CN110480029B - Positive pressure reaction device and method for dehydrogenation of titanium hydride powder - Google Patents
Positive pressure reaction device and method for dehydrogenation of titanium hydride powder Download PDFInfo
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- CN110480029B CN110480029B CN201910667405.3A CN201910667405A CN110480029B CN 110480029 B CN110480029 B CN 110480029B CN 201910667405 A CN201910667405 A CN 201910667405A CN 110480029 B CN110480029 B CN 110480029B
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 139
- 239000000843 powder Substances 0.000 title claims abstract description 106
- -1 titanium hydride Chemical compound 0.000 title claims abstract description 106
- 229910000048 titanium hydride Inorganic materials 0.000 title claims abstract description 106
- 238000006356 dehydrogenation reaction Methods 0.000 title claims abstract description 71
- 238000000034 method Methods 0.000 title claims abstract description 31
- 239000007789 gas Substances 0.000 claims abstract description 222
- 239000011261 inert gas Substances 0.000 claims abstract description 86
- 239000001257 hydrogen Substances 0.000 claims abstract description 80
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 80
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 74
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 21
- 239000001301 oxygen Substances 0.000 claims abstract description 14
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 14
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 13
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 54
- 238000010438 heat treatment Methods 0.000 claims description 41
- 239000002516 radical scavenger Substances 0.000 claims description 37
- 229940123973 Oxygen scavenger Drugs 0.000 claims description 34
- 239000000919 ceramic Substances 0.000 claims description 27
- 229910052751 metal Inorganic materials 0.000 claims description 24
- 239000002184 metal Substances 0.000 claims description 24
- 238000001816 cooling Methods 0.000 claims description 21
- 238000007789 sealing Methods 0.000 claims description 13
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 11
- 238000004321 preservation Methods 0.000 claims description 10
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 9
- 229910052791 calcium Inorganic materials 0.000 claims description 9
- 239000011575 calcium Substances 0.000 claims description 9
- 238000005507 spraying Methods 0.000 claims description 9
- 239000010936 titanium Substances 0.000 claims description 7
- 229910052719 titanium Inorganic materials 0.000 claims description 7
- 238000009423 ventilation Methods 0.000 claims description 7
- 239000000428 dust Substances 0.000 claims description 6
- 150000002431 hydrogen Chemical class 0.000 claims description 5
- 229910052749 magnesium Inorganic materials 0.000 claims description 5
- 239000011777 magnesium Substances 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims description 5
- 238000005086 pumping Methods 0.000 claims description 4
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 3
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 3
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 3
- 230000007423 decrease Effects 0.000 claims description 2
- 239000011148 porous material Substances 0.000 claims 3
- 230000009286 beneficial effect Effects 0.000 abstract description 4
- 238000000354 decomposition reaction Methods 0.000 abstract description 4
- 230000000149 penetrating effect Effects 0.000 abstract description 3
- 238000002360 preparation method Methods 0.000 abstract description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 62
- 229910052786 argon Inorganic materials 0.000 description 32
- 239000001307 helium Substances 0.000 description 18
- 229910052734 helium Inorganic materials 0.000 description 18
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 18
- 239000012535 impurity Substances 0.000 description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 10
- 239000000203 mixture Substances 0.000 description 8
- 238000009413 insulation Methods 0.000 description 5
- 229910052757 nitrogen Inorganic materials 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 230000000903 blocking effect Effects 0.000 description 4
- 239000000498 cooling water Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000007599 discharging Methods 0.000 description 3
- 238000011049 filling Methods 0.000 description 3
- 238000005984 hydrogenation reaction Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000004663 powder metallurgy Methods 0.000 description 3
- 239000007921 spray Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 238000006073 displacement reaction Methods 0.000 description 2
- 230000008595 infiltration Effects 0.000 description 2
- 238000001764 infiltration Methods 0.000 description 2
- 238000002955 isolation Methods 0.000 description 2
- DOTMOQHOJINYBL-UHFFFAOYSA-N molecular nitrogen;molecular oxygen Chemical compound N#N.O=O DOTMOQHOJINYBL-UHFFFAOYSA-N 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000007664 blowing Methods 0.000 description 1
- 230000036760 body temperature Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000009694 cold isostatic pressing Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000001513 hot isostatic pressing Methods 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 238000001144 powder X-ray diffraction data Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/30—Making metallic powder or suspensions thereof using chemical processes with decomposition of metal compounds, e.g. by pyrolysis
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Powder Metallurgy (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention provides a positive pressure reaction device and a dehydrogenation method for dehydrogenating titanium hydride powder, and belongs to the technical field of powder preparation. The positive pressure reaction device for dehydrogenating the titanium hydride powder can heat the titanium hydride powder by using the inert gas as a carrier, can bring hydrogen generated by dehydrogenation out of a reaction tank while creating a positive pressure atmosphere to prevent external air from penetrating, is beneficial to the decomposition and dehydrogenation of the titanium hydride powder, and can recycle the inert gas and remove hydrogen and oxygen contained in the inert gas by using a dehydrogenation agent and an deoxidizer, thereby reducing gas consumption and improving the purity of a product while ensuring thorough dehydrogenation of the titanium hydride.
Description
Technical Field
The invention relates to the technical field of powder preparation, and particularly provides a positive pressure reaction device and a dehydrogenation method for dehydrogenating titanium hydride powder.
Background
Titanium has the characteristics of high specific strength, low specific gravity, corrosion resistance and the like, and is widely applied to the fields of aviation, aerospace, weapons, ships, energy and the like. The titanium powder is used for powder metallurgy (hot isostatic pressing, cold isostatic pressing, etc. depressurization and injection molding), so that titanium parts with complex shapes can be manufactured, and the titanium processing cost is greatly reduced. Titanium powder is metal titanium particles with a size of less than 1mm, and is used for powder metallurgy, and the particle size is required to be fine, low-oxygen and high-purity. Titanium powder has large surface free energy, and is easier to react with other elements or compounds than massive metallic titanium, so that the purity and the performance of the titanium powder depend on the preparation method and the process conditions.
The hydrogenation dehydrogenation method (HDH method for short) is the most common method for preparing titanium powder at present, and the main working procedure is that firstly, sponge titanium is subjected to hydrogenation treatment, then is crushed to obtain titanium hydride powder, and finally, the titanium hydride powder is subjected to high-temperature dehydrogenation under vacuum, and is cooled to obtain the titanium powder. The hydrogenation dehydrogenation method is characterized in that the process flow is long, impurities are easily led in the actual application of the production to cause the increase of the nitrogen and oxygen content of the final product, and the links of high-temperature dehydrogenation and cooling are most easily polluted by nitrogen and oxygen. The method is mainly characterized in that in the dehydrogenation and cooling process, a negative pressure environment is maintained in a dehydrogenation furnace for a long time, the phenomenon of external air infiltration is unavoidable, the surface area of titanium powder is large, and the infiltrated air reacts with the titanium powder in the high-temperature environment in the furnace, so that the oxygen and nitrogen content of the titanium powder is high, the performance of finally preparing the titanium powder is influenced, and the development of the powder metallurgy titanium industry is severely restricted.
Disclosure of Invention
Aiming at the problems existing in the prior art, the embodiment of the invention provides a positive pressure reaction device and a dehydrogenation method for dehydrogenating titanium hydride powder, which utilize inert gas as a carrier to heat the titanium hydride powder, and can bring hydrogen generated by dehydrogenation out of a reaction tank while creating a positive pressure atmosphere to prevent external gas from penetrating, thereby being beneficial to decomposing and dehydrogenating the titanium hydride powder.
The technical scheme of the invention is as follows:
the positive pressure reaction device for dehydrogenating titanium hydride powder comprises a reaction tank 1, a first gas cooler 2, a gas circulating pump 3, a gas purifier 4, a gas heater 6, a movable heat insulation sleeve 8, an inert gas source and a vacuumizing system, wherein the first gas cooler 2, the gas circulating pump 3, the gas purifier 4 and the gas heater 6 are sequentially connected through pipelines, the input end of the first gas cooler 2 is connected with an air outlet pipe 1-4 of the reaction tank 1, the output end of the gas heater 6 is connected with an air inlet pipe 1-3 of the reaction tank 1 to form a loop, a dust-isolation ventilation screen 1-6 is arranged in the reaction tank 1, the dust-isolation ventilation screen 1-6 divides the inner cavity of the reaction tank 1 into a first cavity and a second cavity, the air outlet pipe 1-4 is positioned in the first cavity, the air inlet pipe 1-3 is positioned in the second cavity, the air inlet pipe 1-3 extends to the end far away from the dust-separation ventilation screen 1-6 in the second cavity to be close to the end part of the reaction tank 1, the movable heat preservation sleeve 8 is used for preserving heat of the second cavity area during reaction dehydrogenation, when titanium hydride powder is dehydrogenated, the vacuum system is firstly used for vacuumizing the loop, then the vacuum system is closed, inert gas is provided for the loop through the inert gas source, the inert gas is purified by the gas purifier 4 and then enters the reaction tank 1 after being heated to 750-800 ℃ by the gas heater 6, titanium hydride powder in the reaction tank 1 is heated, so that the titanium hydride powder is decomposed to release hydrogen, the inert gas brings the generated hydrogen out of the reaction tank 1 under the action of the gas circulating pump 3, dust carried by the inert gas is trapped in the second cavity after passing through the dust-separation ventilation screens 1-6, the inert gas carrying hydrogen is cooled by the first gas cooler 2 and enters the gas purifier 4, and oxygen and hydrogen in the inert gas are removed by the gas purifier 4.
Further, the positive pressure reaction device for dehydrogenating the titanium hydride powder further comprises a second gas cooler 5 arranged between the gas purifier 4 and the gas heater 6, wherein after the vacuum is pumped, inert gas is provided for the loop through the inert gas source, and after the inert gas is purified by the gas purifier 4, the inert gas is cooled to below 30 ℃ by the second gas cooler 5 and circulates in the loop for at least 30min.
Specifically, the gas purifier 4 comprises a sealed cavity, a ceramic block 4-1, an oxygen scavenger 4-2, a hydrogen scavenger 4-3 and a heating plate 4-4, wherein the heating plate 4-4 is sleeved on the inner wall of the sealed cavity, the ceramic block 4-1, the oxygen scavenger 4-2 and the hydrogen scavenger 4-3 are all positioned in a space surrounded by the heating plate 4-4, the oxygen scavenger 4-2 and the hydrogen scavenger 4-3 are of a layered structure, the ceramic block 4-1 is used for isolating each layer of the oxygen scavenger 4-2 and the hydrogen scavenger 4-3, the oxygen scavenger 4-2 is magnesium metal or calcium metal, the hydrogen scavenger 4-3 is titanium sponge, the ceramic block 4-1 is aluminum oxide or zirconium oxide, and the heating plate 4-4 is used for maintaining the temperature in the sealed cavity at 270-330 ℃.
Specifically, the mass ratio of the deoxidizer 4-2 to the dehydrogenation agent 4-3 is 1.5-2.5:1.
Specifically, a pressure relief valve 1-5 is arranged on a shell of the first cavity of the reaction tank 1, and the pressure relief valve 1-5 automatically vents and reduces pressure when the pressure in the reaction tank 1 is greater than 1.5 MPa.
Further, the positive pressure reaction device for dehydrogenating the titanium hydride powder further comprises a spraying device 7 for cooling the reaction tank 1 after the reaction is finished.
Specifically, the dust-proof air-permeable screen 1-6 comprises a plurality of porous metal plates, gaps are arranged among the metal plates, the aperture on the metal plates is gradually decreased along the direction from the second cavity to the first cavity, the maximum aperture is 3-5 mm, and the minimum aperture is 0.3-0.5 mm.
A positive pressure dehydrogenation method for dehydrogenating titanium hydride powder, wherein the positive pressure reaction device is used for dehydrogenating titanium hydride powder.
Specifically, the gas purifier 4 comprises a sealed cavity, a ceramic block 4-1, an oxygen scavenger 4-2, a hydrogen scavenger 4-3 and a heating plate 4-4, wherein the heating plate 4-4 is sleeved on the inner wall of the sealed cavity, the ceramic block 4-1, the oxygen scavenger 4-2 and the hydrogen scavenger 4-3 are all positioned in a space surrounded by the heating plate 4-4, the oxygen scavenger 4-2 and the hydrogen scavenger 4-3 are of a layered structure, the ceramic block 4-1 is used for isolating each layer of the oxygen scavenger 4-2 and the hydrogen scavenger 4-3, the oxygen scavenger 4-2 is magnesium metal or calcium metal, the hydrogen scavenger 4-3 is titanium sponge, the mass ratio of the oxygen scavenger 4-2 to the hydrogen scavenger 4-3 is 1.5-2.5:1, and during reaction, the mass of titanium hydride powder is not more than 30% of the mass of the hydrogen scavenger 4-3.
Specifically, the device comprises a No. two gas cooler 5 arranged between the gas purifier 4 and the gas heater 6, inert gas is provided for the loop through the inert gas source after vacuumizing, so that the pressure in the loop is 0.12-0.15 MPa, and the inert gas is cooled to below 30 ℃ by the No. two gas cooler 5 after being purified by the gas purifier 4 and circulates in the loop for at least 30min.
Compared with the prior art, the invention has the beneficial effects that:
the positive pressure reaction device for dehydrogenating the titanium hydride powder can heat the titanium hydride powder by using the inert gas as a carrier, can bring hydrogen generated by dehydrogenation out of a reaction tank while creating a positive pressure atmosphere to prevent external air from penetrating, is beneficial to the decomposition and dehydrogenation of the titanium hydride powder, and can recycle the inert gas and remove hydrogen and oxygen contained in the inert gas by using a dehydrogenation agent and an deoxidizer, thereby reducing gas consumption and improving the purity of a product while ensuring thorough dehydrogenation of the titanium hydride.
Drawings
FIG. 1 is a schematic diagram of a positive pressure reaction apparatus for dehydrogenation of titanium hydride powder according to the present invention;
FIG. 2 is a schematic diagram of the reaction tank structure of the positive pressure reaction device for dehydrogenating titanium hydride powder;
FIG. 3 is a schematic diagram of the gas purifier of the positive pressure reaction device for dehydrogenating titanium hydride powder;
FIG. 4 is a titanium powder XRD pattern obtained by the positive pressure dehydrogenation process for dehydrogenation of titanium hydride powder provided in examples 2, 3 and 4;
legend description: 1 is a reaction tank, 2 is a first gas cooler, 3 is a gas circulation pump, 4 is a gas purifier, 5 is a second gas cooler, 6 is a gas heater, 7 is a spraying device, 8 is a movable insulating sleeve, 9 is a first valve, 10 is a second valve, 1-1 is a water-cooling sealing flange, 1-2 is a sealing cover, 1-3 is an air inlet pipe, 1-4 is an air outlet pipe, 1-5 is a pressure air release valve, 1-6 is a dust-proof air-permeable screen, 1-7 is a material bed, 4-1 is a ceramic block, 4-2 is an deoxidizer, 4-3 is a dehydrogenation agent, and 4-4 is a heating plate.
Detailed Description
The following description of the embodiments of the present invention will be made in further detail with reference to the accompanying drawings and specific examples.
As shown in fig. 1, the embodiment of the invention provides a positive pressure reaction device for dehydrogenating titanium hydride powder, which comprises a reaction tank 1, a first gas cooler 2, a gas circulating pump 3, a gas purifier 4, a gas heater 6, a movable insulation sleeve 8, an inert gas source and a vacuumizing system, wherein the first gas cooler 2, the gas circulating pump 3, the gas purifier 4 and the gas heater 6 are sequentially connected through pipelines, the input end of the first gas cooler 2 is connected with an air outlet pipe 1-4 of the reaction tank 1, the output end of the gas heater 6 is connected with an air inlet pipe 1-3 of the reaction tank 1 to form a loop, as shown in fig. 2, a dust-proof air-permeable screen 1-6 is arranged in the reaction tank 1, the dust-proof air-permeable screen 1-6 divides the inner cavity of the reaction tank 1 into a first cavity and a second cavity, the air outlet pipe 1-4 is positioned in the first cavity, the air inlet pipe 1-3 is positioned in the second cavity, the air inlet pipe 1-3 extends to the end far away from the dust-proof air-permeable screen 1-6 in the second cavity to be close to the end part of the reaction tank 1, the movable heat preservation sleeve 8 is used for preserving heat of the second cavity area during reaction dehydrogenation, when titanium hydride powder is dehydrogenated, the vacuum pumping system is firstly used for vacuumizing the loop, then the vacuum pumping system is closed, inert gas is provided for the loop through the inert gas source, after the inert gas is purified by the gas purifier 4, the inert gas is heated to 750-800 ℃ by the gas heater 6 and then enters the reaction tank 1, the titanium hydride powder in the reaction tank 1 is heated, so that the titanium hydride powder is decomposed to release hydrogen, the inert gas brings generated hydrogen out of the reaction tank 1 under the action of the gas circulation pump 3, dust carried by the inert gas is trapped in the second cavity after passing through the dust-separation ventilation screen 1-6, the inert gas carrying the hydrogen is cooled by the first gas cooler 2 and enters the gas purifier 4, and the gas purifier 4 removes oxygen and hydrogen in the inert gas.
The traditional dehydrogenation method of titanium hydride powder is to heat a reaction tank by means of an electric furnace outside the reaction tank to promote the decomposition of the titanium hydride powder in the reaction tank to generate hydrogen, and then to suck air from the reaction tank by a vacuum pump and discharge the hydrogen to obtain the titanium powder. The process is that the reaction tank is heated from outside to inside, the reaction tank is heated to a higher temperature of 650-850 ℃, and the reaction tank is vacuumized at the same time, so that the internal dehydrogenation process of the tank is always in a negative pressure state, and the high temperature and the negative pressure act simultaneously, so that the tank body is extremely easy to cause the condition that external air permeates into the tank and then reacts with titanium powder in the tank, and the oxygen and nitrogen content of a dehydrogenation product is higher.
According to the positive pressure reaction device for dehydrogenating the titanium hydride powder, provided by the embodiment of the invention, the heated inert gas is used for directly heating the titanium hydride, so that the possibility of permeation of external gas into the tank is completely eliminated, the tank body temperature is prevented from being too high, gas replacement and powder dehydrogenation are all the time in the inert gas protection of the equipment loop, and the pressure in the tank is higher than the external atmospheric pressure and is more than or equal to 0.15MPa and less than or equal to P and less than 1.5 MPa.
Before heating and dehydrogenating titanium hydride powder by using inert gas as a heating medium, the inert gas firstly passes through a gas purifier 4 and is purified in advance by means of an internal deoxidizer 4-2 and a deoxidizer 4-3, so that the pollution of the gas source purity to the titanium hydride and the dehydrogenated titanium powder is completely avoided; because the temperature difference required by the dehydrogenation of the titanium hydride powder and the purification of the inert gas is large, the device is provided with the independent first gas cooler 2 and the independent gas heater 6 between the reaction tank 1 and the gas purifier 4, so that the inert gas is ensured to have different temperatures at the positions of the reaction tank 1 and the gas purifier 4 in a device loop, and the dehydrogenation of the titanium hydride and the removal of impurity gas are facilitated.
Further, the positive pressure reaction device for dehydrogenating titanium hydride powder further comprises a second gas cooler 5 arranged between the gas purifier 4 and the gas heater 6, wherein after vacuumizing, inert gas is provided for the loop through the inert gas source, and after being purified by the gas purifier 4, the inert gas is cooled to below 30 ℃ by the second gas cooler 5 and circulates in the loop for at least 30min.
The method adopts inert gas to repeatedly purify the gas in the system before heating the titanium hydride powder, and further eliminates the pollution caused by vacuum residual trace air and inert gas impurities. The inert gas passing through the gas purifier 4 is fully cooled to below 30 ℃ by the second gas cooler 5, and then is introduced into the reaction tank 1, so that the problem that titanium hydride powder is polluted by residual unpurified inert gas in the tank caused by heating titanium hydride powder by high-temperature gas can be avoided, when the inert gas circulates in the loop for more than 30min, all inert gas in the loop is ensured to be purified, residual air is completely removed, impurities such as oxygen and nitrogen are not existed in the inert gas in the loop, and the pollution of the impurities to titanium hydride and the dehydrogenated titanium powder is avoided.
Specifically, as shown in fig. 3, the gas purifier 4 includes a sealed cavity, a ceramic block 4-1, an oxygen scavenger 4-2, a hydrogen scavenger 4-3 and a heating plate 4-4, the heating plate 4-4 is sleeved on the inner wall of the sealed cavity, the ceramic block 4-1, the oxygen scavenger 4-2 and the hydrogen scavenger 4-3 are all located in a space surrounded by the heating plate 4-4, the oxygen scavenger 4-2 and the hydrogen scavenger 4-3 are both in a layered structure, the ceramic block 4-1 is used for isolating each layer of the oxygen scavenger 4-2 and the hydrogen scavenger 4-3, the oxygen scavenger 4-2 is magnesium metal or calcium metal, the hydrogen scavenger 4-3 is titanium sponge, the ceramic block 4-1 is aluminum oxide or zirconium oxide, and the heating plate 4-4 is used for maintaining the temperature in the sealed cavity at 270-330 ℃.
The sealing cavity makes the external gas unable to enter the gas purifier 4, and ensures that the hydrogen remover 4-2 and the deoxidizer 4-3 in the gas purifier 4 are not polluted by external impurities, and are all used for purifying the gas in the device. The deoxidizer 4-2 and the dehydrogenation agent 4-3 are of a layered structure, and the ceramic block 4-1 is used for isolating the deoxidizer 4-2 and the dehydrogenation agent 4-3 of each layer, so that inert gas containing impurities can fully contact with the deoxidizer 4-2 and the dehydrogenation agent 4-3 when flowing through the gas purifier, and the ceramic block 4-1 does not chemically react with the deoxidizer 4-2 and the dehydrogenation agent 4-3, so that the deoxidizer 4-2 and the dehydrogenation agent 4-3 are not polluted by substances except impurity gas. The ceramic block 4-1, the deoxidizer 4-2 and the dehydrogenation agent 4-3 are all positioned in the space surrounded by the heating plate 4-4, so that the temperature in the gas purifier 4 is uniform, the gas purifying efficiency is high, the temperature in the cavity is 270-330 ℃, the deoxidizer 4-2 and the dehydrogenation agent 4-3 can absorb impurity gas in inert gas with maximum efficiency, and the gas purifying efficiency is improved.
In an alternative embodiment, the mass ratio of oxygen scavenger 4-2 to hydrogen scavenger 4-3 is 1.5-2.5:1.
The mass ratio is to ensure that the deoxidizer and the deoxidizer are in an absolute excess state relative to the titanium hydride powder in a powder state, and the absolute substance excess state can fully ensure that the gas purifier 4 can fully absorb impurities in inert gas and hydrogen carried by the impurities, although the specific surface area of the deoxidizer and the deoxidizer is smaller than that of the titanium hydride powder due to the layered structure.
In an alternative embodiment, a pressure relief valve 1-5 is arranged on the shell of the first cavity of the reaction tank 1, and the pressure relief valve 1-5 automatically vents and reduces pressure when the pressure in the reaction tank 1 is greater than 1.5 MPa.
In order to ensure that external gas cannot enter the device in the dehydrogenation process, the reaction device is filled with inert gas in a cold state and is in a state higher than external atmospheric pressure, the temperature of the inert gas is about 0.12-0.15 MPa, the pressure in the device can be increased along with the temperature increase of the inert gas after the dehydrogenation reaction is started, and the pressure relief valve 1-5 in the first cavity in the reaction tank can automatically exhaust and relieve pressure under the condition that the pressure in the device is higher than 1.5MPa, so that the reaction speed is reduced due to overhigh pressure in the tank in the dehydrogenation decomposition process of titanium hydride, the safety of equipment in the dehydrogenation process is ensured, and danger caused by overhigh internal pressure is avoided.
The pressure air release valve 1-5 is positioned in the first cavity, so that the pressure in the reaction tank 1 can be accurately measured, and meanwhile, the possibility of dust blockage of the pressure air release valve is effectively avoided due to the existence of the dust-proof air-permeable screen 1-6, and the working reliability of the pressure air release valve is improved.
Further, the positive pressure reaction device for dehydrogenating the titanium hydride powder further comprises a spraying device 7 for cooling the reaction tank 1 after the reaction is finished.
The device can cool down the reaction tank in a mode of spraying cooling water after the reaction is finished, and the interior of the sprayed reaction tank is still in a positive pressure state due to the fact that inert gas of 0.15MPa is filled in advance, so that the cooling efficiency is improved, and the infiltration of external air is avoided.
In an alternative embodiment, the dust-proof air-permeable screen 1-6 comprises a plurality of porous metal plates, gaps are arranged among the metal plates, the aperture on the metal plates decreases progressively along the direction from the second cavity to the first cavity, the maximum aperture is 3-5 mm, and the minimum aperture is 0.3-0.5 mm.
The device can divide the retort into a first cavity and a second cavity, and the inert gas flow introduced into the bottom of the second cavity by the air inlet pipe 1-3 can cause powder to lift up because of blowing of the air flow in the process of heating titanium hydride powder placed in the second cavity, and a small amount of powder can be taken away along with the air flow, so that risks of blocking a loop, wearing equipment and polluting a gas purifier are brought, and the porous metal plate of the dust-separation ventilation screen 1-6 can intercept dust with different particle sizes wrapped in the air flow layer by changing the aperture under the premise of ensuring smooth passing of the air flow, so that the possibility of dust escape in the retort 1 is completely eliminated.
The embodiment of the invention also provides a positive pressure dehydrogenation method for dehydrogenating the titanium hydride powder, which uses the positive pressure reaction device to dehydrogenate the titanium hydride powder. The positive pressure reaction device is provided by the device embodiment, and the specific description and effects refer to the embodiment, so that the invention is not limited.
Specifically, as shown in fig. 3, the gas purifier 4 includes a sealed cavity, a ceramic block 4-1, an oxygen scavenger 4-2, a hydrogen scavenger 4-3 and a heating plate 4-4, the heating plate 4-4 is sleeved on the inner wall of the sealed cavity, the ceramic block 4-1, the oxygen scavenger 4-2 and the hydrogen scavenger 4-3 are all located in a space surrounded by the heating plate 4-4, the oxygen scavenger 4-2 and the hydrogen scavenger 4-3 are both in a layered structure, the ceramic block 4-1 is used for isolating each layer of the oxygen scavenger 4-2 and the hydrogen scavenger 4-3, the oxygen scavenger 4-2 is magnesium metal or calcium metal, the hydrogen scavenger 4-3 is titanium sponge, the mass ratio of the oxygen scavenger 4-2 to the hydrogen scavenger 4-3 is 1.5-2.5:1, and the mass of titanium hydride powder is not more than 30% of the mass of the hydrogen scavenger 4-3 during the reaction.
When titanium hydride powder is added according to the proportion, on the premise that the specific surface area of the titanium hydride powder is far larger than that of the hydrogen removing agent, hydrogen removed by the titanium hydride powder can be completely absorbed by the excessive hydrogen removing agent in the gas purifier 4, and inert gas discharged from the top does not contain hydrogen, so that the dehydrogenation reaction of titanium hydride is positively carried out when the titanium hydride powder is heated.
Specifically, the device comprises a No. two gas cooler 5 arranged between the gas purifier 4 and the gas heater 6, inert gas is provided for the loop through the inert gas source after vacuumizing, so that the pressure in the loop is 0.12-0.15 MPa, and the inert gas is cooled to below 30 ℃ by the No. two gas cooler 5 after being purified by the gas purifier 4 and circulates in the loop for at least 30min.
The inert gas provided by the inert gas source is heated to 270-330 ℃ in the purifying process of the gas purifier 4, and if the inert gas is directly introduced into the reaction tank 1, the inert gas which is not purified in the tank and the titanium hydride powder are heated, and the inert gas and the titanium hydride powder react to cause the titanium hydride powder to be polluted. After the purified high-temperature inert gas is cooled to below 30 ℃ by a second cooler 5, the heat influence of the purified high-temperature inert gas on the raw gas and the titanium hydride in the reaction tank 1 is eliminated, the titanium hydride powder is not polluted, the inert gas and the residual air in the tank fully react with a gas purifier (4) after the inert gas circulates in a loop for 30min, and the inert gas in the loop is not polluted on the titanium hydride powder.
Example 1:
as shown in fig. 1, the present embodiment provides a positive pressure reaction device for dehydrogenation of titanium hydride powder, which comprises a reaction tank 1, a first gas cooler 2, a gas circulation pump 3, a gas purifier 4, a second gas cooler 5, a gas heater 6, a spraying device 7 and a movable thermal insulation sleeve 8. In this embodiment, as shown in fig. 2, the structure of the reaction tank 1 is a stainless steel pressure-bearing container with an opening at the head end and a closed tail end, the stainless steel pressure-bearing container is divided into a high-temperature section and a low-temperature section according to the coating area of the reaction tank by the movable insulation sleeve 8, the opening side of the reaction tank 1 is the low-temperature section, the closed side is the high-temperature section, the movable insulation sleeve 8 can be sleeved on the high-temperature section or removed from the high-temperature section according to the requirement, a water-cooling sealing flange 1-1 is arranged at the opening of the reaction tank 1 and can be matched with the sealing cover 1-2 to seal the reaction tank 1, the low-temperature section of the reaction tank is connected with an air inlet pipe 1-3, an air outlet pipe 1-4 and a pressure relief valve 1-5, the pressure relief valve 1-5 is automatically exhausted and depressurized when the pressure in the reaction tank 1-1 is higher than 1.5MPa, the air inlet pipe 1-3 penetrates the tank wall and then extends from the tank to the tail end of the reaction tank 1, a dust-proof air-permeable screen 1-6 is arranged in the reaction tank 1, the air outlet pipe 1-4 port and the pressure relief valve 1-5 port is isolated on the opening side of the reaction tank 1, and the air inlet pipe 1-3 port is isolated on the closed side of the reaction tank 1.
In this embodiment, the structure of the gas purifier 4 is shown in fig. 3, and is a heat-sealable cavity with bottom gas inlet and top gas outlet, and the cavity is internally stacked with an oxygen scavenger 4-2 and a hydrogen scavenger 4-3 separated by a ceramic block 4-1, wherein the oxygen scavenger 4-2 is magnesium metal or calcium metal, the hydrogen scavenger 4-3 is titanium sponge, the mass ratio of the oxygen scavenger 4-2 to the hydrogen scavenger 4-3 is 2:1, and the inner wall of the cavity is provided with a heating plate 4-4, so that the oxygen scavenger 4-2 and the hydrogen scavenger 4-3 can be heated.
In this embodiment, the first gas cooler 2, the gas circulation pump 3, the gas purifier 4, the second gas cooler 5 and the gas heater 6 are sequentially connected through pipelines, the input end of the first gas cooler 2 is connected with the gas outlet pipe 1-4 of the reaction tank 1, the output end of the gas heater 6 is connected with the gas inlet pipe 1-3 of the reaction tank 1, a three-way pipe is arranged between the gas purifier 4 and the second gas cooler 5, the third end of the three-way pipe is connected with the vacuumizing system through the first valve 9, a three-way pipe is also arranged between the gas circulation pump 3 and the gas purifier 4, and the third section of the three-way pipe is connected with a high-purity inert gas source through the second valve 10.
Example 2:
the positive pressure dehydrogenation method for dehydrogenating titanium hydride powder provided in this example uses the positive pressure reaction device for dehydrogenating titanium hydride powder described in example 1, and comprises the following steps:
step (1) feeding and gas replacement:
placing titanium hydride powder accounting for 25% of the mass of a dehydrogenation agent into a material bed 1-7 at a high temperature section of a reaction tank, closing a sealing cover 1-2, starting cooling water circulation of a water-cooling sealing flange 1-1, and sleeving a movable heat preservation sleeve at the high temperature section of the reaction tank; opening a first valve 9 to vacuumize the device, closing the first valve 9 after the vacuum degree of the device reaches 0.5Pa, opening a second valve 10 to introduce argon with the purity of 99.5wt%, and closing the second valve 10 after the device is boosted to 0.12 MPa; repeating the operations of vacuumizing and argon introducing for 10 times, finally filling argon with the purity of 99.8 weight percent to ensure that the pressure in the reaction tank reaches 0.15MPa, and closing a valve number one 9 and a valve number two 10;
step (2) purifying the gas inside the device
The gas circulation pump 3, the gas purifier 4 and the second gas cooler 5 are started in sequence, the metal magnesium and the titanium sponge are heated to 300 ℃ by the heating plate 4-4 in the gas purifier, argon in the device enters the gas purifier 4 from the bottom under the pushing of the gas circulation pump 3, fully contacts with the metal magnesium and the titanium sponge, is discharged from the top, and the purified argon is cooled to 27 ℃ by the second gas cooler 5 for 35 minutes, so that the gas in the device is completely purified;
step (3) dehydrogenation of titanium hydride powder
Closing a second gas cooler 5, starting a first gas cooler 2 and a gas heater 6, heating the argon completely purified by the gas purifier to 770 ℃ by the gas heater 6, introducing the argon into a high-temperature section at the bottom of the reaction tank 1 through an air inlet pipe 1-3, contacting the high-temperature argon with titanium hydride powder, decomposing and dehydrogenating the titanium hydride powder, mixing the removed hydrogen with the argon, discharging the mixed gas through an air outlet pipe 1-4, and blocking the powder carried by the air flow by a dust-proof and air-permeable screen;
step (4) cooling and purifying the hydrogen-argon mixture
The argon mixed with hydrogen is discharged from an air outlet pipe 1-4, cooled to 255 ℃ by a first gas cooler 2, sent into a gas purifier 4 by a gas circulating pump 3, absorbed by titanium sponge and discharged to obtain pure argon;
finishing the dehydrogenation of the titanium hydride powder in the step (5)
The pure argon discharged from the gas purifier is heated to 770 ℃ again through the gas heater, and is introduced into the reaction tank to continuously dehydrogenate the titanium hydride powder for 8 hours;
step (6) device and dehydrogenated titanium powder cooling
After dehydrogenation is finished, stopping the operation of the gas heater 6 and the heating plate 4-4 in the gas purifier 4, moving the heat preservation sleeve 8 away from the high-temperature section of the reaction tank, starting the spraying device 7 to spray water to cool the outer wall of the reaction tank 1, starting the second gas cooler 5 to cool argon in an enhanced manner while maintaining the operation of the first gas cooler 2 and the gas circulating pump 3, introducing cooled argon into the reaction tank 1, and cooling the dehydrogenated titanium powder until the reaction tank and the titanium powder are cooled to 25 ℃.
Phase composition of powder obtained by D/MAX-2250 type X-ray diffractometer, copper target K α The diffraction angle range is 20-80 degrees, the scanning step length is 0.02 degrees, the standard PDF card standard phase composition in the database is compared by using JADE software, the result is shown in figure 4, the titanium hydride is completely dehydrogenated and decomposed, the product is pure titanium powder, and the oxygen content of the titanium powder is 490ppm by using a LECO TCH-600 nitrogen-oxygen-hydrogen analyzer.
Example 3:
the positive pressure dehydrogenation method for dehydrogenating titanium hydride powder provided in this example uses the positive pressure reaction device for dehydrogenating titanium hydride powder described in example 1, and comprises the following steps:
step (1) charging and gas displacement
Placing titanium hydride powder accounting for 23% of the mass of a dehydrogenation agent into a material bed at a high temperature section of a reaction tank, closing a sealing cover, starting cooling water circulation of a water-cooling sealing flange, and sleeving a movable heat preservation sleeve at the high temperature section of the reaction tank; opening a first valve to vacuumize the device, closing the first valve after the vacuum degree of the device reaches 0.15Pa, opening a second valve to introduce helium with the purity of 99.3wt%, and closing the second valve after the device is boosted to 0.12 MPa; repeating the operations of vacuumizing and introducing helium for 10 times, and finally filling helium with the purity of 99.7wt% to ensure that the pressure in the reaction tank reaches 0.15MPa, and closing a valve I and a valve II;
step (2) purifying the gas inside the device
Sequentially starting a gas circulation pump, a gas purifier and a second gas cooler, wherein a heating plate in the gas purifier heats metal calcium and titanium sponge to 310 ℃, helium in the device enters the gas purifier from the bottom under the pushing of the gas circulation pump, fully contacts with the metal calcium and the titanium sponge, is discharged from the top, and then cools the purified helium to 25 ℃ through the second gas cooler for 40 minutes, so that the gas in the device is completely purified;
step (3) dehydrogenation of titanium hydride powder
Closing a second gas cooler, starting a first gas cooler and a gas heater, heating the helium completely purified by the gas purifier to 790 ℃ by the gas heater, introducing the helium into a high-temperature section at the bottom of the reaction tank through an air inlet pipe, enabling the high-temperature helium to contact with titanium hydride powder, decomposing and dehydrogenating the titanium hydride powder, mixing the removed hydrogen and helium, discharging the hydrogen and helium through an air outlet pipe, and blocking the powder carried by the air flow by a dust-proof and air-permeable screen;
step (4) cooling and purifying the hydrogen-mixed helium gas
After the helium mixed with hydrogen is discharged from an air outlet pipe, the helium is cooled to 245 ℃ by a first gas cooler, and then is pumped into a gas purifier by a gas circulating pump, the hydrogen mixed with the helium is absorbed by titanium sponge, and pure helium is discharged;
finishing the dehydrogenation of the titanium hydride powder in the step (5)
The pure helium gas discharged from the gas purifier is heated to 790 ℃ again through the gas heater, and is introduced into the reaction tank to continuously dehydrogenate the titanium hydride powder for 6 hours;
step (6) device and dehydrogenated titanium powder cooling
After dehydrogenation is finished, stopping the operation of a heating plate in the gas heater and the gas purifier, moving the heat preservation sleeve away from the high-temperature section of the reaction tank, starting the spraying device to spray water to cool the outer wall of the reaction tank, maintaining the operation of the first gas cooler and the gas circulating pump, starting the second gas cooler to cool the helium in an enhanced mode, introducing the cooled helium into the reaction tank, and cooling the dehydrogenated titanium powder until the reaction tank and the titanium powder are cooled to 23 ℃.
Phase composition of powder obtained by D/MAX-2250 type X-ray diffractometer, copper target K α The diffraction angle range is 20-80 degrees, the scanning step length is 0.02 degrees, the standard PDF card standard phase composition in the database is compared by using JADE software, the result is shown in figure 4, the titanium hydride is completely dehydrogenated and decomposed, the product is pure titanium powder, and the oxygen content of the titanium powder is 550ppm by using a LECO TCH-600 nitrogen oxygen hydrogen analyzer.
Example 4:
the positive pressure dehydrogenation method for dehydrogenating titanium hydride powder provided in this example uses the positive pressure reaction device for dehydrogenating titanium hydride powder described in example 1, and comprises the following steps:
step (1) charging and gas displacement
Placing titanium hydride powder accounting for 20% of the mass of a dehydrogenation agent into a material bed at a high temperature section of a reaction tank, closing a sealing cover, starting cooling water circulation of a water-cooling sealing flange, and sleeving a movable heat preservation sleeve at the high temperature section of the reaction tank; opening a first valve to vacuumize the device, closing the first valve after the vacuum degree of the device reaches 0.1Pa, opening a second valve to introduce argon with the purity of 99.3wt%, and closing the second valve after the device is boosted to 0.12 MPa; repeating the operations of vacuumizing and argon introducing for 10 times, finally filling argon with the purity of 99.5wt% to ensure that the pressure in the reaction tank reaches 0.15MPa, and closing a valve I and a valve II;
step (2) purifying the gas inside the device
Sequentially starting a gas circulation pump, a gas purifier and a second gas cooler, wherein a heating plate in the gas purifier heats metal magnesium and titanium sponge to 330 ℃, argon in the device enters the gas purifier from the bottom under the pushing of the gas circulation pump, fully contacts with the metal magnesium and the titanium sponge, is discharged from the top, and then cools the purified argon to 24 ℃ through the second gas cooler, and the operation is continued for 50 minutes, so that the gas in the device is completely purified;
step (3) dehydrogenation of titanium hydride powder
Closing a second gas cooler, starting a first gas cooler and a gas heater, heating the argon completely purified by the gas purifier to 790 ℃ by the gas heater, introducing the argon into a high-temperature section at the bottom of the reaction tank through an air inlet pipe, enabling the high-temperature argon to contact with titanium hydride powder, decomposing and dehydrogenating the titanium hydride powder, mixing the removed hydrogen and the argon, discharging the hydrogen and the argon through an air outlet pipe, and blocking the powder carried by the air flow by a dust-proof and air-permeable screen;
step (4) cooling and purifying the hydrogen-argon mixture
After being discharged from an air outlet pipe, the argon mixed with the hydrogen is cooled to 285 ℃ by a first gas cooler, and then is pumped into a gas purifier by a gas circulating pump, the hydrogen mixed with the argon is absorbed by the titanium sponge, and pure argon is discharged;
finishing the dehydrogenation of the titanium hydride powder in the step (5)
The pure argon discharged from the gas purifier is heated to 790 ℃ again through the gas heater, and is introduced into the reaction tank to continuously dehydrogenate the titanium hydride powder for 7 hours;
step (6) device and dehydrogenated titanium powder cooling
After dehydrogenation is finished, stopping the operation of a heating plate in the gas heater and the gas purifier, moving the heat preservation sleeve away from the high-temperature section of the reaction tank, starting the spraying device to spray water to cool the outer wall of the reaction tank, maintaining the operation of the first gas cooler and the gas circulating pump, starting the second gas cooler to cool argon in an enhanced mode, introducing the cooled argon into the reaction tank, and cooling the dehydrogenated titanium powder until the reaction tank and the titanium powder are cooled to 28 ℃.
Phase composition of powder obtained by D/MAX-2250 type X-ray diffractometer, copper target K α The diffraction angle range is 20-80 degrees, the scanning step length is 0.02 degrees, the standard PDF card standard phase composition in the database is compared by using JADE software, the result is shown in figure 4, the titanium hydride is completely dehydrogenated and decomposed, the product is pure titanium powder, and the oxygen content of the titanium powder is measured to be 520ppm by using a LECO TCH-600 nitrogen oxygen hydrogen analyzer.
The foregoing is merely one specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions easily contemplated by those skilled in the art within the technical scope of the present invention should be included in the scope of the present invention.
The non-detailed description of the invention is within the knowledge of a person skilled in the art.
Claims (8)
1. The positive pressure reaction device for dehydrogenating titanium hydride powder is characterized by comprising a reaction tank (1), a first gas cooler (2), a gas circulation pump (3), a gas purifier (4), a gas heater (6), a movable heat preservation sleeve (8), an inert gas source and a vacuumizing system, wherein the first gas cooler (2), the gas circulation pump (3), the gas purifier (4) and the gas heater (6) are sequentially connected through pipelines, the input end of the first gas cooler (2) is connected with an air outlet pipe (1-4) of the reaction tank (1), the output end of the gas heater (6) is connected with an air inlet pipe (1-3) of the reaction tank (1) to form a loop, a dust-separation and air-permeable screen (1-6) is arranged in the reaction tank (1), the inner cavity of the reaction tank (1) is divided into a first cavity and a second cavity, the air outlet pipe (1-4) is positioned in the first cavity, the second cavity is positioned in the air inlet pipe (1-3), and extends to the second cavity (1-3) to the heat preservation sleeve when the first cavity is far away from the first end of the reaction tank (1-8), when titanium hydride powder is dehydrogenated, firstly vacuumizing the loop through the vacuumizing system, then closing the vacuumizing system, providing inert gas for the loop through the inert gas source, purifying the inert gas through the gas purifier (4), heating the inert gas to 750-800 ℃ by the gas heater (6), then entering the reaction tank (1), heating the titanium hydride powder in the reaction tank (1) so as to decompose the titanium hydride powder and release hydrogen, taking the generated hydrogen out of the reaction tank (1) by the inert gas under the action of the gas circulating pump (3), intercepting dust carried by the inert gas in the second cavity after passing through the dust-isolating and ventilation screen (1-6), cooling the inert gas carrying the hydrogen through the first gas cooler (2), and then entering the gas purifier (4), wherein the gas purifier (4) removes oxygen and hydrogen in the inert gas;
the vacuum-pumping device is characterized by further comprising a second gas cooler (5) arranged between the gas purifier (4) and the gas heater (6), wherein after the vacuum-pumping device is used for vacuumizing, inert gas is provided for the loop through the inert gas source, and after the inert gas is purified by the gas purifier (4), the inert gas is cooled to below 30 ℃ by the second gas cooler (5) and circulates in the loop for at least 30min.
2. The positive pressure reaction device for dehydrogenating titanium hydride powder according to claim 1, wherein the gas purifier (4) comprises a sealed cavity, a ceramic block (4-1), a deoxidizer (4-2), a hydrogen removing agent (4-3) and a heating plate (4-4), wherein the heating plate (4-4) is sleeved on the inner wall of the sealed cavity, the ceramic block (4-1), the deoxidizer (4-2) and the hydrogen removing agent (4-3) are all located in a space surrounded by the heating plate (4-4), the deoxidizer (4-2) and the hydrogen removing agent (4-3) are of a layered structure, the ceramic block (4-1) is used for isolating each layer of the deoxidizer (4-2) and the hydrogen removing agent (4-3), the deoxidizer (4-2) is magnesium metal or calcium metal, the hydrogen removing agent (4-3) is titanium sponge, the ceramic block (4-1) is aluminum oxide or zirconium oxide, and the ceramic block (4-1) is used for maintaining the temperature of the heating plate (4-4) in the sealed cavity at 330 ℃.
3. The positive pressure reaction device for dehydrogenation of titanium hydride powder according to claim 2, wherein the mass ratio of the oxygen scavenger (4-2) to the hydrogen scavenger (4-3) is (1.5-2.5): 1.
4. The positive pressure reaction device for dehydrogenation of titanium hydride powder according to claim 1 is characterized in that a pressure relief valve (1-5) is arranged on a shell of a first cavity of the reaction tank (1), and the pressure relief valve (1-5) automatically vents and reduces pressure when the pressure in the reaction tank (1) is higher than 1.5 MPa.
5. Positive pressure reaction device for the dehydrogenation of titanium hydride powder according to claim 1, characterized by further comprising spraying means (7) for cooling the reaction tank (1) after the end of the reaction.
6. The positive pressure reaction apparatus for dehydrogenation of titanium hydride powder according to claim 1, characterized in that the dust-proof and gas-permeable screen (1-6) comprises a plurality of porous metal plates having gaps therebetween, and the pore diameter on the metal plates decreases in the direction from the second chamber to the first chamber, with a maximum pore diameter of 3-5 mm and a minimum pore diameter of 0.3-0.5 mm.
7. A positive pressure dehydrogenation process for dehydrogenating titanium hydride powder, characterized by: use of the positive pressure reaction apparatus of any one of claims 1 to 6 for dehydrogenation of titanium hydride powder;
the gas purifier (4) comprises a sealing cavity, a ceramic block (4-1), an oxygen scavenger (4-2), a hydrogen scavenger (4-3) and a heating plate (4-4), wherein the heating plate (4-4) is sleeved on the inner wall of the sealing cavity, the ceramic block (4-1), the oxygen scavenger (4-2) and the hydrogen scavenger (4-3) are all located in a space surrounded by the heating plate (4-4), the oxygen scavenger (4-2) and the hydrogen scavenger (4-3) are of a layered structure, the ceramic block (4-1) is used for separating the oxygen scavenger (4-2) and the hydrogen scavenger (4-3) from each layer, the oxygen scavenger (4-2) is metal magnesium or metal calcium, the hydrogen scavenger (4-3) is sponge titanium, and the mass ratio of the oxygen scavenger (4-2) to the hydrogen scavenger (4-3) is (1.5-2.5): 1, and the mass of the hydrogen scavenger (4-3) is not more than 30% of the mass of the hydrogenated titanium powder during the reaction.
8. The positive pressure dehydrogenation process for the dehydrogenation of titanium hydride powder according to claim 7, characterized in that: the device comprises a second gas cooler (5) arranged between the gas purifier (4) and the gas heater (6), wherein after vacuumizing, inert gas is provided for the loop through an inert gas source, so that the pressure in the loop is 0.12-0.15 MPa, and after being purified by the gas purifier (4), the inert gas is cooled to below 30 ℃ by the second gas cooler (5) and circulates in the loop for at least 30min.
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