CN115725859B - Titanium sponge fluidization reaction system and method - Google Patents
Titanium sponge fluidization reaction system and method Download PDFInfo
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- CN115725859B CN115725859B CN202211456012.6A CN202211456012A CN115725859B CN 115725859 B CN115725859 B CN 115725859B CN 202211456012 A CN202211456012 A CN 202211456012A CN 115725859 B CN115725859 B CN 115725859B
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- sieve plate
- plate
- feed inlet
- reaction
- titanium sponge
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 49
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 238000005243 fluidization Methods 0.000 title claims abstract description 17
- 238000000034 method Methods 0.000 title claims description 12
- 239000000463 material Substances 0.000 claims abstract description 30
- 239000002893 slag Substances 0.000 claims description 27
- 229910052719 titanium Inorganic materials 0.000 claims description 14
- 239000010936 titanium Substances 0.000 claims description 14
- 239000000571 coke Substances 0.000 claims description 11
- 238000009826 distribution Methods 0.000 claims description 10
- 230000036632 reaction speed Effects 0.000 abstract description 5
- 239000002245 particle Substances 0.000 abstract description 3
- 239000002006 petroleum coke Substances 0.000 description 5
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 5
- 238000005660 chlorination reaction Methods 0.000 description 4
- 238000007599 discharging Methods 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 230000002349 favourable effect Effects 0.000 description 3
- 238000012216 screening Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000013049 sediment Substances 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
Classifications
-
- 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
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- Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)
Abstract
The invention relates to a titanium sponge fluidization reaction system, which comprises a reaction furnace, wherein the reaction furnace is a fluidized bed reaction furnace, an exhaust port is arranged at the top of the reaction furnace, an air inlet is arranged at the bottom of the reaction furnace, an upper sieve plate and a lower sieve plate are arranged in the reaction furnace, an upper feed inlet and a lower feed inlet are arranged on the side wall of the fluidized bed, the upper feed inlet is positioned above the upper sieve plate, and the lower feed inlet is positioned between the upper sieve plate and the lower sieve plate. The invention adopts a double-layer sieve plate fluidized bed, the upper space of the lower sieve plate is used as a main fluidized reaction area, and an upper sieve plate is arranged above the upper space, so that in the aspect of controlling the granularity of materials, the lower sieve plate adopts materials with finer granularity, the specific surface area of the particles is increased, and the reaction speed is improved.
Description
Technical Field
The invention relates to a titanium sponge fluidization reaction system and a titanium sponge fluidization reaction method, and belongs to the technical field of titanium sponge production.
Background
The high titanium slag and petroleum coke are subjected to chlorination reaction to obtain titanium tetrachloride, and the titanium tetrachloride is reduced to obtain titanium sponge. In the prior art, boiling chlorination is widely adopted to prepare titanium tetrachloride, and the boiling chlorination is carried out in a fluidized bed reactor. Because impurities such as calcium and magnesium exist in the high titanium slag, liquid chloride is generated in the reaction furnace after chlorination reaction, the chloride is easy to bond with materials into clusters, gas distribution holes of a sieve plate are blocked, slag discharge is inconvenient, and most manufacturers adopt a fluidized bed without the sieve plate at present. However, the fluidized bed without the sieve plate has unstable fluidization state and great control difficulty due to uneven gas distribution. In addition, in the aspect of material granularity control, because the petroleum coke has low density and light texture relative to high titanium slag, the petroleum coke is easy to float on the upper layer under the driving of air flow, so that the titanium slag and coke are not fully mixed, and finer coke powder is easy to be taken away by the air flow, so that the petroleum coke granularity is generally controlled to be more than 1 mm. However, the petroleum coke has large granularity and small surface area, and limits the reaction speed.
Disclosure of Invention
Aiming at the problems, the invention provides a titanium sponge fluidization reaction system and a method, and the specific scheme is as follows:
the utility model provides a titanium sponge fluidization reaction system, includes the reacting furnace, and the reacting furnace is the fluidized bed reacting furnace, and the reacting furnace top is equipped with the gas vent, and the bottom is equipped with the air inlet, is equipped with upper screen plate and sieve down in the reacting furnace, and the fluidized bed lateral wall is equipped with feed inlet and feed inlet down, and upper feed inlet is located upper screen plate top, and lower feed inlet is located between upper screen plate and the sieve down.
Further, the upper sieve plate is provided with an overflow pipe, and the height of the overflow pipe is not more than 10cm.
Further, the distance between the upper screen plate and the lower screen plate is not less than 1/2 of the height of the furnace body. The space between the upper screen plate and the lower screen plate is used as the main reaction area, and the height of the space should be
Further, the lower sieve plate comprises a fixed plate and a movable plate which are overlapped up and down, the fixed plate is positioned on the upper layer, the movable plate is positioned on the lower layer, the surfaces of the fixed plate and the movable plate are formed by V-shaped grooves, the groove wall at one side of each V-shaped groove is provided with gas distribution holes, the gas distribution holes are positioned in the middle part or the upper part of the groove wall, the groove wall at the other side of each V-shaped groove is provided with slag discharge holes, and the heights of the slag discharge holes are consistent with the heights of the groove walls; the movable plate is provided with a vibrating mechanism.
Further, the side wall of the reaction furnace is provided with an airtight chamber, the edge of the movable plate is provided with an ear plate, and the ear plate is positioned in the airtight chamber; the vibration mechanism is an electromagnetic vibrator, the electromagnetic vibrator is arranged in the airtight chamber, and an armature of the electromagnetic vibrator is fixed on the ear plate.
Further, the air inlet is provided with a pressure sensor, and the pressure sensor is used for controlling the electromagnetic vibrator.
According to the control method for the fluidization reaction of the titanium sponge, the titanium sponge fluidization reaction system is used, the granularity of the material at the upper feed inlet is 1-3 mm, and the granularity of the material at the lower feed inlet is 0.1-0.5 mm; the mass ratio of the titanium slag to the coke in the upper feed inlet is 1:0.3, the mass ratio of titanium slag to coke in the lower feed inlet is 1:3.
further, the temperature between the upper screen plate and the lower screen plate is controlled to be 1000-1050 ℃, and the temperature above the upper screen plate is controlled to be below 1000 ℃.
In the invention, a double-layer sieve plate fluidized bed is adopted, the upper space of the lower sieve plate is used as a main fluidized reaction area, and an upper sieve plate is arranged above the upper space, so that in the aspect of controlling the granularity of materials, the lower sieve plate is fed with materials with finer granularity, the specific surface area of the particles is increased, and the reaction speed is improved. The upper sieve plate is fed with materials with larger granularity, and an isolating layer is formed above the upper sieve plate, so that finer coke particles below the upper sieve plate can be prevented from being taken away by airflow. In addition, in the improvement scheme, the lower sieve plate adopts the composite structure of fixed plate and fly leaf, when the pressure of admitting air is unusual, through vibration mechanism drive fly leaf vibration, carry out the sediment, can solve the problem that the adhesion material takes place to block up of sieve gas distribution hole.
Drawings
FIG. 1 is a schematic structural view of a reaction furnace according to the present invention;
FIG. 2 is a schematic cross-sectional view of a lower screen panel of the present invention;
fig. 3 is a schematic structural view of a movable plate according to the present invention.
Detailed Description
The following describes the aspects of the present invention in detail with reference to specific examples.
Example 1
As shown in fig. 1 to 3, a titanium sponge fluidization reaction system of the present embodiment includes a reaction furnace, which is a fluidized bed reaction furnace. The top of the reaction furnace is provided with an exhaust port, the exhaust port is used for connecting a cyclone separator and a condensing tower, the cyclone separator is used for separating coke powder and other solid impurities in the gas, and the condensing tower is used for condensing gaseous titanium tetrachloride into liquid for recycling. The bottom of the reaction furnace is provided with an air inlet 1 which is used for introducing chlorine. In this scheme, be equipped with sieve 2 and lower sieve 3 in the reacting furnace, the fluidized bed lateral wall is equipped with feed inlet 4 and lower feed inlet 5, goes up the feed inlet and is located the sieve top, and lower feed inlet is located between sieve and the lower sieve.
In the prior art, a multi-layer sieve plate fluidized bed is arranged, which is generally used for drying materials, a feed inlet of the multi-layer sieve plate fluidized bed is arranged at the uppermost layer, and the materials firstly enter the uppermost layer sieve plate and then sequentially enter the lower layer sieve plate along an overflow pipe. The difference between the scheme and the prior art is that the upper and lower sides of the upper layer sieve plate are provided with feed inlets, wherein the lower feed inlet is a main feed inlet, most of materials enter the reaction furnace along the lower feed inlet, the upper feed inlet is a secondary feed inlet, and a small part of materials enter the reaction furnace along the upper feed inlet. The mass ratio of the feed amount of the upper feed port and the lower feed port can be selected as 1: 6-10. The lower layer serves as the main reaction region, and the upper layer is used only to form a single isolation layer.
In this scheme, go up the sieve and be equipped with overflow pipe 6, the height of overflow pipe is not more than 10cm. The height referred to herein is the height of the overflow pipe relative to the upper end of the screening surface of the upper screening deck, which height is related to the thickness of the material on the upper screening deck during operation. Because the upper sieve plate is not used as a main reaction area, an isolating layer is formed, and fine powder below the structure is taken away by airflow, the material thickness of the upper sieve plate is not required to be controlled too much. When the upper sieve plate material is piled up to exceed the upper end of the overflow pipe, the material falls into the lower part along the overflow pipe. The overflow pipe can be provided with a plurality of overflow pipes which are uniformly distributed on the upper sieve plate.
In order to ensure that a larger reaction space exists between the upper sieve plate 2 and the lower sieve plate 3, the distance between the upper sieve plate and the lower sieve plate is not less than 1/2 of the height of the furnace body.
Aiming at the technical problem that the reaction furnace with the sieve plate is inconvenient to slag, in the scheme, the lower sieve plate comprises a fixed plate 7 and a movable plate 8 which are overlapped up and down, the fixed plate is positioned on the upper layer, the movable plate is positioned on the lower layer, the surfaces of the fixed plate and the movable plate are both formed by V-shaped grooves, one side groove wall of each V-shaped groove is provided with a gas distribution hole 9, the gas distribution hole is positioned in the middle part or the upper part of the groove wall, the groove wall of the other side is provided with a slag hole 10, and the height of the slag hole is consistent with the height of the groove wall; the movable plate is provided with a vibrating mechanism 11. When the fixed plate and the movable plate are attached, the slag discharging hole with large aperture is shielded, the movable plate vibrates up and down when the vibrating mechanism works, the slag discharging hole is exposed when the movable plate is separated from the fixed plate downwards, and the agglomerated solid slag deposited in the groove can roll down below the lower sieve plate along the slag discharging hole and is discharged by the slag discharging valve at the bottom of the reaction furnace at regular intervals. The vibrating mechanism provides a vibrating force for the movable plate at the same time, which is beneficial to separating the solid slag adhered on the sieve plate from adhesion.
In this embodiment, a specific connection structure of the movable plate is that an airtight chamber is provided at a side wall of the reaction furnace, and the airtight chamber is isolated from the outside. The edge of the movable plate is provided with an ear plate 12 which is positioned in the airtight chamber; the vibration mechanism is an electromagnetic vibrator, the electromagnetic vibrator is arranged in the airtight chamber, and an armature of the electromagnetic vibrator is fixed on the ear plate. When the electromagnetic vibrator is electrified, the armature is driven to vibrate, and the movable plate is driven to vibrate.
In this scheme, be equipped with pressure sensor at the air inlet, pressure sensor is used for controlling electromagnetic vibrator. When the gas distribution holes on the lower sieve plate are blocked, the air inlet pressure is increased, and when the pressure signal acquired by the pressure sensor exceeds a threshold value, the electromagnetic vibrator is controlled to be started.
The control method of the reaction system comprises the steps of controlling the material granularity of each feed inlet and the mass ratio of titanium slag coke, wherein the material granularity of the upper feed inlet is 1-3 mm, and the material granularity of the lower feed inlet is 0.1-0.5 mm; the material granularity of the lower feed inlet is finer, the surface area is large, and the reaction speed is improved. The upper feed inlet has larger material granularity, avoids being taken away by air flow, is beneficial to forming a stable material layer on the upper sieve plate, and prevents fine powder below from being taken away along with the air flow.
In addition, the mass ratio of the titanium slag to the coke in the upper feed inlet is 1:0.3, the mass ratio of titanium slag to coke in the lower feed inlet is 1:3. the lower feeding adopts higher coke proportion, which is beneficial to the complete reaction of titanium slag. The titanium slag content in the material that goes into of last feed inlet is high, can not fully react at last sieve, and when the material of last sieve piles up more, falls into below along the overflow pipe and continues the reaction.
Another benefit of this design is that the coke is light and easily floats under the air flow. In this scheme, the titanium sediment of last sieve just in time mixes with the coke powder of come-up along the overflow pipe whereabouts back, avoids appearing layering, is favorable to the stable of reaction to go on.
In the scheme, the temperature between the upper sieve plate and the lower sieve plate is controlled to be 1000-1050 ℃, and the temperature above the upper sieve plate is controlled to be below 1000 ℃. The temperature in the main reaction area is kept higher, which is favorable for improving the reaction speed, the temperature above the upper sieve plate is controlled to be slightly lower, the temperature of the tail gas can be reduced, and the condensation recovery of the titanium tetrachloride by the subsequent condensing tower is favorable. The temperature control of each section in the reaction furnace can be realized by the preheating temperature control of the materials at each feed inlet. For example, when the temperature above the upper screen plate needs to be reduced, the preheating temperature of the materials conveyed to the upper feed inlet can be reduced.
Claims (5)
1. The utility model provides a titanium sponge fluidization reaction control method, the reaction system who uses includes the reacting furnace, and the reacting furnace is fluidized bed reacting furnace, and the reacting furnace top is equipped with the gas vent, and the bottom is equipped with air inlet, its characterized in that: an upper sieve plate and a lower sieve plate are arranged in the reaction furnace, an upper feed inlet and a lower feed inlet are arranged on the side wall of the fluidized bed, the upper feed inlet is positioned above the upper sieve plate, and the lower feed inlet is positioned between the upper sieve plate and the lower sieve plate; the upper sieve plate is provided with an overflow pipe, and the height of the overflow pipe is not more than 10cm;
the control method of the titanium sponge fluidization reaction system comprises the steps that the granularity of the material at the upper feed inlet is 1-3 mm, and the granularity of the material at the lower feed inlet is 0.1-0.5 mm; the mass ratio of the titanium slag to the coke in the upper feed inlet is 1:0.3, the mass ratio of titanium slag to coke in the lower feed inlet is 1:3, a step of; the temperature between the upper sieve plate and the lower sieve plate is controlled to be 1000-1050 ℃, and the temperature above the upper sieve plate is controlled to be below 1000 ℃.
2. The method for controlling fluidization reaction of titanium sponge according to claim 1, wherein: the distance between the upper sieve plate and the lower sieve plate is not less than 1/2 of the height of the furnace body.
3. The method for controlling fluidization reaction of titanium sponge according to claim 1, wherein: the lower screen plate comprises a fixed plate and a movable plate which are overlapped up and down, the fixed plate is positioned on the upper layer, the movable plate is positioned on the lower layer, the surfaces of the fixed plate and the movable plate are formed by V-shaped grooves, the groove wall on one side of each V-shaped groove is provided with gas distribution holes, the gas distribution holes are positioned in the middle part or the upper part of the groove wall, the groove wall on the other side of each V-shaped groove is provided with slag discharge holes, and the heights of the slag discharge holes are consistent with the heights of the groove walls; the movable plate is provided with a vibrating mechanism.
4. A method for controlling a fluidization reaction of titanium sponge according to claim 3, wherein: the side wall of the reaction furnace is provided with an airtight chamber, the edge of the movable plate is provided with an ear plate, and the ear plate is positioned in the airtight chamber; the vibration mechanism is an electromagnetic vibrator, the electromagnetic vibrator is arranged in the airtight chamber, and an armature of the electromagnetic vibrator is fixed on the ear plate.
5. The method for controlling fluidization reaction of titanium sponge according to claim 4, wherein: the air inlet is provided with a pressure sensor which is used for controlling the electromagnetic vibrator.
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