CN113373305B - Titanium sponge production reactor - Google Patents
Titanium sponge production reactor Download PDFInfo
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- CN113373305B CN113373305B CN202110779372.9A CN202110779372A CN113373305B CN 113373305 B CN113373305 B CN 113373305B CN 202110779372 A CN202110779372 A CN 202110779372A CN 113373305 B CN113373305 B CN 113373305B
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- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 29
- 239000007788 liquid Substances 0.000 claims abstract description 22
- 239000000463 material Substances 0.000 claims abstract description 20
- 238000005507 spraying Methods 0.000 claims abstract description 7
- 239000010936 titanium Substances 0.000 claims description 11
- 229910052719 titanium Inorganic materials 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 abstract description 45
- 230000017525 heat dissipation Effects 0.000 abstract description 17
- 229910003074 TiCl4 Inorganic materials 0.000 description 20
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 13
- 239000011777 magnesium Substances 0.000 description 12
- 238000000034 method Methods 0.000 description 12
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 8
- 229910052749 magnesium Inorganic materials 0.000 description 8
- 238000006722 reduction reaction Methods 0.000 description 8
- 239000000243 solution Substances 0.000 description 7
- 230000009467 reduction Effects 0.000 description 6
- 238000003723 Smelting Methods 0.000 description 5
- 239000012295 chemical reaction liquid Substances 0.000 description 5
- 238000001816 cooling Methods 0.000 description 5
- 229910001069 Ti alloy Inorganic materials 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 238000007599 discharging Methods 0.000 description 4
- 238000011049 filling Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 239000007921 spray Substances 0.000 description 4
- 238000007664 blowing Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 239000002826 coolant Substances 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L magnesium chloride Substances [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 2
- 229910001629 magnesium chloride Inorganic materials 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000004408 titanium dioxide Substances 0.000 description 2
- 238000005292 vacuum distillation Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- WYTGDNHDOZPMIW-RCBQFDQVSA-N alstonine Natural products C1=CC2=C3C=CC=CC3=NC2=C2N1C[C@H]1[C@H](C)OC=C(C(=O)OC)[C@H]1C2 WYTGDNHDOZPMIW-RCBQFDQVSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000005056 compaction Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000014509 gene expression Effects 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B5/00—General methods of reducing to metals
- C22B5/02—Dry methods smelting of sulfides or formation of mattes
- C22B5/04—Dry methods smelting of sulfides or formation of mattes by aluminium, other metals or silicon
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/10—Obtaining titanium, zirconium or hafnium
- C22B34/12—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
- C22B34/1263—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining metallic titanium from titanium compounds, e.g. by reduction
- C22B34/1268—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining metallic titanium from titanium compounds, e.g. by reduction using alkali or alkaline-earth metals or amalgams
- C22B34/1272—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining metallic titanium from titanium compounds, e.g. by reduction using alkali or alkaline-earth metals or amalgams reduction of titanium halides, e.g. Kroll process
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention discloses a titanium sponge production reactor, which comprises a tank body, a feeding device and a flow guide device, wherein the flow guide device is arranged below the liquid level of the tank body; the flow guide device is provided with an upper surface gradually reduced from the center of the tank body to the periphery and a through hole superposed with the vertical center of the tank body; the feeding device is used for feeding materials by spraying. According to the titanium sponge production reactor provided by the invention, the diversion device is arranged, and the jet feeding of the jet device is combined, so that the materials in the reactor flow under the jet kinetic energy and the diversion of the diversion device, the heat dissipation capability of the reactor is improved, and meanwhile, due to the existence of the diversion device, the reaction area is closer to the inner wall of the reactor, the reaction heat can be dissipated from the inner wall more quickly, and the heat conduction capability of the reaction area is improved.
Description
Technical Field
The invention relates to the technical field of titanium sponge production, in particular to a titanium sponge production reactor.
Background
Titanium and titanium alloy have the characteristics of high specific strength, corrosion resistance, good high temperature resistance and the like, and have wide application in the fields of aerospace, deep sea exploration, chemical engineering, medical treatment and the like. Titanium sponge is used as a raw material for preparing titanium and titanium alloy, and is industrially prepared by a magnesium thermal method. Before the titanium sponge is subjected to vacuum consumable smelting, the titanium sponge needs to be pressed into a compact electrode, and when the electrode is not pressed tightly, accidents such as material falling and the like are easy to occur in the smelting process, so that the smelting is interrupted. In order to avoid the falling of the titanium sponge blocks in the smelting process, smelting enterprises continuously improve the working pressure of the press on the one hand and select titanium sponge with better porosity to press the electrodes on the other hand.
The preparation process of the titanium sponge is violent exothermic reaction, when the reaction heat can not be dissipated out of the reactor in time, the problem that the center of the titanium lump is compact in pore structure and the like can be caused, and the titanium sponge with the compact center is commonly called as a hard core in the titanium sponge industry. In order to solve the problem of 'hard core' of the titanium lump, various enterprises apply for a plurality of patents from the aspects of uniform release of reaction heat, forced heat dissipation of a reactor and the like. Uniformity of heat of reactionAnd releasing, wherein a multi-material-pipe dispersion method is generally adopted. For example, CN202786386U A feeding device for producing titanium sponge discloses TiCl4The feeding comprises a main pipe and feeding branch pipes, wherein titanium tetrachloride enters from the main pipe and is sprayed out from the feeding branch pipes, the number of the branch pipes is 2-6, the diameter and the length are the same, the included angle of each branch pipe is the same, and the included angle between each branch pipe and the main pipe is 100-160 degrees, so that the series problems caused by the higher central temperature of the reactor are solved; CN201553769U produces reduction reaction unit of titanium sponge, has proposed that evenly set up a plurality of feeding devices on the reacting furnace apron to stretch into the reacting furnace, in order to solve the reduction period and add the intensive and compact problem of titanium sponge structure that brings of material. CN206298627U has proposed to be equipped with the bulk cargo device at the lower extreme of filling tube, and the bulk cargo device passes through connecting rod and filling tube welded connection, is equipped with the umbelliform uniform material spare of back taper in the bulk cargo device to improve TiCl4The problem of uneven distribution.
For improving the heat dissipation capacity of the reaction vessel, methods such as forced air blowing of the tank wall, the tank cover and the addition of a cooling device in the center of the reactor are adopted to improve the heat dissipation capacity of the reaction vessel. For example, CN110760699A discloses a titanium lump central forced heat dissipation and vaporization feeding device for titanium sponge reduction production, which is implemented by gas-phase TiCl4Feeding while inserting the heat exchanger into the central part of the reactor to realize TiCl in the reactor4The heat dissipation capacity of the center of the reaction vessel is improved; CN201560227U discloses a reduction device in the process of producing titanium sponge by a magnesium method, wherein a heat dissipation part is arranged on a large cover of a reactor, and a cooling medium inlet and a cooling medium outlet are arranged on the heat dissipation part, so as to solve the problem of compact structure of the titanium sponge; CN208829744U discloses a reactor with a heat dissipation device in the production of titanium sponge, and proposes that a serpentine cooler is arranged in a middle-upper reduction reaction zone outside a reactor cylinder body so as to improve the heat dissipation capacity of the reactor wall; CN106521156A discloses a forced heat dissipation energy-saving device for titanium sponge reduction production, which uses a blower fan to perform blast cooling on the wall of a reaction vessel.
However, the inventors have recognized that there is still room for further improvement in such current solutions.
Disclosure of Invention
In order to solve the technical problem, the embodiment of the invention provides a titanium sponge production reactor, which aims to solve the problem of 'hard core' in titanium sponge production in the prior art.
The invention discloses a titanium sponge production reactor, which comprises a tank body, a feeding device and a flow guide device, wherein the flow guide device is arranged below the liquid level of the tank body;
the flow guide device is provided with an upper surface gradually reduced from the center of the tank body to the periphery and a through hole superposed with the vertical center of the tank body;
the feeding device is used for feeding materials by spraying. Further, the ratio of the distance between the outer edge of the flow guide device and the inner side wall of the tank body to the inner diameter of the tank body is as follows: 1 (5-7), preferably 1: 6.
further, the ratio of the through hole to the inner diameter of the tank body is 1 (4-6), preferably 1: 5.
furthermore, the upper surface of guiding device has the titanium layer that oozes.
Further, the feeding device also comprises a tank cover, and the feeding branch pipes are uniformly arranged on the tank cover.
Further, the upper surface of the flow guide device is located 100-300mm below the liquid level.
Further, the flow guide device is an annular flow guide plate, and an included angle between an extension line of the annular flow guide plate and a vertical center line of the tank body is 15-45 degrees, and preferably 30 degrees.
Further, the feeding device comprises a feeding speed control device and at least two feeding branch pipes;
the charging branch pipes are uniformly arranged on the tank cover and partially extend into the tank body; a first included angle is formed between the extension line of the feeding branch pipe and the vertical central line of the tank body;
the feeding speed control device is used for controlling the feeding speed of the feeding branch pipe.
Further, the internal diameter at the outlet of the charging branch is smaller than the internal diameter at the inlet of the charging branch.
Further, the ratio of the inner diameter at the inlet to the inner diameter at the outlet is (10-15): 1.
by adopting the technical scheme, the invention at least has the following beneficial effects:
according to the titanium sponge production reactor provided by the invention, the diversion device is arranged, and the injection feeding of the injection device is combined, so that the materials in the reactor flow under the injection kinetic energy and the diversion of the diversion device, the heat dissipation capability of the reactor is improved, and meanwhile, due to the existence of the diversion device, the reaction area is closer to the inner wall of the reactor, the reaction heat can be dissipated by the inner wall more quickly, and the heat conduction capability of the reaction area is improved.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
Fig. 1 is a schematic structural diagram of a titanium sponge production reactor according to an embodiment of the present invention.
FIG. 2 is a schematic structural diagram of a titanium sponge production reactor according to an embodiment of the present invention.
FIG. 3 is a schematic view of a feeding branch pipe of a titanium sponge production reactor according to an embodiment of the present invention.
Fig. 4 is a schematic structural diagram of a flow guiding device of a titanium sponge production reactor according to an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the following embodiments of the present invention are described in further detail with reference to the accompanying drawings.
It should be noted that all expressions using "first" and "second" in the embodiments of the present invention are used for distinguishing two entities with the same name but different names or different parameters, and it should be noted that "first" and "second" are merely for convenience of description and should not be construed as limitations of the embodiments of the present invention, and they are not described in any more detail in the following embodiments.
The titanium sponge is used as an important raw material for preparing titanium and titanium alloy, the compaction performance of the consumable electrode is seriously influenced by the porosity, the aperture size and other loosening characteristics of the titanium sponge, the current titanium sponge has better loosening performance, and the titanium sponge with lower barreled density value is popular in the market.
As shown in fig. 2 and fig. 4, some embodiments of the present invention disclose a titanium sponge production reactor, which can provide titanium sponge with low density value and good loosening property, and comprises a tank 1, a feeding device and a flow guiding device 4, wherein the flow guiding device 4 is arranged below the liquid level of the tank 1; the flow guide device 4 is provided with an upper surface gradually reduced from the center of the tank body 1 to the periphery and a through hole 42 superposed with the vertical center of the tank body 1; the feeding device is used for feeding materials by spraying. This embodiment combines together through the mode that sets up guiding device 4 and spray the feeding, makes the material in the reactor flow under the water conservancy diversion of spraying kinetic energy and guiding device 4, improves the heat-sinking capability of reactor, simultaneously because guiding device 4's existence for the inner wall distance of reaction zone and reactor is nearer, makes the reaction heat can be gived off by the inner wall sooner, thereby improves the heat-conduction ability of reaction zone.
In the titanium sponge production reactor disclosed by some embodiments of the invention, as shown in fig. 2 and 4, the distance between the outer edge of the flow guide device 4 and the inner side wall of the tank 1 is preferably 200mm and 400 mm. In some embodiments, the flow guiding device 4 is an annular flow guiding plate 41, such as an inverted bowl structure, and the extension line of the annular flow guiding plate forms an angle of 15 ° to 45 °, preferably 30 °, with the vertical center line of the tank 1. During the reaction, guiding device 4 is located the below liquid level of filling tube, and titanium tetrachloride that sprays gives the liquid level an impact, impels the reaction liquid to flow, under guiding of guiding device 4, when the impact force is located jar body 1 and is close to the edge, the reaction liquid sinks by guiding device 4 outer fringe, then flows to jar body 1 center, upwards overflows by the through-hole of guiding device 4 again, finally flows down along guiding device 4 upper surface, forms the circulation to the flow velocity of near reaction zone liquid magnesium has been accelerated. In the reaction process, the wall of the reaction container can be cooled in a blowing mode, and the height of an air inlet of cooling air can be the same as the surface height of the liquid level. The diversion device 4 can be welded and fixed on the lower surface of the reaction container cover, namely the tank cover 2, through the connecting column 43, and the surface of the diversion device is subjected to titanizing treatment before use, namely the upper surface of the diversion device 4 is provided with a titanizing layer.
Referring to fig. 1 and 3, some embodiments of the present invention disclose a titanium sponge production reactor, which comprises a tank body 1, a tank cover 2, a feeding rate control device, and at least two feeding branch pipes 3; wherein, the charging branch pipe 3 is uniformly arranged on the tank cover 2 and partially extends into the tank body 1; a first included angle is formed between the extension line of the feeding branch pipe 3 and the vertical central line of the tank body 1; the feeding speed control device is used for controlling the feeding speed of the feeding branch pipe 3. The sponge titanium production reactor and the feeding method provided by the embodiment spray and feed through the plurality of feeding branch pipes 3 which are inclined and evenly arranged, so that the position of titanium tetrachloride when entering the surface of magnesium liquid is close to the inner wall of the tank body 1, the rapid heat dissipation is facilitated, meanwhile, the spraying and feeding mode with a certain speed is realized, the surface of the liquid magnesium is impacted, the reaction liquid can be promoted to have better fluidity, and the heat dissipation capability is further improved. As shown in figure 1, the high temperature material in the reactor will move fast to the reaction wall, and the heat dissipating capacity of the reactor can be improved obviously by blowing air to the wall. In addition, a manifold is adopted for dispersing and feeding, so that on one hand, the reaction heat can be uniformly released, in addition, the distance between the reaction zone and the cooling wall can be shortened, and the heat dissipation capacity of the reaction zone is improved.
On the basis of the above embodiment, a flow guide device 4 is additionally arranged in the reactor, and finally the materials in the reactor flow in the direction shown in fig. 2. As shown in FIG. 2, high temperature MgCl is formed in the reactor2The titanium sponge can move to the reaction wall surface rapidly, and the heat dissipation capacity of the reactor can be improved remarkably. In addition, the multi-branch pipe is adopted for dispersing and feeding, so that the reaction heat can be uniformly released, the distance between the reaction zone and the cooling wall of the reactor can be shortened, and the reaction zoneHeat transfer capability.
The charging branch pipes 3 are uniformly arranged on the tank cover 2 in the circumferential direction, the number of the charging branch pipes 3 can be 3-4, generally, 4 charging branch pipes 3 are the preferred configuration mode, 3 charging branch pipes 3 are selected, and the charging branch pipes 3 form an angle of 120 degrees with each other on the surface of the tank cover 2; when 4 feeding branch pipes 3 are selected, the feeding branch pipes 3 mutually form an angle of 90 degrees on the surface of the tank cover 2; for a reactor with the inner diameter of 1400-2200 and the longitudinal height of 3500-5500 mm, TiCl of a single feeding branch pipe 34The feeding speed can be 80-120 kg/h, and is preferably 120 kg/h; feed branch 3 with TiCl4The height difference of the storage tanks is 10-15 m, preferably 15 m; TiCl (titanium dioxide)4The feeder and the feeding branch pipe 3 can adopt a piston volume type feeder, the piston moves for 1 time to feed 1kg, and the movement time is less than or equal to 1 second.
In the reactor for producing titanium sponge disclosed in some embodiments of the present invention, the first included angle is 30-60 °, preferably 45 °. And the charging branch 3 is gradually distanced from the vertical centre line in the charging direction of the charging branch 3. Preferably, the feed manifold 3 is of a necked down configuration, i.e. the internal diameter at the outlet of the feed manifold 3 is smaller than the internal diameter at the inlet of the feed manifold 3, combined with an inclined configuration, to accelerate the titanium tetrachloride away from the outlet of the feed manifold 3 to spray it onto the surface of the liquid magnesium at a higher velocity to achieve greater momentum to impact the reaction surface. Preferably the ratio of the internal diameter at the inlet to the internal diameter at the outlet is (10-15): 1, preferably 15: 1.
in some embodiments of the present invention, as shown in fig. 3, the charging branch 3 comprises an inlet straight section 33, a necking section 32 and an outlet straight section 31 which are connected in sequence, wherein the inner diameter of the inlet straight section 33 is larger than the inner diameter of the outlet straight section 31, and the inner diameter of the necking section 32 is gradually reduced along the charging direction of the charging branch 3. Also, the inner walls of the inlet straight section 33, the neck section 32 and the outlet straight section 31 are shown as smoothly transitioning to minimize drag. The length ratio of the inlet straight section to the necking section to the outlet straight section is (1.8-2.2): (0.8-1.2): 1; preferably, the ratio of 2: 1: 1; or the total length of the feeding branch pipe is 100-1000 mm; in some embodiments, the inner diameter of the outlet straight section 31 may be 1-4mm, preferably 1 mm. The ratio of the distance between the installation position of the charging branch pipe 3 on the tank cover 2 and the vertical central line of the tank body 1 to the inner diameter of the tank body is 1: (16-20), preferably 1: 18. in some embodiments, the distance between the location of the charging branch 3 on the can lid 2 and the vertical centre line of the can body 1 may be 100 mm. The ratio of the distance from the outlet of the feeding branch pipe to the liquid level of the reaction liquid in the tank body to the longitudinal height in the tank body is 1: (8-10), preferably 1: 9; in some embodiments, the outlet of the feed manifold 3 may be 600mm above the reaction solution in the tank 1. In order to connect the feeding branch pipe 3 with the titanium tetrachloride delivery pipeline, the feeding branch pipe 3 further comprises a connecting flange 34, and the connecting flange 34 is connected with a flange on the titanium tetrachloride delivery pipeline so as to realize connection, and a flow meter is arranged on the titanium tetrachloride delivery pipeline and is used for controlling the flow of the delivered titanium tetrachloride.
For the problems that the pore structure of titanium sponge is compact and titanium lumps have hard cores, the embodiment of the invention also discloses a feeding method for titanium sponge production reaction from the angle that the heat of a reaction container is uniformly released and the flowing speed of materials in the reaction container is accelerated, wherein the feeding method comprises the steps of carrying out jet feeding through a plurality of feeding branch pipes 3 which are inclined and uniformly arranged, and the ratio of the distance between the falling point of titanium tetrachloride in the feeding branch pipes when the titanium tetrachloride falls to the surface of reaction liquid and the inner side wall of the tank body to the inner diameter of the tank body is 1: (5-7), in some embodiments, the distance between the point of the titanium tetrachloride in the feed branch pipe 3 falling to the surface of the reaction solution and the inner side wall of the tank 1 is 200mm to 400mm, preferably 200 mm.
Example 1
As shown in FIG. 1 and FIG. 3, TiCl4When the feeding branch pipes 3 are arranged, 4 feeding branch pipes 3 are uniformly arranged on the tank cover 2 of the reduction reactor, each feeding branch pipe 3 forms an angle of 45 degrees with the center line of the reactor, and the feeding branch pipes 3 mutually form an angle of 90 degrees; the feed manifold 3 was mounted on the tank cover 2 at a position 100mm from the center line of the reactor. Feeding branch pipe 3 flange and TiCl4The pipes are connected by means of a connecting flange 34 to TiCl of a longitudinal height of 15m4TiCl is injected into the storage tank4Control of TiCl4The liquid level is 1-9 mm. During the reaction, the reaction solution is added into a reaction vessel with the diameter of 1800mm, namely a tank body 1Feeding liquid Mg, wherein the distance between the surface of the liquid Mg and the outlet of the branch pipe is 600 mm; heating the liquid magnesium to 780-850 ℃, and opening TiCl4A charging valve and a remote control volume type flowmeter for charging and controlling TiCl4The total pipe material speed is 400kg/h, and each branch pipe material speed is 100 kg/h. Single batch TiCl4After the addition amount reaches 1000kg, MgCl is added into the reactor2Discharging, single batch MgCl2The discharge amount is 822 kg; after the discharge was completed, the next TiCl batch was started4Adding until TiCl4After the total amount of the added solution reaches 30000kg, the TiCl addition is stopped4Adding materials and carrying out vacuum distillation operation.
Example 2
As shown in FIG. 2, FIG. 3, FIG. 4, TiCl4When the feeding pipes are arranged, 4 feeding branch pipes 3 are uniformly arranged on a tank cover 2 of the reduction reactor, each feeding branch pipe 3 forms an angle of 45 degrees with the center line of the reactor, and the feeding branch pipes 3 mutually form an angle of 90 degrees; the feed manifold 3 was mounted on the tank cover 2 at a position 100mm from the center line of the reactor. Connecting flange 34 of charging branch 3 with TiCl4The pipes are connected by means of a connecting flange 34 to TiCl of a longitudinal height of 15m4TiCl is injected into the storage tank4Control of TiCl4The liquid level is 1-9 mm; carrying out titanizing treatment on the flow guide device 4, using water as a binder, and uniformly coating hydrogenated and dehydrogenated titanium powder on the surface of the flow guide device 4; placing the flow guide device 4 in a vacuum furnace, heating the vacuum furnace to 500 ℃, pumping the vacuum degree to be below 9Pa, and staying for 5 hours; heating the vacuum furnace to 1000 ℃, controlling the vacuum degree to be below 9Pa, and staying for 20 hours; filling argon into the vacuum furnace, and controlling the gauge pressure to be more than 5 kPa; the vacuum furnace is closed, the temperature of the vacuum furnace is reduced to room temperature, and the flow guide device 4 is taken out. When the flow guide device 4 is installed, before the reactor is put into use, the flow guide device 4 is welded with the lower surface of the tank cover 2 of the reaction vessel, the center line of the flow guide device 4 is ensured to be coincident with the center line of the reaction vessel, namely the tank body 1, and the upper surface of the flow guide device 4 is controlled to be 1000mm away from the lower surface of the tank cover 2; controlling the edge of the flow guide device 4 to be 300mm away from the inner wall of the reaction vessel; TiCl (titanium dioxide)4When feeding, adding liquid Mg into a reactor with the diameter of 1800mm, and enabling the distance between the surface of the liquid Mg and the outlet of the feeding branch pipe 3 to be 600 mm; heating the liquid magnesium to 780-850 ℃, and opening TiCl4Charging valve, remote controlPreparing volume type flowmeter for feeding and controlling TiCl4The total pipe material speed is 400kg/h, and each branch pipe material speed is 100 kg/h. Single batch TiCl4After the addition amount reaches 1000kg, MgCl is added into the reactor2Discharging, single batch MgCl2Stopping discharging after the discharging amount is 822 kg; starting the next batch of TiCl4Adding until TiCl4After the total amount of the added TiCl had reached 30000kg, the TiCl addition was stopped4Adding materials and carrying out vacuum distillation operation.
In summary, the reactor for producing titanium sponge and the feeding method disclosed in the embodiments of the present invention add titanium tetrachloride into the reaction vessel in a manner of tilting at a certain angle and high-speed spraying through the manifold, so as to shorten the distance between the reaction area and the wall of the reactor, accelerate the flow rate of the material in the reactor, and achieve uniform generation and rapid dissipation of heat in the reactor. The heat dissipation capability of the reaction vessel is obviously improved, and the sponge titanium with a loose pore structure can be obtained under the condition of high TiCl4 feeding speed.
It should be noted that, the components or steps in the above embodiments can be intersected, replaced, added or deleted, and therefore, the combination formed by reasonable permutation and combination conversion shall also belong to the protection scope of the present invention, and shall not limit the protection scope of the present invention to the above embodiments.
The above is an exemplary embodiment of the present disclosure, and the order of disclosure of the above embodiment of the present disclosure is only for description and does not represent the merits of the embodiment. It should be noted that the discussion of any embodiment above is exemplary only, and is not intended to intimate that the scope of the disclosure, including the claims, of embodiments of the invention is limited to those examples, and that various changes and modifications may be made without departing from the scope, as defined in the claims. The functions, steps and/or actions of the method claims in accordance with the disclosed embodiments described herein need not be performed in any particular order. Furthermore, although elements of the disclosed embodiments of the invention may be described or claimed in the singular, the plural is contemplated unless limitation to the singular is explicitly stated.
Those of ordinary skill in the art will understand that: the discussion of any embodiment above is meant to be exemplary only, and is not intended to intimate that the scope of the disclosure, including the claims, of embodiments of the invention is limited to these examples; within the idea of an embodiment of the invention, also technical features in the above embodiment or in different embodiments may be combined and there are many other variations of the different aspects of an embodiment of the invention as described above, which are not provided in detail for the sake of brevity. Therefore, any omissions, modifications, substitutions, improvements, and the like that may be made without departing from the spirit and principles of the embodiments of the present invention are intended to be included within the scope of the embodiments of the present invention.
Claims (7)
1. A titanium sponge production reactor is characterized by comprising a tank body, a tank cover, a feeding device and a flow guide device, wherein the flow guide device is arranged below the liquid level of the tank body;
the flow guide device is provided with an upper surface gradually reduced from the center of the tank body to the periphery and a through hole superposed with the vertical center of the tank body;
the feeding device is used for feeding materials by spraying;
the flow guide device is an annular flow guide plate, and the included angle between the extension line of the annular flow guide plate and the vertical center line of the tank body is 15-45 degrees;
the feeding device comprises a feeding speed control device and at least two feeding branch pipes;
the feeding branch pipes are uniformly arranged on the tank cover and partially extend into the tank body; a first included angle is formed between the extension line of the feeding branch pipe and the vertical central line of the tank body;
the feeding speed control device is used for controlling the feeding speed of the feeding branch pipe.
2. The titanium sponge production reactor as claimed in claim 1,
the ratio of the distance between the outer edge of the flow guide device and the inner side wall of the tank body to the inner diameter of the tank body is as follows: 1: (5-7).
3. The titanium sponge production reactor as claimed in claim 1, wherein the ratio of the through hole to the inner diameter of the tank body is 1 (4-6).
4. The titanium sponge production reactor as claimed in claim 1, wherein the upper surface of said deflector has a titanium infiltrated layer.
5. The titanium sponge production reactor as claimed in claim 4, wherein the upper surface of the flow guide device is located 100-300mm below the liquid level.
6. The titanium sponge production reactor according to claim 1, wherein the internal diameter at the outlet of said feeding branch is smaller than the internal diameter at the inlet of said feeding branch.
7. The titanium sponge production reactor as claimed in claim 6 wherein the ratio of the internal diameter at the inlet to the internal diameter at the outlet is (10-15): 1.
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| JPH10306974A (en) * | 1997-05-06 | 1998-11-17 | Nippon Samusun Kk | Humidifying refrigerator |
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