A, the area B, the area C, the area D and the area E to perform counting periodic heating control taking 3h as a unit; wherein the first counting is that the area A and the area C stop heating; stopping heating the zone B and the zone D during the second counting, and recovering heating the zone A and the zone C; stopping heating the A area, the C area and the E area during the third counting, and recovering heating the B area and the D area; stopping heating the B area and the D area and recovering heating the A area, the C area and the E area during the fourth counting; stopping heating the zone A, the zone C and the zone E when counting for the fifth time, and recovering heating the zone B and the zone D; stopping heating the zone B and the zone D and recovering heating the zone A, the zone C and the zone E during the sixth counting; stopping heating in the seventh zone A, the seventh zone C and the seventh zone E, and recovering heating in the seventh zone B and the seventh zone D;
6) After the periodic heating control is completed, continuously heating and preserving the temperature of the A area, the B area, the C area, the D area and the E area for 20-30 hours, wherein the temperature of the A area is controlled to 950 ℃, and the temperatures of the B area, the C area, the D area and the E area are controlled to 960-980 ℃;
7) Vacuum pumps are started to vacuumize the cooler, so that the vacuum degree of the A area, the B area, the C area, the D area and the E area is less than or equal to 4Pa, the vacuumizing is stopped, the temperature of the A area is kept unchanged at 950 ℃, the temperatures of the B area, the C area, the D area and the E area are subjected to secondary temperature rise, and the temperature rise is controlled to be 1020-1040 ℃; the heat preservation time is 50-60 h;
8) After the heat preservation time is up, closing the A area, the B area, the C area, the D area and the E area for heating; the distillation pot was purged back with argon, and the pressure of the purged back was shown to be 10 to 20kPa.
The invention has the advantages that:
the invention can solve the problems of hard core part, excessive chlorine element, different product hardness, unstable smelting process and substandard performance of the titanium sponge core part, so as to meet the use requirements of the field of rotor-grade titanium sponge.
(1) The invention not only can effectively control the distillation temperature by controlling the heating and heat preservation process and realize the continuity of a flow field temperature field in the distillation process, but also solves the problems of blockage in the distillation process and closing of the surface of the titanium lump due to overhigh distillation temperature. Realizing the effectiveness and the duration of the titanium lump distillation.
(2) The method provided by the invention has the advantages that the titanium lump components are reproducible, the operation is convenient, the multi-heat homogeneity control of the titanium lump components can be realized, the high quality of the titanium lump is realized, and the product has good market competitiveness.
Drawings
FIG. 1 is a view showing a heating section of a cylindrical distillation furnace according to an embodiment of the present invention.
1-A region; a region 2-B; 3-C region; a 4-D region; 5-E region.
Detailed Description
In order to overcome the defects, the invention provides a temperature control method for a rotor-grade titanium sponge inverted U-shaped distillation process, which solves the problems in the prior art.
A temperature control method for a rotor-grade titanium sponge inverted U-shaped distillation process comprises the following steps:
1) Dividing a heating area of a cylindrical distillation furnace into an A area, a B area, a C area, a D area and an E area from top to bottom;
2) Dividing an A zone, a B zone and a C zone, wherein the D zone and the E zone are controllable independent heating zones;
3) After the reduction process is finished, closing a chlorine inlet switch, opening an argon gas charging switch, charging the argon gas atmosphere in the inner container furnace filled with the titanium sponge round titanium lump to 5+/-0.5 kPa, and then maintaining the pressure for 5 minutes; the leakage amount is less than or equal to 10Pa/min, the reduction furnace is connected with the cooler through the inverted U-shaped connecting pipe, after the edge connection is finished, a valve of the U-shaped connecting pipe is opened, the cooler is vacuumized through the vacuum pump set, the vacuum pump set is closed after the vacuum pump set is vacuumized to 50+/-5 Pa;
4) Then distilling by a cylindrical distillation furnace, heating the A area, the B area, the C area, the D area and the E area to 650 ℃ simultaneously, keeping the B area and the C area at constant temperature, heating the A area at 5 ℃/min, after 60min, keeping the A area at 950 ℃ for 2 h; heating the zone B, after 64min, maintaining the temperature of the zone B at 970 ℃ for 2 h; heating the C area, after 64min, maintaining the temperature of the C area at 970 ℃ for 2 h; heating the zone D, after 64min, maintaining the temperature of the zone D at 970 ℃ for 2 h; heating the E area, after 64min, maintaining the E area at 970 ℃ for 2 h; at the moment, the area A, the area B, the area C and the area D are all at 970 ℃, and the temperature of the area E is maintained for 5 to 20 hours;
5) After the temperature of the area A, the area B, the area C and the area D and the area E reach 970 ℃, controlling the area A, the area B, the area C, the area D and the area E to perform counting periodic heating control taking 3h as a unit; wherein the first counting is that the area A and the area C stop heating; stopping heating the zone B and the zone D during the second counting, and recovering heating the zone A and the zone C; stopping heating the A area, the C area and the E area during the third counting, and recovering heating the B area and the D area; stopping heating the B area and the D area and recovering heating the A area, the C area and the E area during the fourth counting; stopping heating the zone A, the zone C and the zone E when counting for the fifth time, and recovering heating the zone B and the zone D; stopping heating the zone B and the zone D and recovering heating the zone A, the zone C and the zone E during the sixth counting; stopping heating in the seventh zone A, the seventh zone C and the seventh zone E, and recovering heating in the seventh zone B and the seventh zone D;
6) After the periodic heating control is completed, continuously heating and preserving the temperature of the A area, the B area, the C area, the D area and the E area for 20-30 hours, wherein the temperature of the A area is controlled to 950 ℃, and the temperatures of the B area, the C area, the D area and the E area are controlled to 960-980 ℃;
7) Vacuum pumps are started to vacuumize the cooler, so that the vacuum degree of the A area, the B area, the C area, the D area and the E area is less than or equal to 4Pa, the vacuumizing is stopped, the temperature of the A area is kept unchanged at 950 ℃, the temperatures of the B area, the C area, the D area and the E area are subjected to secondary temperature rise, and the temperature rise is controlled to be 1020-1040 ℃; the heat preservation time is 50-60 h;
8) After the heat preservation time is up, closing the A area, the B area, the C area, the D area and the E area for heating; the distillation pot was purged back with argon, and the pressure of the purged back was shown to be 10 to 20kPa.
The controllable independent heating area in the step 2) is one of a heating resistance mode or an independent heating unit mode controlled by a PLC.
The heating temperature deviation in the step 5) is within +/-5 ℃.
In the step 6), the temperature difference of the zone B, the zone C, the zone D and the zone E is controlled to be 970.
In the step 7), the temperatures of the zone B, the zone C, the zone D and the zone E are controlled at 1030 ℃.
The invention is further described in connection with the following embodiments in order to make the technical means, the creation features, the achievement of the purpose and the effect of the invention easy to understand.
Example 1
(1) Equally dividing the heating area of the cylindrical distillation furnace into five equal parts along the length from top to bottom in the height direction, and sequentially named as an A area, a B area, a C area, a D area and an E area;
(2) Setting/modifying the heating resistors of the divided heating areas into independent heating units which can be controlled by a PLC (programmable logic controller);
(3) After the reduction process is finished, closing a chlorine inlet switch, opening an argon gas charging switch, charging the argon gas atmosphere in the inner container furnace filled with the titanium sponge round titanium lump to 5kPa, and then maintaining the pressure for 5 minutes. The leakage amount is less than or equal to 10Pa/min. The reduction furnace is connected with the cooler through an inverted U-shaped connecting pipe, a valve of the U-shaped connecting pipe is opened after the edge connection is finished, the cooler is vacuumized through a vacuum pump set, the pressure is pumped to 50Pa, and the vacuum pump set is closed;
(4) And then hanging the liner furnace into a cylindrical distillation furnace for distillation, heating the A region, the B region, the C region and the D region to 650 ℃ simultaneously, keeping the B region and the C region at constant temperature, heating the A region at 5 ℃/min, heating the B region after 60min, keeping the temperature of the A region at 950 ℃ for 2h, heating the B region after 64min, keeping the temperature of the B region at 970 ℃ for 2h, heating the C region after 64min, and keeping the temperature of the C region at 970 ℃ for 2 h. Heating the zone D, after 64min, maintaining the temperature of the zone D at 970 ℃ for 2h, heating the zone E, after 64min, maintaining the temperature of the zone E at 970 ℃ for 2 h. At this point, the five zones were all at 970℃for 5h.
(5) After the five areas reach the temperature, the temperature areas are subjected to counting periodic heating control by taking 3h as a unit through a PLC. The first count is A, C and then B, D, at which time the first count resumes heating at A, C. After the end of the second count B, D, B, D resumes heating, at which point A, C, E stops heating. The next group B, D and group A, C, E are cycled 7 times.
(6) After 7 times of circulation are finished, continuously heating and preserving heat for 20 hours in the A-E area, controlling the temperature of the A area at 950 ℃ and controlling the temperature of the B-E area at 970 ℃.
(7) And (3) starting a vacuum pump to vacuumize the cooler, stopping vacuumizing to ensure that the vacuum degree of each region is less than or equal to 4Pa, keeping the temperature of the region A unchanged at 950 ℃, and carrying out secondary temperature rise on the temperatures of the regions B to E, wherein the temperature rise is controlled to be 1030 ℃. The incubation time was 50h.
(8) And after the heat preservation time is up, turning off the heating power supply of all the temperature areas. The distillation pot was flushed back with argon, the pressure of which was shown to be 10kPa.
Example 2
(1) Equally dividing the heating area of the cylindrical distillation furnace into five equal parts along the length from top to bottom in the height direction, and sequentially named as an A area, a B area, a C area, a D area and an E area;
(2) Setting/modifying the heating resistors of the divided heating areas into independent heating units which can be controlled by a PLC (programmable logic controller);
(3) After the reduction process is finished, closing a chlorine inlet switch, opening an argon gas charging switch, charging the argon gas atmosphere in the inner container furnace filled with the titanium sponge round titanium lump to 4.95kPa, and then maintaining the pressure for 5 minutes. The leakage amount is less than or equal to 10Pa/min. The reduction furnace is connected with the cooler through an inverted U-shaped connecting pipe, a valve of the U-shaped connecting pipe is opened after the edge connection is finished, the cooler is vacuumized through a vacuum pump set, the pressure is pumped to 45Pa, and the vacuum pump set is closed;
(4) Heating the A area, the B area, the C area and the D area simultaneously until the E area is heated to 650 ℃, keeping the B area and the C area at constant temperature, heating the A area at 5 ℃/min, heating the B area after 60min, keeping the A area at 955 ℃ for 2h, heating the B area after 64min, keeping the B area at 975 ℃ for 2h, heating the C area after 64min, and keeping the C area at 975 ℃ for 2 h. Heating the zone D, after 64min, maintaining the temperature of the zone D at 975 ℃ for 2h, heating the zone E, after 64min, maintaining the temperature of the zone E at 970 ℃ for 2 h. At this point, the five zones were all at 970℃for 5h.
(5) After the five areas reach the temperature, the temperature areas are subjected to counting periodic heating control by taking 3h as a unit through a PLC. The first count is A, C and then B, D, at which time the first count resumes heating at A, C. After the end of the second count B, D, B, D resumes heating, at which point A, C, E stops heating. The next group B, D and group A, C, E are cycled 7 times.
(6) After 7 times of circulation are finished, continuously heating and preserving heat for 25 hours in the A-E area, controlling the temperature of the A area at 955 ℃, and controlling the temperature of the B area to the E area at 975 ℃.
(7) And (3) starting a vacuum pump to vacuumize the cooler, stopping vacuumizing to ensure that the vacuum degree of each region is less than or equal to 4Pa, keeping the temperature of the region A at 955 ℃, carrying out secondary temperature rise on the temperature of the regions B to E, and controlling the temperature rise to 1030 ℃. The heat preservation time is 55h.
(8) And after the heat preservation time is up, turning off the heating power supply of all the temperature areas. The distillation pot was flushed back with argon, the pressure of which was shown to be 15kPa.
Example 3
(1) Equally dividing the heating area of the cylindrical distillation furnace into five equal parts along the length from top to bottom in the height direction, and sequentially named as an A area, a B area, a C area, a D area and an E area;
(2) Setting/modifying the heating resistors of the divided heating areas into independent heating units which can be controlled by a PLC (programmable logic controller);
(3) After the reduction process is finished, closing a chlorine inlet switch, opening an argon gas charging switch, charging the argon gas atmosphere in the inner container furnace filled with the titanium sponge round titanium lump to 5.5kPa, and then maintaining the pressure for 5 minutes. The leakage amount is less than or equal to 10Pa/min. The reduction furnace is connected with the cooler through an inverted U-shaped connecting pipe, a valve of the U-shaped connecting pipe is opened after the edge connection is finished, the cooler is vacuumized through a vacuum pump set, the pressure is pumped to 55Pa, and the vacuum pump set is closed;
(4) Heating the A area, the B area, the C area and the D area at the same time, keeping the B area and the C area at a constant temperature after the E area is heated to 645 ℃, heating the A area at 5 ℃/min, heating the B area after the A area reaches 945 ℃ for 2 hours after 60 minutes, heating the C area after the B area reaches 965 ℃ for 2 hours after 64 minutes, heating the C area after the C area reaches 965 ℃ for 2 hours after 64 minutes, and keeping the C area at the temperature of 965 ℃ after 2 hours. Heating the zone D, after 64min, maintaining the temperature of the zone D at 965 ℃ for 2h, heating the zone E, after 64min, maintaining the temperature of the zone E at 965 ℃ for 2 h. At this point, the five zones were maintained at 965℃for 5h.
(5) After the five areas reach the temperature, the temperature areas are subjected to counting periodic heating control by taking 3h as a unit through a PLC. The first count is A, C and then B, D, at which time the first count resumes heating at A, C. After the end of the second count B, D, B, D resumes heating, at which point A, C, E stops heating. The next group B, D and group A, C, E are cycled 7 times.
(6) After 7 times of circulation are finished, continuously heating and preserving heat for 30 hours in the A-E area, controlling the temperature of the A area at 945 ℃, and controlling the temperature of the B area to the E area at 965 ℃.
(7) And (3) starting a vacuum pump to vacuumize the cooler, stopping vacuumizing to ensure that the vacuum degree of each region is less than or equal to 4Pa, keeping the temperature of the region A at 945 ℃, carrying out secondary temperature rise on the temperature of the regions B to E, and controlling the temperature rise to 1030 ℃. The heat preservation time is 60h.
(8) And after the heat preservation time is up, turning off the heating power supply of all the temperature areas. The distillation pot was flushed back with argon, the pressure of which was shown to be 20kPa.
Example 4
1) Dividing a heating area of a cylindrical distillation furnace into an A area, a B area, a C area, a D area and an E area from top to bottom;
2) Dividing an A zone, a B zone and a C zone, wherein the D zone and the E zone are controllable independent heating zones;
3) After the reduction process is finished, closing a chlorine inlet switch, opening an argon gas charging switch, charging the argon gas atmosphere in the inner container furnace filled with the titanium sponge round titanium lump to 5+/-0.5 kPa, and then maintaining the pressure for 5 minutes; the leakage amount is less than or equal to 10Pa/min, the reduction furnace is connected with the cooler through the inverted U-shaped connecting pipe, after the edge connection is finished, a valve of the U-shaped connecting pipe is opened, the cooler is vacuumized through the vacuum pump set, the vacuum pump set is closed after the vacuum pump set is vacuumized to 50+/-5 Pa;
4) Then distilling by a cylindrical distillation furnace, heating the A area, the B area, the C area, the D area and the E area to 650 ℃ simultaneously, keeping the B area and the C area at constant temperature, heating the A area at 5 ℃/min, after 60min, keeping the A area at 950 ℃ for 2 h; heating the zone B, after 64min, maintaining the temperature of the zone B at 970 ℃ for 2 h; heating the C area, after 64min, maintaining the temperature of the C area at 970 ℃ for 2 h; heating the zone D, after 64min, maintaining the temperature of the zone D at 970 ℃ for 2 h; heating the E area, after 64min, maintaining the E area at 970 ℃ for 2 h; at the moment, the area A, the area B, the area C and the area D are all at 970 ℃, and the temperature of the area E is maintained for 5 to 20 hours;
5) After the temperature of the area A, the area B, the area C and the area D and the area E reach 970 ℃, controlling the area A, the area B, the area C, the area D and the area E to perform counting periodic heating control taking 3h as a unit; wherein the first counting is that the area A and the area C stop heating; stopping heating the zone B and the zone D during the second counting, and recovering heating the zone A and the zone C; stopping heating the A area, the C area and the E area during the third counting, and recovering heating the B area and the D area; stopping heating the B area and the D area and recovering heating the A area, the C area and the E area during the fourth counting; stopping heating the zone A, the zone C and the zone E when counting for the fifth time, and recovering heating the zone B and the zone D; stopping heating the zone B and the zone D and recovering heating the zone A, the zone C and the zone E during the sixth counting; stopping heating in the seventh zone A, the seventh zone C and the seventh zone E, and recovering heating in the seventh zone B and the seventh zone D;
6) After the periodic heating control is completed, continuously heating and preserving the temperature of the A area, the B area, the C area, the D area and the E area for 20-30 hours, wherein the temperature of the A area is controlled to 950 ℃, and the temperatures of the B area, the C area, the D area and the E area are controlled to 960-980 ℃;
7) Vacuum pumps are started to vacuumize the cooler, so that the vacuum degree of the A area, the B area, the C area, the D area and the E area is less than or equal to 4Pa, the vacuumizing is stopped, the temperature of the A area is kept unchanged at 950 ℃, the temperatures of the B area, the C area, the D area and the E area are subjected to secondary temperature rise, and the temperature rise is controlled to be 1020-1040 ℃; the heat preservation time is 50-60 h;
8) After the heat preservation time is up, closing the A area, the B area, the C area, the D area and the E area for heating; the distillation pot was purged back with argon, and the pressure of the purged back was shown to be 10 to 20kPa.
The controllable independent heating area in the step 2) is one of a heating resistance mode or an independent heating unit mode controlled by a PLC.
The heating temperature deviation in the step 5) is within +/-5 ℃.
In the step 6), the temperature difference of the zone B, the zone C, the zone D and the zone E is controlled to be 970.
In the step 7), the temperatures of the zone B, the zone C, the zone D and the zone E are controlled at 1030 ℃.
The foregoing has shown and described the basic principles, main features and advantages of the present invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and that the above embodiments and descriptions are merely illustrative of the principles of the present invention, and various changes and modifications may be made without departing from the spirit and scope of the invention, which is defined in the appended claims. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (3)
1. The temperature control method for the inverted U-shaped distillation process of the rotor-grade titanium sponge is characterized by comprising the following steps of:
1) Dividing a heating area of a cylindrical distillation furnace into an A area, a B area, a C area, a D area and an E area from top to bottom;
2) Dividing an A zone, a B zone and a C zone, wherein the D zone and the E zone are controllable independent heating zones; the controllable independent heating area is one of a heating resistance mode or an independent heating unit mode controlled by a PLC (programmable logic controller);
3) After the reduction process is finished, closing a chlorine inlet switch, opening an argon gas charging switch, charging the argon gas atmosphere in the inner container furnace filled with the titanium sponge round titanium lump to 5+/-0.5 kPa, and then maintaining the pressure for 5 minutes; the leakage amount is less than or equal to 10Pa/min, the reduction furnace is connected with the cooler through the inverted U-shaped connecting pipe, after the edge connection is finished, a valve of the U-shaped connecting pipe is opened, the cooler is vacuumized through the vacuum pump set, the vacuum pump set is closed after the vacuum pump set is vacuumized to 50+/-5 Pa;
4) Then distilling by a cylindrical distillation furnace, heating the A area, the B area, the C area, the D area and the E area to 650 ℃ simultaneously, keeping the B area and the C area at constant temperature, heating the A area at 5 ℃/min, after 60min, keeping the A area at 950 ℃ for 2 h; heating the zone B, after 64min, maintaining the temperature of the zone B at 970 ℃ for 2 h; heating the C area, after 64min, maintaining the temperature of the C area at 970 ℃ for 2 h; heating the zone D, after 64min, maintaining the temperature of the zone D at 970 ℃ for 2 h; heating the E area, after 64min, maintaining the E area at 970 ℃ for 2 h; at the moment, the area A, the area B, the area C and the area D are all at 970 ℃, and the temperature of the area E is maintained for 5 to 20 hours;
5) After the temperature of the area A, the area B, the area C and the area D and the area E reach 970 ℃, controlling the area A, the area B, the area C, the area D and the area E to perform counting periodic heating control taking 3h as a unit; wherein the first counting is that the area A and the area C stop heating; stopping heating the zone B and the zone D during the second counting, and recovering heating the zone A and the zone C; stopping heating the A area, the C area and the E area during the third counting, and recovering heating the B area and the D area; stopping heating the B area and the D area and recovering heating the A area, the C area and the E area during the fourth counting; stopping heating the zone A, the zone C and the zone E when counting for the fifth time, and recovering heating the zone B and the zone D; stopping heating the zone B and the zone D and recovering heating the zone A, the zone C and the zone E during the sixth counting; stopping heating in the seventh zone A, the seventh zone C and the seventh zone E, and recovering heating in the seventh zone B and the seventh zone D; the heating temperature deviation is +/-5 ℃;
6) After the periodic heating control is completed, continuously heating and preserving the temperature of the A area, the B area, the C area, the D area and the E area for 20-30 hours, wherein the temperature of the A area is controlled to 950 ℃, and the temperatures of the B area, the C area, the D area and the E area are controlled to 960-980 ℃;
7) Vacuum pumps are started to vacuumize the cooler, so that the vacuum degree of the A area, the B area, the C area, the D area and the E area is less than or equal to 4Pa, the vacuumizing is stopped, the temperature of the A area is kept unchanged at 950 ℃, the temperatures of the B area, the C area, the D area and the E area are subjected to secondary temperature rise, and the temperature rise is controlled to be 1020-1040 ℃; the heat preservation time is 50-60 h;
8) After the heat preservation time is up, closing the A area, the B area, the C area, the D area and the E area for heating; the distillation pot was purged back with argon, and the pressure of the purged back was shown to be 10 to 20kPa.
2. The rotor-grade titanium sponge inverted U-shaped distillation process temperature control method of claim 1, wherein the method comprises the steps of: in the step 6), the temperatures of the zone B, the zone C, the zone D and the zone E are controlled to be 970 ℃.
3. The rotor-grade titanium sponge inverted U-shaped distillation process temperature control method of claim 1, wherein the method comprises the steps of: in the step 7), the temperatures of the zone B, the zone C, the zone D and the zone E are controlled at 1030 ℃.
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| GB768124A (en) * | 1953-06-13 | 1957-02-13 | Peter Spence & Sons Ltd | Improved method and apparatus for obtaining ductile titanium or zirconium |
| US5582630A (en) * | 1995-02-21 | 1996-12-10 | Sony Corporation | Ultra high purity magnesium vacuum distillation purification method |
| CN102534261B (en) * | 2012-01-18 | 2013-04-10 | 深圳市新星轻合金材料股份有限公司 | Process method for preparing titanium sponge |
| CN103215461B (en) * | 2013-05-22 | 2014-11-26 | 朝阳金达钛业股份有限公司 | 15-ton inverted-U-shaped combination device and production process for producing sponge titanium |
| CN106350687B (en) * | 2016-09-05 | 2018-08-14 | 成都先进金属材料产业技术研究院有限公司 | The device and method of separating-purifying titanium sponge |
| CN107287449A (en) * | 2017-08-17 | 2017-10-24 | 东方弗瑞德（北京）科技有限公司 | A kind of argon gas introducing device and introducing method produced for magnesium method titanium sponge |
| CN109988916A (en) * | 2019-05-21 | 2019-07-09 | 贵州省钛材料研发中心有限公司 | A kind of method that reverse"U"connecting furnace produces high-purity titanium sponge |
| CN113721571A (en) * | 2021-08-31 | 2021-11-30 | 朝阳金达钛业股份有限公司 | Control method of DCS (distributed control System) for producing titanium sponge |
| CN114703380A (en) * | 2022-03-24 | 2022-07-05 | 朝阳金达钛业股份有限公司 | Production method of titanium sponge with ultralow chlorine content |
| CN115094249B (en) * | 2022-07-12 | 2023-08-08 | 朝阳金达钛业股份有限公司 | Application method of reduction distillation heating furnace for reducing packaging density of titanium sponge |
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